CN103885010A - SQUID sealing cavity system for magnetic and electrical property synchronous measurement - Google Patents
SQUID sealing cavity system for magnetic and electrical property synchronous measurement Download PDFInfo
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- CN103885010A CN103885010A CN201410157558.0A CN201410157558A CN103885010A CN 103885010 A CN103885010 A CN 103885010A CN 201410157558 A CN201410157558 A CN 201410157558A CN 103885010 A CN103885010 A CN 103885010A
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Abstract
The invention provides an SQUID sealing cavity system for magnetic and electrical property synchronous measurement. The SQUID sealing cavity system comprises a sample cavity, a sample rod, a conveying table and a sealing column-shaped body. The sample rod extends into the sample cavity. A sample to be tested is fixed on a sample support at the lower section of the sample rod. The conveying table is in sealing connection with the sample cavity. The sealing column-shaped body comprises a column-shaped body inner cylinder with openings in the two sides, a column-shaped body outer cylinder with an opening in one side and a quick connector. The lower side of the column-shaped body inner cylinder is fixed on the conveying table. The lower side of the column-shaped body outer cylinder is provided with the opening, the column-shaped body outer cylinder is connected to the outer side of the column-shaped body inner cylinder in a sleeved mode, the column-shaped body outer cylinder and the column-shaped body inner cylinder are sealed by squeezing an O-shaped rubber sealing ring, and a hole is formed in the upper portion of the column-shaped body outer cylinder. The quick connector is fixed at the hole in a sealing mode in the upper portion of the column-shaped body outer cylinder. The quick connector is provided with a plurality of conducting pins. A lead wire is guided out from a corresponding testing point of the sample to be tested, and the lead wire is guided out form the sample cavity through the conducting pins on the quick connector. Connecting of the lead wire in the sample cavity of the SQUID sealing cavity system is achieved, and magnetic and electrical property synchronous measurement can be well achieved.
Description
Technical field
The present invention relates to high precision magnetic moment and electric signal measurement technology on low temperature high-intensity magnetic field platform, relate in particular to a kind of SQUID annular seal space system for magnetics and electrical properties synchro measure.
Background technology
Along with deepening continuously of Semiconductor Spintronics research, the testing apparatus functional requirement of spin correlation physical property in semiconductor spin-electronic material and related device structure is also constantly being improved.Magnetic property measuring system (the MPMS of Quantum Design company based superconductive quantum inteferometer (SQUID), Magnetic Property Measurement System) be universally acknowledged top measuring table, have very high magnetic moment measurement precision (～10-8emu), the magnetic property to magnetic semiconductor sample (magnetic signal is only 10-7～10-5emu conventionally) characterizes well.But along with the development of Semiconductor Spintronics research, simple electricity and magnetics discrete testing can not meet the demand of further investigation, the magnetics based on SQUID-MPMS and electrical properties method for synchronously measuring for exploring semiconductor spin-electronic material that high-quality can be practical, regulate and control its electron spin degree of freedom and development related semiconductor spin electric device is particularly important.
Fig. 1 is the structural representation of annular seal space system in prior art superconducting quantum interference device (SQUID).As shown in Figure 1, sealing chamber system comprises: closed chamber 10, band to band transfer module 20, superconducting magnet 30, cylindrical sample chamber 40 and specimen holder 60.Wherein, the main part of specimen holder 60 (61 and 63) stretches in cylindrical sample chamber 40, and its hypomere 63 is provided for the nonmagnetic sample carrier of fixing testing sample 50, and its epimere 62 has groove.Band to band transfer module 20 is positioned at the top of specimen holder 60, and its correspondence position at specimen holder epimere 62 grooves has clip 21.This clip 21 clamps the groove of specimen holder epimere, drives specimen holder 60 to move up and down in cylindrical sample chamber 40.Superconducting magnet 30 is positioned at the left and right sides in cylindrical sample chamber.Specimen holder 60, cylindrical sample chamber 40 and superconducting magnet 30 are positioned at Dewar system 10.
Fig. 2 is the schematic diagram of band to band transfer module end sealing in annular seal space system described in Fig. 1.As shown in Figure 2, the plexiglas right cylinder 22 of the fixing hollow of band to band transfer module 20 end sealings.Plastic seal plug 23 clogs the opening part of plexiglas right cylinder 22.In order to realize positiver sealing, plexiglas cylindrical hollow portion has groove, and O type rubber seal 24 is set in this groove, and this O type rubber seal 24 closely cooperates with the plastic seal plug 23 of inner side.
