WO2010003179A1 - A method of fabricating a material - Google Patents
A method of fabricating a material Download PDFInfo
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- WO2010003179A1 WO2010003179A1 PCT/AU2009/000877 AU2009000877W WO2010003179A1 WO 2010003179 A1 WO2010003179 A1 WO 2010003179A1 AU 2009000877 W AU2009000877 W AU 2009000877W WO 2010003179 A1 WO2010003179 A1 WO 2010003179A1
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- WIPO (PCT)
- Prior art keywords
- material component
- substrate
- component
- diamond
- incorporated
- Prior art date
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/274—Diamond only using microwave discharges
Definitions
- the present invention broadly relates to a method of fabricating a material.
- Quantum communication systems are optical data transmission systems that enable secure transmission of the data. Quantum communication relies on the principals of quantum mechanics and requires transmission of single photons in contrast to large number of photons that are transmitted using conventional optical data transmission systems. If the data is transmitted in the form of pulses from a single photon source, it can be verified if the data has been accessed and/or changed in any way by an unauthorised party.
- Diamond crystals may be used for fabricating such single photon sources.
- Diamond crystals may contain optical centres that are arranged for emission of single photons.
- Such diamond crystals can be fabricated so that each diamond crystal only contains one optical centre and consequently each diamond crystal emits in use single photons.
- the optical centres comprise impurities that result in specific defects in the matrix of the diamond crystals and may for example comprise a nitrogen-vacancy optical centre or an optical centre that includes nitrogen and a metallic impurity or a vacancy and a metallic impurity.
- Diamond crystals having such optical centres may be fabricated using chemical vapour deposition (CVD) .
- CVD chemical vapour deposition
- the present invention provides technological advancement.
- the present invention provides in a first aspect a method of fabricating a material comprising first and second material components, the method comprising the steps of: providing a source of a first material component; providing a substrate comprising a third material component into which the second material component is incorporated in a manner such that a surface of the substrate is at least partially composed of the third material component and wherein the second material component is located in the proximity of the surface of the substrate; and fabricating the material on the substrate by forming the first material component on the substrate and transporting the second material component from the substrate to a location at which the material is fabricated so that the second material component is incorporated into the first material component.
- the step of providing the substrate typically comprises forming the substrate by incorporating the second component material into the third material component .
- the method typically is conducted so that, typically during formation of a portion of the first material component on the substrate, at least a portion of the second material component diffuses to a location of the first material component. Diffusion may comprise solid state diffusion or gas phase diffusion or a combination of solid state and gas phase diffusion.
- the incorporation usually occurs with less structural defects than incorporation for example by direct ion implantation into the first material. Incorporating the second material during formation of a portion of the first material component may also lead to a different charge state for the second material component and therefore a different optical response of the material compared to, for example, a material formed by direct ion implantation into the first material.
- the step of forming the substrate typically comprises incorporating the second material component into a depth of 10-50nm below a surface of the third material.
- Incorporating the second material component into the third material component typically comprises implanting the . second material component into the third material component.
- the step of forming the substrate typically comprises selecting at least one area of the surface of the third material component for incorporating the second material component so that, during fabrication of the material, the second material component is predominantly or solely incorporated into the first material component at the at least one selected area.
- the at least one selected area may have any size and may also be a relatively small area having a diameter of the order of 50 - 500 nm, such as 50 - lOOnm. Further, the selected area may be one of a plurality of selected areas and the selected area may also comprise a pattern.
- a local density of the second material component incorporated into the first material component may be controlled by controlling growth conditions and thereby controlling transportation of the second material component .
- the step of providing a source of the first material component typically comprises chemical vapour deposition (CVD) .
- the second material component typically is incorporated into the first material component by a solid state or gas diffusion process during formation of the first material component.
- the method typically is conducted so that at least one optical centre is formed in the material. Further, the method typically comprises controlling a number of optical centres in the formed material by controlling at least one growth parameter.
- the first material component is diamond
- the second material component comprises atoms or ions of a metallic material, such as nickel ions
- the third material component is silica or the like.
- the substrate may be formed by implanting the second material component into the silica at a selected area, such as a relatively small area having a diameter smaller than a typical diameter of the formed material. Formation of the diamond on the substrate may be conducted so that diamond crystallites form on the substrate having a diameter of the order of 10 to 500 nm, 30 - 300nm, 40 - 200nm and typically 50 - lOOnm.
- nickel related optical centres in the diamond crystal is limited to only one diamond crystal. Consequently, the controlled formation of a single photon source is facilitated. Further, a number of formed nickel related centres in the diamond material may be controlled by controlling growth conditions and thereby controlling the transportation of the nickel ions into the diamond material, which further facilitates the formation of a single photon source having one or nickel related optical centre .
- the second material component comprises atoms or ions of a metallic material, such as chromium ions, and the . third material component is sapphire including chromium impurities.
- Formation of the diamond on the substrate may be conducted so that diamond crystallites form on the substrate having a diameter of the order of 10 to 500 nm, 30 - 300nm, 40 - 200nm and ⁇ typically 50 - lOOnm.
- a number of formed chromium related centres in the diamond material may be controlled by controlling growth conditions and thereby controlling the transportation of the chromium ions into the diamond material .
- Embodiments of the present invention provide the advantage that the second material component may be incorporated into the first material component without the need to provide the second material component in a gas phase. This has the further practical advantage that contamination of an interior of a growth chamber by the second material component can be substantially avoided.
- the method typically comprises controlling a density of optical centres in the formed material by controlling at least one growth parameter.
- the method comprises selecting a plurality of areas of the third material at which the second material component will be located.
- the method may be conducted so that the second material component is implanted into a plurality of areas of the third material, each of which may have the above-described extension.
- the areas at which the second material component will be located may for example form an array.
- the material components and the areas may be arranged so that a plurality of single photon sources are formed, such as an array comprising diamond crystals each having a single chromium or nickel related optical centre.
