WO2003044122A1 - Particles for use in cmp slurries and method for producing them - Google Patents
Particles for use in cmp slurries and method for producing them Download PDFInfo
- Publication number
- WO2003044122A1 WO2003044122A1 PCT/US2002/035373 US0235373W WO03044122A1 WO 2003044122 A1 WO2003044122 A1 WO 2003044122A1 US 0235373 W US0235373 W US 0235373W WO 03044122 A1 WO03044122 A1 WO 03044122A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- particles
- titanium
- solution
- crystallization promoter
- cerium
- Prior art date
Links
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/76—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by a space-group or by other symmetry indications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Definitions
- the present invention provides a process for producing particles suitable for use as abrasives in chemical-mechanical polishing slurries and particles formed according to the process.
- CMP Chemical-mechanical polishing
- slurries are used, for example, to planarize surfaces during the fabrication of semiconductor chips and the like.
- CMP slurries typically include chemical etching agents and abrasive particles dispersed in a liquid carrier. The abrasive particles perform a grinding function when pressed against the surface being polished using a polishing pad.
- abrasive particles formed of, for example, alumina (AI 2 O 3 ), eerie oxide (CeO 2 ), iron oxide (Fe 2 O 3 ), silica (SiO 2 ), silicon carbide (SiC), silicon nitride (Si 3 N 4 ), tin oxide (SnO 2 ), titania (TiO 2 ), titanium carbide (TiC), tungstic oxide (WO 3 ), yttria (Y 2 O 3 ), zirconia (ZrO 2 ), and combinations thereof.
- eerie oxide (CeO 2 ) is the most efficient abrasive in CMP slurries for planarizing silicon dioxide insulating layers in semiconductors because of its high polishing activity.
- Calcination is by far the most common method of producing abrasive particles for use in CMP slurries. During the calcination process, precursors such as carbonates, oxalates, nitrates, and sulphates, are converted into their corresponding oxides. After the calcination process is complete, the resulting oxides must be milled to obtain particle sizes and distributions that are sufficiently small to prevent scratching.
- the calcination process although widely used, does present certain disadvantages. For example, it tends to be energy intensive and thus relatively expensive. Toxic and/or corrosive gaseous byproducts can be produced during calcination. In addition, it is very difficult to avoid the introduction of contaminants during the calcination and subsequent milling processes. Finally, it is difficult to obtain a narrow distribution of appropriately sized abrasive particles.
- CMP slurries containing contaminants and/or over-sized abrasive particles can result in undesirable surface scratching during polishing. While this is less critical for coarse polishing processes, in the production of critical optical surfaces, semiconductor wafers, and integrated circuits, defect-free surfaces are required. This is achievable only when the abrasive particles are kept below about 1.0 ⁇ m in diameter and the CMP slurry is free of contaminants. The production of abrasive particles meeting these requirements by conventional calcination and milling techniques is extremely difficult and often not economically feasible.
- An alternative method of forming abrasive particles for use in CMP slurries is hydrothermal synthesis, which is also known as hydrothermal treatment.
- the present invention provides a process for producing particles suitable for use as abrasives in chemical-mechanical polishing slurries.
- the process comprises adding a crystallization promoter such as titanium(IV) isopropoxide to an aqueous cerium salt solution, adjusting the pH to higher than 7.0 using one or more bases, and subjecting the solution to hydrothermal treatment at a temperature of from about 90 °C to about 500 °C to produce particles.
- a crystallization promoter such as titanium(IV) isopropoxide
- the process comprises adding a crystallization promoter such as titanium(IV) isopropoxide to an aqueous cerium salt solution, adjusting the pH to higher than 7.0 using one or more bases, and subjecting the solution to hydrothermal treatment at a temperature of from about 90 °C to about 500 °C to produce particles.
- Fig. 1 is a graph showing the particle size distribution of particles formed in Example 1.
- the present invention provides a process for producing particles suitable for use as abrasives in chemical-mechanical polishing slurries without the need for calcination and/or milling.
- the process comprises adding a crystallization promoter to an aqueous cerium salt solution, adjusting the pH to higher than 7.0 using one or more bases, and subjecting the solution to hydrothermal treatment at a temperature of from about 90 °C to about 500 °C to produce particles.
- the preferred cerium salt for use in the method according to the invention is (NH 4 ) 2 Ce(NO 3 ) 6 (ammonium cerium(IV) nitrate). However, it will be appreciated that other water soluble cerium salts can also be used.
- cerium salts for use in the invention include, for example, cerium nitrate, cerium chloride, cerium sulfate, cerium bromide, and cerium iodide.
- the solution must also comprise one or more crystallization promoters.
- the presently most preferred crystallization promoter is a titanium compound, namely Ti[OCH(CH 3 ) 2 )] 4 (titanium(IV) isopropoxide).
- Other titanium compounds can be used, such as, for example, titanium chloride, titanium sulfate, titanium bromide, and titanium oxychloride.
