CN101302403B - Polishing solution for ultra-precise low-damage polish of large size diamond wafer and preparation thereof - Google Patents
Polishing solution for ultra-precise low-damage polish of large size diamond wafer and preparation thereof Download PDFInfo
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- CN101302403B CN101302403B CN2008100121814A CN200810012181A CN101302403B CN 101302403 B CN101302403 B CN 101302403B CN 2008100121814 A CN2008100121814 A CN 2008100121814A CN 200810012181 A CN200810012181 A CN 200810012181A CN 101302403 B CN101302403 B CN 101302403B
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- 238000005498 polishing Methods 0.000 title claims abstract description 68
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 46
- 239000010432 diamond Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims description 16
- 239000003082 abrasive agent Substances 0.000 claims abstract description 53
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 6
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004160 Ammonium persulphate Substances 0.000 claims abstract description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000019395 ammonium persulphate Nutrition 0.000 claims abstract description 4
- 229940117975 chromium trioxide Drugs 0.000 claims abstract description 4
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 4
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims abstract description 4
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 claims abstract description 4
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 claims abstract description 3
- 229910001487 potassium perchlorate Inorganic materials 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims description 50
- 239000003795 chemical substances by application Substances 0.000 claims description 42
- 239000008367 deionised water Substances 0.000 claims description 40
- 229910021641 deionized water Inorganic materials 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 239000012530 fluid Substances 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 20
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- 235000019353 potassium silicate Nutrition 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 6
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 6
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 5
- 229940095064 tartrate Drugs 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 4
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000001506 calcium phosphate Substances 0.000 claims description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 2
- 235000011010 calcium phosphates Nutrition 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- -1 norbide Chemical compound 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229960001866 silicon dioxide Drugs 0.000 claims description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 229960002163 hydrogen peroxide Drugs 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
- 235000012431 wafers Nutrition 0.000 description 34
- 238000005516 engineering process Methods 0.000 description 11
- 238000003754 machining Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 229910013553 LiNO Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000009643 growth defect Effects 0.000 description 1
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- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- 238000011105 stabilization Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention belongs to the superhard material polishing technical field and discloses polishing solution used for ultraprecise and low-damage polishing of a large-scale diamond wafer and a method for preparing the same. The method is characterized in that: oxidants with strong oxidbillity including chromium trioxide, ammonium persulphate, potassium permanganate, potassium dichromate, oxydol, potassium ferrate, potassium perchlorate and so on are adopted as main compositions; a proper amount of abrasive material is added for preparing the polishing solution; and micro-removal of surface material of the diamond wafer can be realized by means of chemical and mechanical composite action at normal temperature or low temperature. Moreover, the polishing effect of the polishing solution can be improved by addition of proper amount of catalyst, stabilizer, dispersant and so on as well. The polishing solution and the method have the advantages that: the polishing solution prepared has the advantages of high polishing efficiency, good polishing quality, good stability and so on; and the ultraprecise and low-damage polishing of the large-scale diamond wafer can be realized at the normal temperature or the low temperature.
Description
Technical field
The invention belongs to superhard material polishing technology field, particularly a kind of polishing fluid and preparation method who is used for ultra-precise low-damage polish of large size diamond wafer.
Background technology
Diamond wafer not only has high hardness and wear resistance, and have excellent electric insulation, thermal conductivity, light transmission and acoustics and a mechanical characteristic, be regarded as the most rising novel material of 21 century, all be widely used at high-technology field and national defence sophisticated technology field.But owing to be subjected to the restriction of crystal phase growth mechanism, increase along with wafer thickness, its surfaceness and grain size also can increase to several microns even tens microns, must adopt precision machining method that its surfaceness is reduced to nanometer scale, and reach certain surface precision, just can come into operation.When high-technology field is used, not only require diamond wafer to have minimum surfaceness especially, also its surface precision and surface integrity have been proposed very high requirement simultaneously.Relatively lagging behind of the planarization of diamond wafer polishing at present, especially the ultraprecise not damaged of large size CVD diamond wafer polishing planarization has become the bottleneck problem that diamond wafer is used widely at high-technology field.
Because diamond is the highest and high chemically inert material of present known hardness, make existing polishing technology be difficult to realize the ultraprecise not damaged surface working of large size diamond wafer.For example, polishing technologies such as laser beam polishing, ion beam polishing are primarily aimed at the diamond wafer of small size (φ≤1 inch) at present, and equipment complexity, cost height, are difficult to industrialization production; Thermo-chemical polishing technology and spark polishing technology, though can realize large size diamond wafer polishing planarization at present, its glazed surface roughness Ra only can reach the hundreds of nanometer level, and finished surface is brought damage and pollution; Though traditional mechanical polishing technology can be realized the nano level polishing, polishing efficiency is extremely low, and stays the cut equivalent damage at finished surface easily.Chemically machinery polished (CMP) is the optimal working method that realizes large-sized silicon wafers ultra-smooth not damaged surface working at present as a kind of Ultraprecision Machining based on chemistry and mechanical compound action principle, is used widely in IC manufacturing field.