- the second material component may not necessarily comprise chromium or nickel ions, but may alternatively comprise any other suitable atoms or ions and typically comprises atoms or ions of a metallic material, such as Ni, Li, Be, B, Al, P, S Co, Ni, Zn, As, Sb or Ir.
- the third material component may not necessarily be silica or sapphire, but may be any other suitable material.
- the first material component may not necessarily be diamond, but may also be any other suitable material in which the second material component may be incorporated.
- the method may comprise incorporating a plurality of second component materials into the third component material.
- the first material component may be diamond into which two or more different metallic material components are incorporated, or 'into which metallic and non-metallic components are incorporated. This may allow for the fabrication of optical centres comprising a combination of impurities such as Si/Ni, Cr/Al, Cr/O or other combinations .
- the method may further comprise selecting a concentration of the at least one second material component in the first material component by controlling a concentration at which the at least one second material component is incorporated in the third material prior to formation of the material.
- the step of forming the material may comprise positioning the substrate near a plasma in a CVD reactor so that the substrate is etched by the plasma whereby at least a portion of the second material component is exposed to the plasma to facilitate diffusion and subsequent incorporation of the second material component into the first material component.
- the method in accordance with the first aspect of the present invention has a number, of applications in many fields of science and technology.
- the method may be used to form materials, such as diamond crystallites, having any number of optical centres and applications.
- the present invention provides in a second aspect a single photon source formed by the method in accordance with the first aspect of the present invention.
- the present invention provides in a third aspect a biomarker formed by the method in accordance with the first aspect of the present invention.
- the biomarker typically is one of a plurality of biomarkers that may be fabricated simultaneously.
- the biomarker comprises a diamond crystal having one or more nickel or chromium related optical centres.
- Diamond is largely inert and consequently has no adverse effect on tissue, such as human tissue.
- the nickel for example nickel related optical centres emit in use photons at a wavelength of approximately 750nm - 900nm and the tissue is largely transparent at that wavelength. Consequently, such diamond crystals have properties that make the diamond crystals suitable for use as biomarkers.
- the present invention provides in a fourth aspect a biomarker, the biomarker comprising diamond, the diamond incorporating at least one optical centre arranged for the emission of photons have a wavelength in the range of 700- lOOOnm.
- the diamond typically comprises at least one chromium related optical centre that typically is arranged for emission of photons at a wavelength of approximately 750 - 900nm.
- Figure 1 shows a flow chart of a method of fabricating a material according to a first specific embodiment of the present invention
- Figures 2 (a) - (c) illustrate steps of the method of fabricating a material according to the first specific embodiment of the present invention
- Figure 3 shows a graph of photoluminescence spectra attributed to the material fabricated by the method according to the specific embodiment of the present invention
- Figure 4 shows a normalised autocorrelation function of the material fabricated by the method according to the specific embodiment of the present invention
- Figure 5 shows graph of a counting rate recorded from the material fabricated by the method according to the specific embodiment of the present invention.
- Figure 6 shows (a) a photoluminescence spectrum, (b) a normalised autocorrelation function and (c) fluorescence intensity saturation graphs for a material fabricated by a method according to a further specific embodiment of the present invention.
- Embodiments of the present invention generally relate to a method of fabricating a material.
- the material includes a first material component and a second material component that is incorporated into the first material component.
- the method comprises initially incorporating the second material component into a third material component, which then forms a substrate on which the material is fabricated.
- the second material component typically is located in the proximity of the surface of the substrate.
- the fabrication of the material typically is conducted so that at least a portion of the second material component is incorporated into the first material component by a solid state or gas diffusion process during growth of the material .
- Figure 1 illustrates a method 10 of fabricating photon sources.
- the photon sources include in this example a diamond material which incorporates nickel in the form of a nickel related optical centre.
- the first step 12 of the method 10 comprises incorporating a second material component into a third material .
- the second material component comprises nickel ions or atoms and the third material is provided in the form of a silica substrate. Ions of the nickel are implanted into the silica substrate and the implanted nickel ions or atoms are dispersed in the proximity of the surface of the silica without forming larger clusters that have metallic properties.
- Figures 2a to 2c further illustrate the method 10.
- Figure 2a shows a sample 20 comprising a silica substrate 22 having nickel ions 24 implanted below a surface of the silica substrate 22.
- the implantation of the nickel ions 24 was conducted by exposing the silica substrate 22 to a beam of nickel ions having an energy of the order of 20keV to 30keV.
- the direction of acceleration of the nickel ions 24 is indicated by arrows shown in Figure 2a.
- the energies of 20keV and 30keV cause implantation of the nickel ions 24 to a depth of approximately 20nm to 30 nm below the surface of the silica substrate 22. Doses of between 10 10 and 10 12 ions/cm 2 of nickel ions are implanted into the silica substrate 22
- a second step 14 of the method 10 forms the first material component on the surface of the substrate.
- the first material component is a diamond material 26 which is grown on the silica substrate 22.
- the sample 20, now comprising the silica substrate 22 which contains the implanted nickel ions 24, is transferred to a microwave chemical vapour deposition (CVD) reactor.
- the diamond material 26 shown in Figure 2b is then grown on the upper surface of the silica substrate 22 from nano-diamond seeds using a microwave plasma technique.
- at least a portion of the second material component is incorporated into the first material component (step 16 of method 10) .
- the nickel ions 24 are transported, for example by- diffusion, into the diamond material 26. This is illustrated in Figure 2b where arrows indicate the transportation of the nickel ions 24 into the diamond material 26. This transportation process may also continue to occur when the sample 20 is annealed.
- the method 10 may comprise selecting at least, one area of the surface of the substrate 22 prior to implanting the nickel ions 24 into the substrate 22.
- the at least one selected area may have any size and may also be a relatively small area having a diameter of the order within the range of 50 - lOOnm.
- the nickel ion beam is then focused onto the selected area so that the nickel ions are implanted predominantly in the selected area.