- Use of a crystallization promoter is essential in order to obtain particles having a relatively large crystallite size.
- One or more bases must be added to raise the pH of the solution to above 7.0 and assist in the formation of a solution having a gel-like consistency.
- Suitable bases include, for example, ammonium hydroxide, organoamines such as ethyl amine and ethanol amine, and/or polyorganoamines such as polyethylene imine.
- organoamines such as ethyl amine and ethanol amine
- polyorganoamines such as polyethylene imine.
- Other compounds such as urea can also be added to assist in crystal growth.
- the gel-like solution will break down into small particles upon rapid stirring.
- the gel-like solution is then subject to hydrothermal treatment. This is typically accomplished by transferring the solution to a stainless steel vessel, sealing the vessel, and then heating the solution in an oven to a temperature of from about 90°C to about 500°C for a period of time from about 10 minutes to many hours. At the completion of the reaction, the stainless steel vessel can be quenched in cold water, or it can be permitted to cool gradually over time.
- the solution can, but need not be, stirred during hydrothermal treatment. It is also possible to carry out the reaction in an autoclave unit with constant stirring.
- the average particle size (diameter) of the particles can be controlled by varying the initial concentration of the cerium salt: the higher the initial cerium ion concentration, the larger the particles produced.
- Use of additives such as urea tends to produce smaller particles. Reaction time, temperature, and pH appear to have little or no effect on particle size.
- a range of particle sizes from about 5 nm to about 1000 nm can be obtained via the process, but particles having an average diameter within the range of from about 50 nm to about 250 nm are most preferred.
- a solution containing a titanium(IV) isopropoxide crystallization promoter produced particles having an average crystallite size of 210 A whereas a solution containing no titanium(IV) isopropoxide crystallization promoter produced particles having a an average crystallite size of only 42 A.
- a crystallization promoter in the solution accelerates the crystal growth of crystallites during hydrothermal treatment.
- CMP slurries formed using particles having larger crystallite sizes tend to polish surfaces such as tetraethoxyorthosilicate (TEOS) silicon dioxide films at a much higher rate than CMP slurries formed using particles having smaller crystallite sizes.
- TEOS tetraethoxyorthosilicate
- the compounds used as crystallization promoters in the invention tend to rapidly decompose in aqueous media, which reduces their efficiency in promoting the formation of particles having larger crystallite sizes. Accordingly, it is preferable for one or more stabilizing compounds such as, for example, acetyl acetone, to be added with the crystallization promoters in order to prevent or delay the aqueous decomposition of such compounds.
- the crystallization promoters have sufficient time to homogeneously mix with the cerium salts at a molecular level before the gel-like solution is formed via the addition of one or more bases. Applicants have discovered that when the crystallization promoters are stabilized in this manner, the particles formed during hydrothermal treatment tend to have substantially larger crystallite sizes.
- the particles formed according to the process of the invention are particularly well-suited for use in CMP slurries.
- CMP slurries can be formed using the particles as obtained via the process or by adding water, acid and/or base to adjust the abrasive concentration and pH to desired levels.
- Surfaces that can be polished using CMP slurries containing the particles according to the invention include, but are not limited to TEOS silicon dioxide, spin-on glass, organosilicates, silicon nitride, silicon oxynitride, silicon, silicon carbide, computer memory hard disk substrates, silicon-containing low-k dielectrics, and silicon- containing ceramics.
- the solution was stirred for 5 minutes and then transferred to a clean 1000 ml stainless steel vessel.
- the stainless steel vessel was closed, shaken for 5 minutes, and then placed into a furnace and heated at 300°C for 6.0 hours.
- the stainless steel vessel was then removed from the furnace and allowed to cool to room temperature.
- the reaction product formed in the vessel was transferred to a clean 1000 ml plastic bottle.
- the cerium oxide particles had an average crystallite size of 210 A.
- a dispersion of cerium oxide particles was formed using the same materials and procedures as set forth in Example 1, except that no Ti[OCH(CH 3 ) 2 )] 4 (titanium(IV) isopropoxide) was used.
- a dispersion of cerium oxide particles was formed using the same materials and procedures as set forth in Example 1 , except that no acetyl acetone (CH 3 COCH 2 OCCH 3 ) was used.
- Slurry A consisted of 100 parts by weight of the cerium oxide nanoparticle dispersion formed in Example 1.
- Slurry B was identical to Slurry A, except that the cerium oxide nanoparticle dispersion formed in Example 2 was used instead of the cerium oxide nanoparticle solution formed in Example 1.
- Slurry C was identical to Slurry A, except that the cerium oxide nanoparticle dispersion formed in Example 3 was used instead of the cerium oxide nanoparticle solution formed in Example 1.