Fig. 3 is the schematic diagram of acquisition of signal in the SQUID annular seal space system of magnetics and electrical properties synchro measure.Please refer to Fig. 3, in SQUID annular seal space system, the magnetic signal of testing sample 50 is gathered by electromagnetic induction principle by the magnetic signal detecting coil 70 that is positioned at 40 outsides, cylindrical sample chamber, need to be by the interior wire that arranges in cylindrical sample chamber 40; And the electric signal of testing sample 50 need to be by wire 80 by being transferred to outside in cylindrical sample chamber 40.In this case, conventional SQUID annular seal space systems face the problem of following several respects:
(1) high precision Magnetic Measurement requires high temperature stability and magnetic field homogeneity, and to be therefore designed to internal diameter be only the cylindrical sample chamber of 9mm to the sample cavity of SQUID magnetometer, and the exercisable space of lead-in conductor is very little;
(2) in order to prevent the magnetic background signal of the oxygen introducing with higher paramagnetic susceptibility, must guarantee the sealing in cylindrical sample chamber;
(3), in order to reduce the impact of background magnetic signal as far as possible, require sample carrier evenly elongated and be diamagnetism, and sample to be positioned near the centre position of sample carrier.Therefore the nonmagnetic plastic suction pipe that, original system is used is not easy to be welded with the packing into of sample of wire very much.
Summary of the invention
(1) technical matters that will solve
In view of above-mentioned technical matters, the invention provides a kind of SQUID annular seal space system for magnetics and electrical properties synchro measure.
(2) technical scheme
The present invention comprises for the SQUID annular seal space system of magnetics and electrical properties synchro measure: Dewar system 10; Cylindrical shape sample cavity 40, is positioned at this Dewar system 10; Specimen holder 60, its stage casing 61 and hypomere 63 stretch in cylindrical shape sample cavity 40, and testing sample 50 is fixed on the sample carrier of specimen holder hypomere 63, and band to band transfer module 20 is arranged at the top of Dewar system 10, is connected side opening on it with sample cavity 40 is airtight; Seal column, be fixed on the top of band to band transfer module 20, comprising: the column inner core 25 of both-side opening, its downside is sealingly fastened in band to band transfer module 20; The column urceolus 26 of one-sided opening, its open lower side, the outside of socket and column inner core 25, and realize sealing by extruding O type rubber seal 27 between the two, the top of this column urceolus offers the threaded circular hole of tool; Quick union 28, is sealingly fastened in the circular hole of column urceolus 26 tops by O type rubber seal 29, this quick union has several conductive pins 28a; Wherein, wire 80 is drawn by the corresponding test point of testing sample, fixing on specimen holder 60, and by the conductive pin on quick union by drawing in cylindrical shape sample cavity 40.
(3) beneficial effect
Can find out from technique scheme, the present invention has following beneficial effect for the SQUID annular seal space system of magnetics and electrical properties synchro measure:
(1) designed the inside and outside cylindrical drum of plexiglas, both are by O type rubber seal rings for seal; Process threaded hole on urceolus top again, for sealing the fixing of quick union, both are also by extruding O type rubber seal rings for seal, thereby realize the introducing of wire, the design of inside and outside circle column casing has facilitated the connection between specimen holder top wire and quick union, has overcome the difficulty of narrow space.
(2) substitute nonmagnetic plastic suction pipe as sample carrier with non-magnetic long narrow silicon strip, facilitated the installation of the sample that is welded with wire, simultaneously therefore obtained more stable magnetics signal because silicon strip is not yielding in motion process.
Accompanying drawing explanation
Fig. 1 is the structural representation of annular seal space system in prior art superconducting quantum interference device (SQUID);
Fig. 2 is the schematic diagram of band to band transfer module end sealing in annular seal space system described in Fig. 1;
Fig. 3 is the schematic diagram of acquisition of signal and transmission in the SQUID annular seal space system of magnetics and electrical properties synchro measure;
Fig. 4 is the structural representation for the SQUID annular seal space system top of magnetics and electrical properties synchro measure according to the embodiment of the present invention;
Fig. 5 A is according to the structural representation of specimen holder leading portion in embodiment of the present invention SQUID annular seal space system;
Fig. 5 B is according to the structural representation of specimen holder back segment in embodiment of the present invention SQUID annular seal space system;
Fig. 6 is the curve map that uses the present embodiment SQUID annular seal space system to carry out the measurement of dilute magnetic semiconductor material magnetic property;
Fig. 7 utilizes the present embodiment SQUID annular seal space system to carry out the curve map of dilute magnetic semiconductor material magnetics and electric property synchro measure.