- the Ni ions can be implanted into the substrate through a mask. Further, a plurality of areas may be selected and the selected area may also form a pattern. For fabrication of one single photon source typically nickel ions are predominantly implanted into one area having an extension that is smaller that a typical extension of a diamond crystal. Consequently, it is likely that a nickel -related centre is formed in one diamond • crystal only. Alternatively, a plurality of areas may be selected for implantation so that a plurality of single photons sources may be formed, such as an array of single photon sources . Further, the second material component may be one of two or more different second material components which may be implanted at different selected areas of the third material.
- the second material components may comprise dopant materials, such as boron and phosphorous, that are implanted at selected areas.
- the first material component may for example be silicon and the boron and the phosphorous may be implanted at substrate areas selected so that on the substrate doped silicon having a p-n junction is formed.
- the method 10 has a variety of applications for forming many different types of devices.
- the second material component may be a plurality of different second material components which may be implanted in close proximity to one another so that different dopants may interact with each other. This may allow for the fabrication of optical centres comprising a combination of impurities such as Si/Ni, Cr/Al, Cr/O or other combinations.
- the rate of transportation or diffusion of the second material component is dependent on the properties of the second and third materials and the temperature at which the transportation or diffusion process occurs at. In the case of diffusion the rate of the diffusion is also dependent on the diffusion coefficient of atoms or ions in silica.
- an annealing process occurs after the diamond material 26 is grown in the microwave CVD reactor.
- the annealing process causes a stress relief in the diamond crystal as well as stabilizing the crucial structure of the centre.
- the ions or atoms 24 is transported or diffuse so as to be incorporated into at least some of the diamond material 26 thereby forming photon sources 28 as shown in Figure 2c.
- the ions or atoms 24 is transported or diffuse so as to be incorporated into at least some of the diamond material 26 thereby forming photon sources 28 as shown in Figure 2c.
- not all diamond material 26 has been incorporated with the nickel ions 24 to form the photon sources 28.
- the fabrication of the material may be accelerated in the following manner.
- the sample 20 may be moved to the proximity of a plasma of a microwave CVD reactor during growth of the first material component so as to etch the silica substrate 22 by the plasma.
- the silica substrate 22 is etched by the plasma, the nickel, atoms' or ions 24 are exposed to the plasma and subsequently to the diamond material 26 which promotes incorporation of the nickel atoms or ions 24 into the diamond material 26.
- a subsequent annealing process enhances °the vacancy diffusion and promotes the formation of optical centres.
- the annealing process can also relieve residual stress in the diamond material 26 caused during growth.
- IxIO 6 to IxIO 8 diamond crystals/cm 2 may be grown on the substrate 22.
- the crystal density depends on the initial nucleation density of the diamond seed.
- the ratio of implanted nickel atoms or ions to individual diamond crystals is approximately 100:1. This high ratio increases the probability of the incorporation of the nickel atoms or ions 24 into the diamond material 26. This high ratio, combined with the relatively large size of the nickel atoms or ions 24 compared to the carbon atoms that form the diamond material 26, improves the chances of forming single nickel related centres in the diamond material 26.
- an average of one to two diamond crystals containing an optical centre were detected within an area of lOO ⁇ m 2 .
- an average crystal density of IxIO 6 to IxIO 8 crystals/cm 2 as described above it is- estimated that approximately one in five diamond crystals will, on average, contain a single nickel related optical centre. This is an improvement in the formation probability of optically active centres in CVD diamonds over previously known methods .
- the substrate 22 is provided in the form of a core region of an end- face of an optical fibre, such as a cleaved optical fibre.
- the method 10 forms the material, such as a diamond material comprising an optical centre, directly on the core of the optical fibre in which emitted photons may be guided.
- the photon sources 28 and a diamond materials 26 that was fabricated by method 10 were subjected to photoluminescence (PL) measurements to obtain a PL spectra 30 shown in Figure 3.
- the PL measurements were conducted using a Renishaw RM 1000 Raman Stellar Pro 514 Modulaser (514nm excitation source) with 13mW power at the sample.
- the spectral lines 32, 34, 38 correspond to emission from individual diamond crystals each with a different nickel related optical centre.
- the spectral line 36 corresponds to a diamond material 26 that does not have a nickel related optical centre.
- Each spectrum 32, 34, 36, 38 shows a Raman peak 40 corresponding to a 552nm diamond Raman line.
- the spectral lines 32, 34, 38 each have a respective PL peak 42, 44, 48 which are attributed to different nickel related optical centres.
- the PL peaks 42, 44, 48 are narrow and most of the signal is concentrated in a zero phonon line which is preferable for quantum key distribution.
- the spectral lines 32, 34, 38 each only show a single characteristic PL peak meaning each photon source 28 that was subject to measurement only . contained a single nickel centre.
- the PL spectra 30 did not reveal any PL peaks . corresponding to nitrogen-vacancy or nickel-nitrogen optical centres. This is attributed to the method 10 not including a step involving the intentional introduction of nitrogen and the evacuation of an atmosphere surrounding the sample 20 to below 8xlO "4 Torr during method 10.
- the sample 20 was irradiated with a 30keV ion beam to introduce damage and vacancies into the photon sources 28. If a nitrogen-vacancy optical centre was present, this step would allow vacancy diffusion towards the nitrogen atom to occur which would enable activation of the nitrogen-vacancy optical centre. After the irradiation process, PL measurements were taken and PL peaks that would be attributed to nitrogen-vacancy optical centres were still not observed, showing that no nitrogen-vacancy optical centres existed in the photon source 28.
- the histogram of the time separation between successive photodetection events is equivalent to measuring the g 2 ( ⁇ ) function.
- Figure 4 shows a second order normalised autocorrelation function 56 from the diamond crystal that incorporates the nickel optical centre.
- Dots 58 represent experimental data and line 60 represents the simulation of the autocorrelation function g 2 ( ⁇ ) .
- the approximate lifetime of the nickel optical centre observed in the experiments was estimated to be approximately 3ns .
- Figure 5 shows the total counting rate 64 attributed to the nickel optical centre as a function of excitation power.