- Identical TEOS SiO 2 (silicon dioxide) wafers were polished using Slurries A, B, C, and D, respectively. The polishing was performed using a Strasbaugh 6EC polisher, a Rodel IC1000 pad with Suba IV backing at a down pressure of 3.2 psi, and a table rotation speed of 60 rpm, and slurry flow rate of 150 ml/min.
- the wafer polished using Slurry A had a SiO 2 removal rate of 3500 A/min and produced a surface having a root-mean-square average roughness of 0.8 A.
- the wafer polished using Slurry B had a SiO 2 removal rate of 85 A/min and produced a surface having a root-mean-square average roughness of 1.0 A.
- the wafer polished using Slurry C had a SiO 2 removal rate of 1875 A/min and produced a surface having a root-mean-square average roughness of 2.0 A.
- the wafer polished using Slurry D had a SiO 2 removal rate of 4200 A/min and produced a surface having a root-mean-square average roughness of 3.0 A.
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2003545749A JP4202257B2 (en) | 2001-11-16 | 2002-11-04 | Method of forming particles for use in a chemical mechanical polishing slurry and particles formed by the method |
AU2002357690A AU2002357690B2 (en) | 2001-11-16 | 2002-11-04 | Particles for use in CMP slurries and method for producing them |
CA2467030A CA2467030C (en) | 2001-11-16 | 2002-11-04 | Method of forming particles for use in chemical-mechanical polishing slurries and the particles formed by the process |
EP02792227A EP1444309A4 (en) | 2001-11-16 | 2002-11-04 | Particles for use in cmp slurries and method for producing them |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/992,485 US6596042B1 (en) | 2001-11-16 | 2001-11-16 | Method of forming particles for use in chemical-mechanical polishing slurries and the particles formed by the process |
US09/992,485 | 2001-11-16 |
Publications (1)
Publication Number | Publication Date |
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WO2003044122A1 true WO2003044122A1 (en) | 2003-05-30 |
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ID=25538391
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2002/035373 WO2003044122A1 (en) | 2001-11-16 | 2002-11-04 | Particles for use in cmp slurries and method for producing them |
Country Status (7)
Country | Link |
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US (2) | US6596042B1 (en) |
EP (1) | EP1444309A4 (en) |
JP (1) | JP4202257B2 (en) |
KR (1) | KR20050043789A (en) |
CN (1) | CN1296454C (en) |
CA (1) | CA2467030C (en) |
WO (1) | WO2003044122A1 (en) |
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US8080231B2 (en) | 2003-04-02 | 2011-12-20 | Saint-Gobain Ceramics & Plastics, Inc. | Process for making nanoporous ultrafine alpha-alumina powder |
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US7666239B2 (en) * | 2001-11-16 | 2010-02-23 | Ferro Corporation | Hydrothermal synthesis of cerium-titanium oxide for use in CMP |
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-
2001
- 2001-11-16 US US09/992,485 patent/US6596042B1/en not_active Expired - Lifetime
-
2002
- 2002-09-25 US US10/255,136 patent/US6818030B2/en not_active Expired - Lifetime
- 2002-11-04 JP JP2003545749A patent/JP4202257B2/en not_active Expired - Fee Related
- 2002-11-04 WO PCT/US2002/035373 patent/WO2003044122A1/en active IP Right Grant
- 2002-11-04 CA CA2467030A patent/CA2467030C/en not_active Expired - Fee Related
- 2002-11-04 KR KR1020047007234A patent/KR20050043789A/en not_active Application Discontinuation
- 2002-11-04 EP EP02792227A patent/EP1444309A4/en not_active Withdrawn
- 2002-11-04 CN CNB02822664XA patent/CN1296454C/en not_active Expired - Fee Related
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7422730B2 (en) | 2003-04-02 | 2008-09-09 | Saint-Gobain Ceramics & Plastics, Inc. | Nanoporous ultrafine α-alumina powders and sol-gel process of preparing same |
US8080231B2 (en) | 2003-04-02 | 2011-12-20 | Saint-Gobain Ceramics & Plastics, Inc. | Process for making nanoporous ultrafine alpha-alumina powder |
CN103923570A (en) * | 2014-05-06 | 2014-07-16 | 济南大学 | Preparation method of rare earth-doped silicon carbide composite polishing powder |
Also Published As
Publication number | Publication date |
---|---|
US20030093957A1 (en) | 2003-05-22 |
US6818030B2 (en) | 2004-11-16 |
AU2002357690A1 (en) | 2003-06-10 |
EP1444309A1 (en) | 2004-08-11 |
CN1296454C (en) | 2007-01-24 |
EP1444309A4 (en) | 2007-07-18 |
CA2467030C (en) | 2010-10-12 |
US6596042B1 (en) | 2003-07-22 |
JP4202257B2 (en) | 2008-12-24 |
JP2005509725A (en) | 2005-04-14 |
KR20050043789A (en) | 2005-05-11 |
CN1585811A (en) | 2005-02-23 |
CA2467030A1 (en) | 2003-05-30 |
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