[component symbol explanation]
10-closed chamber; 30-superconducting magnet;
40-cylindrical sample chamber; 50-testing sample;
70-magnetic signal detecting coil; 80-wire;
20-band to band transfer module;
21-clip; 22-plexiglas right cylinder;
23-plastic seal plug; 24-O type rubber seal;
25-column inner core; 26-column urceolus;
27-O type rubber seal; 28-quick union;
28a-conductive pin; 29-O type rubber seal.
60-specimen holder;
61-specimen holder stage casing; 62-specimen holder epimere;
63-specimen holder hypomere; 64-groove;
65-O type rubber seal.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.It should be noted that, in accompanying drawing or instructions description, similar or identical part is all used identical figure number.The implementation that does not illustrate in accompanying drawing or describe is form known to a person of ordinary skill in the art in affiliated technical field.In addition, although the demonstration of the parameter that comprises particular value can be provided herein, should be appreciated that, parameter is without definitely equaling corresponding value, but can in acceptable error margin or design constraint, be similar to corresponding value.The direction term of mentioning in embodiment, for example " on ", D score, 'fornt', 'back', " left side ", " right side " etc., be only the direction with reference to accompanying drawing.Therefore, the direction term of use is to be not used for limiting the scope of the invention for explanation.
The invention provides a kind of SQUID annular seal space system for magnetics and electrical properties synchro measure.This SQUID annular seal space system has realized the introducing of vacuum condition lower wire.Wire extends to specimen holder end by being wound around specimen holder, and specimen holder end, has facilitated the installation of the sample that is welded with wire and fixed as sample carrier with silicon strip, does not destroy the high precision magnetic measurement of original SQUID system simultaneously.
In one exemplary embodiment of the present invention, provide a kind of SQUID annular seal space system for magnetics and electrical properties synchro measure.Fig. 4 is the structural representation for the SQUID annular seal space system top of magnetics and electrical properties synchro measure according to the embodiment of the present invention.Please refer to Fig. 1 and Fig. 4, the present embodiment specimen holder parts comprise: Dewar system 10; Cylindrical shape sample cavity 40, is positioned at this Dewar system 10; Specimen holder 60, its stage casing 61 and hypomere 63 stretch in cylindrical shape sample cavity 40, and testing sample 50 is fixed on the sample carrier of specimen holder hypomere 63, and band to band transfer module 20 is arranged at the top of Dewar system 10, is connected side opening on it with sample cavity 40 is airtight; Seal column, be fixed on the top of band to band transfer module 20, comprising: the column inner core 25 of both-side opening, its downside is sealingly fastened in band to band transfer module 20; The column urceolus 26 of one-sided opening, its open lower side, the outside of socket and column inner core 25, and realize sealing by extruding O type rubber seal 27 between the two, the top of this column urceolus offers the threaded circular hole of tool; Quick union 28, is sealingly fastened in the circular hole of column urceolus 26 tops by O type rubber seal 29, this quick union has several conductive pins 28a; Wherein, wire 80 is drawn by the corresponding test point of testing sample, fixing on specimen holder 60, and by the conductive pin on quick union by drawing in cylindrical shape sample cavity 40.
Below respectively the present embodiment is elaborated for each ingredient of the SQUID annular seal space system of magnetics and electrical properties synchro measure.
Sealing column is prepared by plexiglas material.Wherein, column inner core 25 and urceolus 26, both can separate and be socketed, and when socket, realize sealing by extruding O type rubber seal 27.
Top in column urceolus 26, offers the female circular hole of tool, has the fixing of externally threaded quick union 28 for periphery.In addition, between column urceolus 26 and quick union 28, press and put the 29 realization sealings of O type rubber seal.
In the time that this SQUID annular seal space system is used, column inner core 25 is fixed on band to band transfer module top, and 26 of column urceolus can be dismantled, and are very easy to the installation of specimen holder.Owing to having realized positiver sealing by rubber ring between column inner core 25 and column urceolus 26, thereby can prevent that oxygen that air particularly has a huge paramagnetic susceptibility from entering Dewar system 10 and affecting the measurement of magnetic signal.