- an intensity line 66 There is shown an intensity line 66, a corrected intensity line 68 and a background intensity line 70, wherein the corrected intensity line 68 is the difference between the intensity line 66 and the background intensity line 70.
- the full saturation counting rate, R ⁇ , at the saturation power emission is estimated to be 200,000 counts/s. This is a higher rate than previously reported rates for different nickel-nitrogen optical centres observed in both bulk diamond crystal and CVD nano- diamonds .
- FIG. 6 (a) there is shown a PL spectrum 60 corresponding to emission from an individual diamond crystal that was prepared in accordance with a further embodiment of the present invention. It is postulated that the emission, centred at a wavelength of 756nm, is related to a chromium related optical centre.
- Figure 6 (b) shows a corresponding normalised autocorrelation function 62 and
- Figure 6 (c) shows a corresponding fluorescence intensity saturation curve.
- the data shown in Figure 6 were recorded using similar conditions and instrumentation as described above with reference to measurements taken from diamond crystallites having nickel related optical centres. The data were recorded at room temperature using a 682 nm excitation laser from individual diamond nano-crystals .
- the fluorescence intensity saturation graphs were recorded from the 756 nm single photon emitter as a function of excitation power.
- the circles 62 represent the background noise
- the squares 64 represent the raw data
- the triangles represent 66 the background corrected data.
- the solid line represents a fit.
- the following will describe how crystals exhibiting the properties illustrated in Figure 6 were prepared.
- the crystals were grown to an average size of few hundreds nanometers from diamond seeds (4-6 nm) on a sapphire substrate using a microwave plasma enhanced CVD technique (900 W, 150 Torr) at conditions similar to those described above .
- a microwave plasma enhanced CVD technique 900 W, 150 Torr
- the sapphire substrates contained a significant amount of Cr atoms ( ⁇ ppm) . This was confirmed by exciting the sapphire substrates with 514 nm excitation laser and the observation of strong luminescence at ⁇ 693/695 nm, attributed to Cr 3+ atoms in the sapphire lattice.
- the photon sources 28 have a variety of application.
- the photon sources 28 can be used in quantum cryptography and spintronics applications amongst others.
- the photon sources 28 can be used as biomarkers .
- the diamond material is inert and therefore will not cause harm to biological tissue when introduced into an organism.
- nickel or chromium optical centres are incorporated into diamond, is particularly beneficial as the wavelength emitted by the nickel or chromium related optical centre can penetrate tissue without causing damage.
- the photons emitted, with a wavelength of between approximately 750-900nm can then be observed outside the organism so that the location of the photon source 28 can be detected without the need for invasive techniques.
- the second material component may not necessarily comprise chromium or nickel atoms or ions, but may alternatively comprise ions or atoms of any other suitable material.
- the substrate may comprise any material suitable for the formation of substrates.
- the first material component may be any suitable material that is capable of incorporating the second material component.
- the substrate may not necessarily be prepared by implanting the second material component into the third material.
- the substrate may alternatively comprise a multi- layered structure having a layer of the second material component positioned below a thin layer of the third material at a surface of the substrate, or may comprise the second material, for example Cr that has grown in sapphire .
- selecting at least one area of the third material component for incorporation of the first material may comprise masking a surface portion of the third material.
- a further step of ion implantation by known means may occur wherein more of the second component material is implanted into the first component material, before the annealing process described above. This may offer the advantage of enhancing emissions from the material.
Abstract
The present disclosure provides a method of fabricating a material. The material comprises first and second material components. The method comprises the steps of providing a source of a first material component. Further, the method comprises providing a substrate comprising a second component material in which a third material component is incorporated in a manner such that a surface of the substrate is at least partially composed of the third material component. The second material component is located in the proximity of the surface of the substrate. The method also comprises fabricating the material on the surface by forming the first material component on the substrate and transporting the second material from the substrate to a location at which the material is fabricated so that the second material component is incorporated into the first material component.
Description
A METHOD OF FABRICATING A MATERIAL
Field of the Invention
The present invention broadly relates to a method of fabricating a material.
Background of the Invention
Quantum communication systems are optical data transmission systems that enable secure transmission of the data. Quantum communication relies on the principals of quantum mechanics and requires transmission of single photons in contrast to large number of photons that are transmitted using conventional optical data transmission systems. If the data is transmitted in the form of pulses from a single photon source, it can be verified if the data has been accessed and/or changed in any way by an unauthorised party.
Diamond crystals may be used for fabricating such single photon sources. Diamond crystals may contain optical centres that are arranged for emission of single photons. Such diamond crystals can be fabricated so that each diamond crystal only contains one optical centre and consequently each diamond crystal emits in use single photons. The optical centres comprise impurities that result in specific defects in the matrix of the diamond crystals and may for example comprise a nitrogen-vacancy optical centre or an optical centre that includes nitrogen and a metallic impurity or a vacancy and a metallic impurity.
Diamond crystals having such optical centres may be fabricated using chemical vapour deposition (CVD) . The fabrication of diamond crystals having nitrogen-vacancy optical centres is less challenging than the fabrication of diamond crystals having optical centres optical centres that include metals, such as nickel. However, diamond crystals that include metals, such as nickel, have optical advantages for a number of applications .
The present invention provides technological advancement.
Summary of the Invention
The present invention provides in a first aspect a method of fabricating a material comprising first and second material components, the method comprising the steps of: providing a source of a first material component; providing a substrate comprising a third material component into which the second material component is incorporated in a manner such that a surface of the substrate is at least partially composed of the third material component and wherein the second material component is located in the proximity of the surface of the substrate; and fabricating the material on the substrate by forming the first material component on the substrate and transporting the second material component from the substrate to a location at which the material is fabricated so that the second material component is incorporated into the first material component.
The step of providing the substrate typically comprises forming the substrate by incorporating the second
component material into the third material component . The method typically is conducted so that, typically during formation of a portion of the first material component on the substrate, at least a portion of the second material component diffuses to a location of the first material component. Diffusion may comprise solid state diffusion or gas phase diffusion or a combination of solid state and gas phase diffusion.
As the second material component typically is incorporated during formation of a portion of the first material component, the incorporation usually occurs with less structural defects than incorporation for example by direct ion implantation into the first material. Incorporating the second material during formation of a portion of the first material component may also lead to a different charge state for the second material component and therefore a different optical response of the material compared to, for example, a material formed by direct ion implantation into the first material.
The step of forming the substrate typically comprises incorporating the second material component into a depth of 10-50nm below a surface of the third material.
Incorporating the second material component into the third material component typically comprises implanting the . second material component into the third material component. Further, the step of forming the substrate typically comprises selecting at least one area of the surface of the third material component for incorporating the second material component so that, during fabrication of the material, the second material component is
predominantly or solely incorporated into the first material component at the at least one selected area. The at least one selected area may have any size and may also be a relatively small area having a diameter of the order of 50 - 500 nm, such as 50 - lOOnm. Further, the selected area may be one of a plurality of selected areas and the selected area may also comprise a pattern.
A local density of the second material component incorporated into the first material component may be controlled by controlling growth conditions and thereby controlling transportation of the second material component .
The step of providing a source of the first material component typically comprises chemical vapour deposition (CVD) . The second material component typically is incorporated into the first material component by a solid state or gas diffusion process during formation of the first material component.
The method typically is conduced so that at least one optical centre is formed in the material. Further, the method typically comprises controlling a number of optical centres in the formed material by controlling at least one growth parameter.
In one specific example the first material component is diamond, the second material component comprises atoms or ions of a metallic material, such as nickel ions, and the third material component is silica or the like. In this case the substrate may be formed by implanting the second material component into the silica at a selected area,
such as a relatively small area having a diameter smaller than a typical diameter of the formed material. Formation of the diamond on the substrate may be conducted so that diamond crystallites form on the substrate having a diameter of the order of 10 to 500 nm, 30 - 300nm, 40 - 200nm and typically 50 - lOOnm. If the nickel ions are implanted predominantly into one area that has a diameter that is smaller or in the order of the magnitude of a typical diamond crystal, it is likely that the formation of nickel related optical centres in the diamond crystal is limited to only one diamond crystal. Consequently, the controlled formation of a single photon source is facilitated. Further, a number of formed nickel related centres in the diamond material may be controlled by controlling growth conditions and thereby controlling the transportation of the nickel ions into the diamond material, which further facilitates the formation of a single photon source having one or nickel related optical centre .
Alternatively, the second material component comprises atoms or ions of a metallic material, such as chromium ions, and the . third material component is sapphire including chromium impurities. Formation of the diamond on the substrate may be conducted so that diamond crystallites form on the substrate having a diameter of the order of 10 to 500 nm, 30 - 300nm, 40 - 200nm and ■ typically 50 - lOOnm. A number of formed chromium related centres in the diamond material may be controlled by controlling growth conditions and thereby controlling the transportation of the chromium ions into the diamond material .
Embodiments of the present invention provide the advantage that the second material component may be incorporated into the first material component without the need to provide the second material component in a gas phase. This has the further practical advantage that contamination of an interior of a growth chamber by the second material component can be substantially avoided.
The method typically comprises controlling a density of optical centres in the formed material by controlling at least one growth parameter.
In a variation of the above-described specific example the method comprises selecting a plurality of areas of the third material at which the second material component will be located. For example, the method may be conducted so that the second material component is implanted into a plurality of areas of the third material, each of which may have the above-described extension. The areas at which the second material component will be located may for example form an array. The material components and the areas may be arranged so that a plurality of single photon sources are formed, such as an array comprising diamond crystals each having a single chromium or nickel related optical centre.,
It is to be appreciated that the second material component may not necessarily comprise chromium or nickel ions, but may alternatively comprise any other suitable atoms or ions and typically comprises atoms or ions of a metallic material, such as Ni, Li, Be, B, Al, P, S Co, Ni, Zn, As, Sb or Ir.
Further, the third material component may not necessarily be silica or sapphire, but may be any other suitable material. In addition, the first material component may not necessarily be diamond, but may also be any other suitable material in which the second material component may be incorporated.
The method may comprise incorporating a plurality of second component materials into the third component material. For example, the first material component may be diamond into which two or more different metallic material components are incorporated, or 'into which metallic and non-metallic components are incorporated. This may allow for the fabrication of optical centres comprising a combination of impurities such as Si/Ni, Cr/Al, Cr/O or other combinations .
The method may further comprise selecting a concentration of the at least one second material component in the first material component by controlling a concentration at which the at least one second material component is incorporated in the third material prior to formation of the material.
The step of forming the material may comprise positioning the substrate near a plasma in a CVD reactor so that the substrate is etched by the plasma whereby at least a portion of the second material component is exposed to the plasma to facilitate diffusion and subsequent incorporation of the second material component into the first material component.
It is to be appreciated that the method in accordance with the first aspect of the present invention has a number, of
applications in many fields of science and technology. For example, the method may be used to form materials, such as diamond crystallites, having any number of optical centres and applications.
The present invention provides in a second aspect a single photon source formed by the method in accordance with the first aspect of the present invention.
The present invention provides in a third aspect a biomarker formed by the method in accordance with the first aspect of the present invention.
The biomarker typically is one of a plurality of biomarkers that may be fabricated simultaneously.
In one specific example the biomarker comprises a diamond crystal having one or more nickel or chromium related optical centres. Diamond is largely inert and consequently has no adverse effect on tissue, such as human tissue. Further, the nickel for example nickel related optical centres emit in use photons at a wavelength of approximately 750nm - 900nm and the tissue is largely transparent at that wavelength. Consequently, such diamond crystals have properties that make the diamond crystals suitable for use as biomarkers.
The present invention provides in a fourth aspect a biomarker, the biomarker comprising diamond, the diamond incorporating at least one optical centre arranged for the emission of photons have a wavelength in the range of 700- lOOOnm.
The diamond typically comprises at least one chromium
related optical centre that typically is arranged for emission of photons at a wavelength of approximately 750 - 900nm.