In the present embodiment, specimen holder 60 is made by non-magnetic carbon fiber, and length is about 1.1 meters, is divided into stage casing 61, epimere 62 and hypomere 63.Fig. 5 A is according to the structural representation of specimen holder hypomere in embodiment of the present invention SQUID annular seal space system.Fig. 5 B is according to the structural representation of specimen holder epimere in embodiment of the present invention SQUID annular seal space system.It should be noted that, in order to show corresponding details, Fig. 5 A is different with Fig. 5 B institute accepted scale.
Please refer to Fig. 5 A, be provided with sample carrier at specimen holder hypomere.In order to realize electrical measurement under the prerequisite not affecting high precision Magnetic Measurement, require sample carrier that even non-magnetic diamagnetism background can be provided.
In the present embodiment, sample carrier 50 is long for 200mm, and 2mm is wide, the strip silicon strip that about 0.75mm is thick, and this strip silicon strip is to form along diameter cutting from the Silicon Wafer of 8 inches.Because silicon materials are diamagnetic substances, magnetic background signal is very low, therefore this sample carrier, in fixed sample, has the long even magnetic background signal of a 200mm, and then can under the prerequisite that does not affect high precision Magnetic Measurement, realize electrical measurement while guaranteeing magnetic measurement.
Please refer to Fig. 5 B, at specimen holder epimere 62, be provided with the groove 64 of the clip phase interlock of band to band transfer module 20 inner sides and for the O type rubber seal 65 of fixed sample bar.This draw-in groove 64 matches with the clip on band to band transfer module 20, as shown in Figure 1.
In the present embodiment, wire 80 adopts enamel covered wire.Please refer to Fig. 5 A and Fig. 5 B, one end of some wires is connected to the test point of testing sample, is then wrapped on specimen holder, until the epimere of specimen holder, through the aperture on specimen holder top, is connected to one end of the conductive pin of quick union 28.The other end of the conductive pin 28a of quick union 28 is connected to external electrical measuring equipment.In addition,, for the noise that prevents that the friction of enamel covered wire and cylindrical shape sample cavity inwall from introducing, utilize nonmagnetic adhesive tape that enamel covered wire is fixed on specimen holder 60.
In the present embodiment, sample is that thickness is the dilute magnetic semiconductor GaMnAs film of 20nm.Below introduce the use step of the present embodiment for the above-mentioned dilute magnetic semiconductor GaMnAs of the SQUID annular seal space system testing film of magnetics and electrical properties synchro measure:
Steps A, unloads the original-pack plexiglas sealing column 22 that is fixed on reciprocating band to band transfer module top, changes the sealing column in the present embodiment;
Step B, melts and spreads upon wire end after indium rod and make it to be spherical with electric soldering iron, afterwards by wire bonds on testing sample surface, then sample is fixed on to long narrow silicon strip centre position by nonmagnetic adhesive tape, as shown in Fig. 5 A and Fig. 5 B;
Step C, loads onto specimen holder, makes the tight interlock of clip of groove with the transmission motor on specimen holder top, after connection wire, puts column urceolus to O type rubber seal place, uses helium purge Dewar system 10 3 times.
Step D, the MultiVu software carrying by SQUID system carries out position scanning to sample, generally applies the external magnetic field of 1 tesla for magnetic semiconductor sample, as detectable signal, sample is fixed on to the center of superconducting magnet and detecting coil with diamagnetism signal;
Step e, is connected to computing machine by electronic metering equipment Keithley2400 and Keithley2182 by GPIB connection, calls the dynamic link libraries file that compiling generates in MultiVu software;
Please refer to Fig. 3, the initial position of sample is the central point of superconducting magnet, and this position is also the center of detecting coil, and band to band transfer module 20 drives specimen holder 60 to move up and down, and is fixed on the testing sample of sample carrier and does reciprocating sinusoidal motion at vertical direction.Gather magnetic signal by magnetic induction coil 70 by electromagnetic induction principle.Meanwhile, external electrical measuring equipment can complete the measurement of electrical signal by wire.