The invention will be more fully understood from the following description of specific embodiments of the invention. The description is provided with reference to the accompanying drawings .
Brief Description of the Drawings
Figure 1 shows a flow chart of a method of fabricating a material according to a first specific embodiment of the present invention;
Figures 2 (a) - (c) illustrate steps of the method of fabricating a material according to the first specific embodiment of the present invention;
Figure 3 shows a graph of photoluminescence spectra attributed to the material fabricated by the method according to the specific embodiment of the present invention;
Figure 4 shows a normalised autocorrelation function of the material fabricated by the method according to the specific embodiment of the present invention;
Figure 5 shows graph of a counting rate recorded from the material fabricated by the method according to the specific embodiment of the present invention; and
Figure 6 shows (a) a photoluminescence spectrum, (b)
a normalised autocorrelation function and (c) fluorescence intensity saturation graphs for a material fabricated by a method according to a further specific embodiment of the present invention.
Detailed Description of Specific Embodiments
Embodiments of the present invention generally relate to a method of fabricating a material. The material includes a first material component and a second material component that is incorporated into the first material component. In one example the method comprises initially incorporating the second material component into a third material component, which then forms a substrate on which the material is fabricated. The second material component typically is located in the proximity of the surface of the substrate. The fabrication of the material typically is conducted so that at least a portion of the second material component is incorporated into the first material component by a solid state or gas diffusion process during growth of the material .
Referring initially to Figure 1 and Figures 2 (a) - 2 (d) , a method of fabricating a material in accordance with a first specific embodiment of the present invention is now described. Figure 1 illustrates a method 10 of fabricating photon sources. The photon sources include in this example a diamond material which incorporates nickel in the form of a nickel related optical centre.
The first step 12 of the method 10 comprises incorporating a second material component into a third material . In this example, the second material component comprises nickel
ions or atoms and the third material is provided in the form of a silica substrate. Ions of the nickel are implanted into the silica substrate and the implanted nickel ions or atoms are dispersed in the proximity of the surface of the silica without forming larger clusters that have metallic properties.
Figures 2a to 2c further illustrate the method 10. Figure 2a shows a sample 20 comprising a silica substrate 22 having nickel ions 24 implanted below a surface of the silica substrate 22. The implantation of the nickel ions 24 was conducted by exposing the silica substrate 22 to a beam of nickel ions having an energy of the order of 20keV to 30keV.
The direction of acceleration of the nickel ions 24 is indicated by arrows shown in Figure 2a. The energies of 20keV and 30keV cause implantation of the nickel ions 24 to a depth of approximately 20nm to 30 nm below the surface of the silica substrate 22. Doses of between 1010 and 1012 ions/cm2 of nickel ions are implanted into the silica substrate 22
A second step 14 of the method 10 forms the first material component on the surface of the substrate. In this example, the first material component is a diamond material 26 which is grown on the silica substrate 22. To achieve this, the sample 20, now comprising the silica substrate 22 which contains the implanted nickel ions 24, is transferred to a microwave chemical vapour deposition (CVD) reactor. The diamond material 26 shown in Figure 2b is then grown on the upper surface of the silica substrate 22 from nano-diamond seeds using a microwave plasma
technique. At the same time at least a portion of the second material component is incorporated into the first material component (step 16 of method 10) . In this example, during the growing of the diamond material 26, the nickel ions 24 are transported, for example by- diffusion, into the diamond material 26. This is illustrated in Figure 2b where arrows indicate the transportation of the nickel ions 24 into the diamond material 26. This transportation process may also continue to occur when the sample 20 is annealed.
Further, the method 10 may comprise selecting at least, one area of the surface of the substrate 22 prior to implanting the nickel ions 24 into the substrate 22. The at least one selected area may have any size and may also be a relatively small area having a diameter of the order within the range of 50 - lOOnm. The nickel ion beam is then focused onto the selected area so that the nickel ions are implanted predominantly in the selected area.
Alternatively, the Ni ions can be implanted into the substrate through a mask. Further, a plurality of areas may be selected and the selected area may also form a pattern. For fabrication of one single photon source typically nickel ions are predominantly implanted into one area having an extension that is smaller that a typical extension of a diamond crystal. Consequently, it is likely that a nickel -related centre is formed in one diamond • crystal only. Alternatively, a plurality of areas may be selected for implantation so that a plurality of single photons sources may be formed, such as an array of single photon sources .
Further, the second material component may be one of two or more different second material components which may be implanted at different selected areas of the third material. For example, the second material components may comprise dopant materials, such as boron and phosphorous, that are implanted at selected areas. In this case the first material component may for example be silicon and the boron and the phosphorous may be implanted at substrate areas selected so that on the substrate doped silicon having a p-n junction is formed. It is to be appreciated that the method 10 has a variety of applications for forming many different types of devices. Alternatively, the second material component may be a plurality of different second material components which may be implanted in close proximity to one another so that different dopants may interact with each other. This may allow for the fabrication of optical centres comprising a combination of impurities such as Si/Ni, Cr/Al, Cr/O or other combinations.
The rate of transportation or diffusion of the second material component is dependent on the properties of the second and third materials and the temperature at which the transportation or diffusion process occurs at. In the case of diffusion the rate of the diffusion is also dependent on the diffusion coefficient of atoms or ions in silica.
In this example, an annealing process occurs after the diamond material 26 is grown in the microwave CVD reactor. The sample 20, now comprising the silica substrate 22 with the diamond material 26 grown thereon, undergoes an annealing process conducted at a temperature of 10000C in a
forming gas comprising 95% Ar and 5% H2. The annealing process causes a stress relief in the diamond crystal as well as stabilizing the crucial structure of the centre.
During the CVD growth process and/or the annealing process, the ions or atoms 24 is transported or diffuse so as to be incorporated into at least some of the diamond material 26 thereby forming photon sources 28 as shown in Figure 2c. In this particular example, not all diamond material 26 has been incorporated with the nickel ions 24 to form the photon sources 28.