Fig. 6 is the curve map that utilizes respectively traditional SQUID system and the present embodiment SQUID annular seal space system to carry out the measurement of dilute magnetic semiconductor material magnetic property.As shown in Figure 6, two curves overlap substantially, and high-temperature part is amplified, and the difference of the two is 10
-7the emu order of magnitude, shows that improved specimen holder still possesses high precision magnetic moment measurement function.
Fig. 7 utilizes the present embodiment SQUID annular seal space system to carry out the curve map of dilute magnetic semiconductor material magnetics and electric property synchro measure.Wherein, (a) be 100nm GaMnAs film magnetics and the electrical signal synchro measure result to temperature dependence; (b) be after numerical differentiation resistance to the dependence curve to temperature.Visible, utilize the present embodiment SQUID annular seal space system really can realize magnetics and electric property synchro measure.
So far, by reference to the accompanying drawings the present embodiment be have been described in detail.Describe according to above, those skilled in the art should have clearly understanding to specimen holder parts of the present invention.
In addition, the above-mentioned definition to each element and method is not limited in various concrete structures, shape or the mode in embodiment, mentioned, and those of ordinary skills can change simply or replace it, for example:
(1) plexiglas column can also be used cubic shaped;
(2) carbon fiber specimen holder can replace with nonmagnetic plastic sample bar;
(3) except cylindrical shape, sample cavity 40 can also be other tubular structure.
In sum, the present invention takes full advantage of the low temperature high-intensity magnetic field platform of SQUID magnetometer for the SQUID annular seal space system of magnetics and electrical properties synchro measure, guaranteed sample collection to its magnetics and electrical signal under equivalent environment simultaneously, the error of having avoided different measuring system to bring, improve the accuracy of measuring, can understand more accurately the spin pauper character of semiconductor spin-electronic material, study for solution Semiconductor Spintronics the problem in science facing solution is provided.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. for a SQUID annular seal space system for magnetics and electrical properties synchro measure, it is characterized in that, comprising:
Dewar system (10);
Sample cavity (40), is positioned at described Dewar system (10);
Specimen holder (60), its stage casing (61) and hypomere (63) stretch in described sample cavity (40), and testing sample (50) is fixed on the sample carrier of specimen holder hypomere (63);
Band to band transfer module (20), is arranged at the top of described Dewar system (10), is tightly connected with described sample cavity (40), and side opening on it;
Seal column, be fixed on the upper end of described band to band transfer module (20), comprising:
The column inner core (25) of both-side opening, its downside is sealingly fastened in band to band transfer module (20);
The column urceolus (26) of one-sided opening, its open lower side, the outside of socket and described column inner core (25), and realize sealing, the top perforate of this column urceolus (26) by extruding O type rubber seal (27) between the two; And
Quick union (28), is sealingly fastened in the perforate of described column urceolus (26) top, and this quick union has several conductive pins (28a);
Wherein, wire (80) is drawn by the corresponding test point of testing sample, by the described conductive pin (28a) on quick union by drawing in described sample cavity (40).
2. SQUID annular seal space system according to claim 1, it is characterized in that, described column urceolus (26) upside is offered the female circular hole of tool, the periphery of described quick union (28) has the external thread matching with this internal thread, and described quick union (28) is spirally connected with described column urceolus (26).
3. SQUID annular seal space system according to claim 2, is characterized in that, presses and put O type rubber seal (29) realization sealing between described column urceolus (26) and described quick union (28).
4. SQUID annular seal space system according to claim 1, is characterized in that, described wire is enamel covered wire.
5. SQUID annular seal space system according to claim 4, is characterized in that, described enamel covered wire is fixed on specimen holder by nonmagnetic adhesive tape.
6. SQUID annular seal space system according to claim 1, is characterized in that, described sample carrier is silicon materials sample carrier.
7. SQUID annular seal space system according to claim 6, is characterized in that, described sample carrier is strip.
8. SQUID annular seal space system according to claim 6, is characterized in that, described silicon materials sample carrier is by forming along diameter cutting on Silicon Wafer.
9. according to the SQUID annular seal space system described in any one in claim 1 to 8, it is characterized in that, described sealing column be shaped as cylinder or cube rod, its material is plexiglas.
10. according to the SQUID annular seal space system described in any one in claim 1 to 8, it is characterized in that, described specimen holder (60) is carbon fiber specimen holder or nonmagnetic plastic sample bar.
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| CN103885010B (en) | 2016-04-13 |
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