The fabrication of the material may be accelerated in the following manner. The sample 20 may be moved to the proximity of a plasma of a microwave CVD reactor during growth of the first material component so as to etch the silica substrate 22 by the plasma. When the silica substrate 22 is etched by the plasma, the nickel, atoms' or ions 24 are exposed to the plasma and subsequently to the diamond material 26 which promotes incorporation of the nickel atoms or ions 24 into the diamond material 26.
A subsequent annealing process enhances °the vacancy diffusion and promotes the formation of optical centres. The annealing process can also relieve residual stress in the diamond material 26 caused during growth.
For example IxIO6 to IxIO8 diamond crystals/cm2 may be grown on the substrate 22. The crystal density depends on the initial nucleation density of the diamond seed. The ratio of implanted nickel atoms or ions to individual diamond crystals is approximately 100:1. This high ratio increases the probability of the incorporation of the
nickel atoms or ions 24 into the diamond material 26. This high ratio, combined with the relatively large size of the nickel atoms or ions 24 compared to the carbon atoms that form the diamond material 26, improves the chances of forming single nickel related centres in the diamond material 26.
In the present example, an average of one to two diamond crystals containing an optical centre were detected within an area of lOOμm2. Combined with an average crystal density of IxIO6 to IxIO8 crystals/cm2 as described above it is- estimated that approximately one in five diamond crystals will, on average, contain a single nickel related optical centre. This is an improvement in the formation probability of optically active centres in CVD diamonds over previously known methods .
In one specific example the substrate 22 is provided in the form of a core region of an end- face of an optical fibre, such as a cleaved optical fibre. In this specific example the method 10 forms the material, such as a diamond material comprising an optical centre, directly on the core of the optical fibre in which emitted photons may be guided.
The photon sources 28 and a diamond materials 26 that was fabricated by method 10 were subjected to photoluminescence (PL) measurements to obtain a PL spectra 30 shown in Figure 3. The PL measurements were conducted using a Renishaw RM 1000 Raman Stellar Pro 514 Modulaser (514nm excitation source) with 13mW power at the sample.
Referring to Figure 3, there is shown the PL spectra 30.
The spectral lines 32, 34, 38 correspond to emission from individual diamond crystals each with a different nickel related optical centre. The spectral line 36 corresponds to a diamond material 26 that does not have a nickel related optical centre.
Each spectrum 32, 34, 36, 38 shows a Raman peak 40 corresponding to a 552nm diamond Raman line. The spectral lines 32, 34, 38 each have a respective PL peak 42, 44, 48 which are attributed to different nickel related optical centres. The PL peaks 42, 44, 48 are narrow and most of the signal is concentrated in a zero phonon line which is preferable for quantum key distribution. The spectral lines 32, 34, 38 each only show a single characteristic PL peak meaning each photon source 28 that was subject to measurement only. contained a single nickel centre.
The PL spectra 30 did not reveal any PL peaks . corresponding to nitrogen-vacancy or nickel-nitrogen optical centres. This is attributed to the method 10 not including a step involving the intentional introduction of nitrogen and the evacuation of an atmosphere surrounding the sample 20 to below 8xlO"4 Torr during method 10.
In a separate test conducted after completing method 10, the sample 20 was irradiated with a 30keV ion beam to introduce damage and vacancies into the photon sources 28. If a nitrogen-vacancy optical centre was present, this step would allow vacancy diffusion towards the nitrogen atom to occur which would enable activation of the nitrogen-vacancy optical centre. After the irradiation process, PL measurements were taken and PL peaks that would be attributed to nitrogen-vacancy optical centres
were still not observed, showing that no nitrogen-vacancy optical centres existed in the photon source 28.
It can be assumed then that the optical centres in the photon sources 28 were related only to nickel ions or atoms 24 and not to various nickel-nitrogen complexes..
Antibunching experiments were also taken of the photon sources 28 using continuos excitation (cw) 687nm diode laser with a 780nm long pass filter implementing a Hanbury Brown and Twiss (HBT) interferometer setup which consisted of two avalanche photodiodes and a beamosplitter .
Photon statistics of the photon sources 28 were studied by measuring the autocorrelation function:
[I(t)I(t+τ)] g2d) = [Kt)]2
using the HBT interferometer. For the conditions and short time scale of the measurements, the histogram of the time separation between successive photodetection events is equivalent to measuring the g2(τ) function.
Figure 4 shows a second order normalised autocorrelation function 56 from the diamond crystal that incorporates the nickel optical centre. Dots 58 represent experimental data and line 60 represents the simulation of the autocorrelation function g2(τ) . A dip 62 at zero delay time corresponds to g2(0) = 0.08 which shows that the observed nickel optical centre is a single photon emitter. The approximate lifetime of the nickel optical centre observed
in the experiments was estimated to be approximately 3ns . At least 70% of diamond crystals that were scanned showed a dip 62 of at least 50% at τ = 0.
Figure 5 shows the total counting rate 64 attributed to the nickel optical centre as a function of excitation power. There is shown an intensity line 66, a corrected intensity line 68 and a background intensity line 70, wherein the corrected intensity line 68 is the difference between the intensity line 66 and the background intensity line 70. The full saturation counting rate, R∞, at the saturation power emission is estimated to be 200,000 counts/s. This is a higher rate than previously reported rates for different nickel-nitrogen optical centres observed in both bulk diamond crystal and CVD nano- diamonds .
Referring now to Figure 6 (a) , there is shown a PL spectrum 60 corresponding to emission from an individual diamond crystal that was prepared in accordance with a further embodiment of the present invention. It is postulated that the emission, centred at a wavelength of 756nm, is related to a chromium related optical centre. Figure 6 (b) shows a corresponding normalised autocorrelation function 62 and Figure 6 (c) shows a corresponding fluorescence intensity saturation curve. The data shown in Figure 6 were recorded using similar conditions and instrumentation as described above with reference to measurements taken from diamond crystallites having nickel related optical centres. The data were recorded at room temperature using a 682 nm excitation laser from individual diamond nano-crystals . Only a 794+80 nm band-pass filter was used for the PL measurements while
an additional 760^12 nm band pass filter was used for coincidence measurements . An absence of bunching of the g<2> (τ) function at saturation was observed. The integration time was 300 s with a coincidence time bin of 154 ps .
The fluorescence intensity saturation graphs were recorded from the 756 nm single photon emitter as a function of excitation power. The circles 62 represent the background noise, the squares 64 represent the raw data, the triangles represent 66 the background corrected data. The solid line represents a fit.
The following will describe how crystals exhibiting the properties illustrated in Figure 6 were prepared. The crystals were grown to an average size of few hundreds nanometers from diamond seeds (4-6 nm) on a sapphire substrate using a microwave plasma enhanced CVD technique (900 W, 150 Torr) at conditions similar to those described above .
The sapphire substrates contained a significant amount of Cr atoms (~ppm) . This was confirmed by exciting the sapphire substrates with 514 nm excitation laser and the observation of strong luminescence at ~ 693/695 nm, attributed to Cr3+ atoms in the sapphire lattice.
Furthermore, it is known that Cr related centers in diamond exhibit narrow PL lines in the region of 740-770 nm. Crystal growth conditions of high pressure plasma (150 Torr) lead to considerable etching of the substrate making it more likely that the substrate material will be incorporated into the growing crystals. Control PL studies of the diamond nano-crystals grown on silica did not reveal the PL line shown in Figure 6 (a) .
The photon sources 28 have a variety of application. The photon sources 28 can be used in quantum cryptography and spintronics applications amongst others. In addition, the photon sources 28 can be used as biomarkers . The diamond material is inert and therefore will not cause harm to biological tissue when introduced into an organism. The specific embodiment described above, wherein nickel or chromium optical centres are incorporated into diamond, is particularly beneficial as the wavelength emitted by the nickel or chromium related optical centre can penetrate tissue without causing damage. The photons emitted, with a wavelength of between approximately 750-900nm can then be observed outside the organism so that the location of the photon source 28 can be detected without the need for invasive techniques.
Although the invention has been described with reference to particular examples, it will be appreciated by those skilled in the art that the invention may be embodied in many other forms. For example, the second material component may not necessarily comprise chromium or nickel atoms or ions, but may alternatively comprise ions or atoms of any other suitable material. There may also be a plurality of second material components, for example two or more different metallic material components, or metallic and non-metallic material components. The substrate may comprise any material suitable for the formation of substrates. The first material component may be any suitable material that is capable of incorporating the second material component.
Further, the substrate may not necessarily be prepared by implanting the second material component into the third material. For example, the substrate may alternatively
comprise a multi- layered structure having a layer of the second material component positioned below a thin layer of the third material at a surface of the substrate, or may comprise the second material, for example Cr that has grown in sapphire .
In addition, the selecting at least one area of the third material component for incorporation of the first material may comprise masking a surface portion of the third material.
Further, after forming the first material component in the substrate and incorporating at least a portion of the second component material into the first component material, a further step of ion implantation by known means may occur wherein more of the second component material is implanted into the first component material, before the annealing process described above. This may offer the advantage of enhancing emissions from the material.
Claims
1. A method of fabricating a material comprising first and second material components, the method comprising the steps of: providing a source of a first material component; providing a substrate comprising a third material component into which the second material component is incorporated in a manner such that a surface of the substrate is at least partially composed of the third material component and wherein the second material component is located in the proximity of the surface of the substrate; and fabricating the material on the substrate by forming the first material component on the substrate and transporting the second material component from the substrate to a location at which the material is fabricated so that the second material component is incorporated into the first material component.
2. The method of claim 1 wherein the step of providing the substrate comprises forming the substrate by incorporating the second component material into the third material component .
3. The method of claim 1 or 2 wherein the method is conducted so that, during formation of a portion of the first material component on the substrate, at least a portion of the second material component diffuses to a location of the first material component.
4. The method of claim 2 or claim 3 when dependent on claim 2 wherein the step of forming the substrate comprises selecting at least one area of the surface of the third material component for incorporating the second material component so that, during formation of the first material component, the second material component is predominantly incorporated into the first material component at the at least one selected area.
5. The method of any one of the preceding claims comprising implanting the second material component into the third material component.
6. The method of any one of the preceding claims wherein a local density of the second material component incorporated into the first material component is controlled by controlling growth conditions and thereby controlling the transportation of the second material component .
7. The method of any one of the preceding claims wherein the step of providing a source for the first component comprises providing a chemical vapour deposition (CVD) source.
8. The method of any one of the preceding claims wherein the first material component is diamond.
9. The method of any one of the preceding claims wherein the second material component comprises ions or atoms of a metallic material.
10. The method of any one of the preceding claims wherein the second material component comprises chromium ions or atoms .
11. The method of any one of claims 1 to 9 wherein the second material component comprises nickel ions or atoms .
12. The method of any one of the preceding claims wherein the method is conduced so that at least one optical centre is formed in the material.
13. The method of any one of the preceding claims comprising controlling a density of optical centres in the formed material by controlling at least one growth parameter.
14. The method of any one of the preceding claims wherein a plurality of second material components are incorporated into the third material component.
15. The method of claim 14 wherein the plurality of second material components comprise at least two different second material components.
16. The method of any one of the preceding claims further comprising selecting a concentration of the second material component in the first material component by controlling a concentration at which the second material component is incorporated in the substrate prior to formation of the material.
17. The method of any one of the preceding claims further comprising the step of implanting more of the second material component into the material after at least a portion of the material has been fabricated.
18. The method of claim 17 wherein the second material component is implanted by ion implantation.
19. The method of any one of the preceding claims comprising the further step of annealing the material.
20. A single photon source formed by the method of any one of claims 1 to 15.
21. A biomarker formed by the method of any one of claims 1 to 15.
22. A biomarker, the biomarker comprising diamond, the diamond incorporating at least one optical centre arranged for the emission of photons have a wavelength in the range of 700-lOOOnm.
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