Though the cmp method at diamond film is also arranged at present, owing to adopt KNO
3+ KOH or NaNO
3+ KNO
3+ LiNO
3Deng the mixed melting thing as oxygenant, required polish temperature reaches 324～360 ℃, there are the problems such as stability that energy consumption is big, polishing fluid vaporization losses is big, be difficult to guarantee the polishing fluid composition, especially along with the increase of diamond wafer size, problems such as polishing disk distortion that high temperature causes and diamond wafer buckling deformation are more outstanding.In addition, because existing polishing fluid does not contain composition commonly used such as the polishing fluid that adds catalyzer, stablizer, dispersion agent, exist polishing speed low, problems such as the poor stability of polishing fluid.Existing glossing and equipment can't satisfy the high efficiency, low cost ultraprecise processing request to large size diamond wafer.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of polishing fluid that is suitable for ultra-precise low-damage polish of large size diamond wafer and preparation method thereof, and solving in the chemically machinery polished of present diamond wafer owing to adopting with the mixed melting thing is big, the problems such as working (machining) efficiency is low, quality of finish difference of polish temperature height, equipment cost that the polishing fluid of oxygenant exists.
To achieve these goals, technical scheme of the present invention is:
A kind of polishing fluid that is used for ultra-precise low-damage polish of large size diamond wafer is characterized in that it comprises abrasive material, oxygenant, catalyzer, dispersion agent, stablizer and deionized water, and the shared mass percent of each raw material is:
Abrasive material: 4～20%;
Oxygenant: 5～30%;
Stablizer: 1～5%;
Dispersion agent: 0.1～10%;
Catalyzer: 1～5%;
Deionized water: 42～65%; Each raw materials quality per-cent sum is 100%;
Described abrasive material purity is 98%～100%; Size-grade distribution is 50nm～14 μ m.
The preparation method of above-mentioned polishing fluid comprises the steps:
1) choose abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water raw material for standby, the shared mass percent of each raw material is: abrasive material: 4～20%; Oxygenant: 5～30%; Stablizer: 1～5%; Dispersion agent: 0.1～10%; Catalyzer: 1～5%; Deionized water: 42～65%; Each raw materials quality per-cent sum is 100%;
2) by above-mentioned mass percent abrasive material is joined in the deionized water, ultrasonic stirring 10～30min makes abrasive material fully disperse in deionized water, is mixed with suspension;
3) add oxygenant and catalyzer by above-mentioned mass percent in suspension, ultrasonic stirring 10～15min when heating is so that all kinds of SOLVENTS fully dissolves and disperses.
4) add stablizer and dispersion agent by above-mentioned mass percent in this solution, ultrasonic stirring 10～15min can make polishing fluid.
Described abrasive material is any one or the two or more mixing in the abrasive materials such as titanium dioxide, silicon-dioxide, norbide, silicon carbide, cubic boron nitride, diamond, during any two or more mixing, is any proportioning.
Described oxygenant is any one or the two or more mixing in chromium trioxide, ammonium persulphate, potassium permanganate, potassium bichromate, hydrogen peroxide, potassium ferrate, the potassium perchlorate etc., during any two or more mixing, is any proportioning.
Described catalyzer is any one or the two or more mixing in sulfuric acid, phosphoric acid, nitric acid, ferrous sulfate, the iron nitrate, during any two or more mixing, is any proportioning.
Described stablizer is any one or the two or more mixing in tartrate, potassium primary phosphate, citric acid, toxilic acid, the water glass, during any two or more mixing, is any proportioning.
Described dispersion agent is any one or the two or more mixing in silicon sol, Sodium hexametaphosphate 99, active calcium phosphate, the water glass, during any two or more mixing, is any proportioning.
Effect of the present invention and benefit are: the present invention adopts and can be under cold condition diamond wafer to be had reagent than the strong oxidizer effect as main component, can make required polish temperature reduce to 50～150 ℃, it is big to solve the energy consumption that causes because of the polish temperature height effectively, polishing fluid vaporization losses is big, be difficult to guarantee the problems such as stability of polishing fluid composition, especially in the processing for large size diamond wafer, can effectively solve difficult problems such as large size polishing disk distortion that high temperature causes and diamond wafer buckling deformation, improve the surface precision and the surface quality of diamond wafer, the surfaceness of polishing back diamond wafer can reach nano level.In addition, by adopting dispersion agent and the stronger additives such as stablizer of adsorptivity, improve the dispersion stabilization of polishing fluid.
Description of drawings
Fig. 1 is 500 times of stereoscan photographs on diamond wafer surface before the polishing.
Fig. 2 is 500 times of stereoscan photographs on diamond wafer surface, polishing back.
Embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme and accompanying drawing.
Medicines such as employed oxygenant, stablizer, dispersion agent, catalyzer are common medicine in the method for the present invention.The used equipment of method of the present invention is known device commonly used.
Embodiment 1:
A kind of preparation method who is used for the polishing fluid of ultra-precise low-damage polish of large size diamond wafer, it comprises the steps:
1) by the shared mass percent of each raw material is: abrasive material: oxygenant 18%: stablizer 25%: 3%; Dispersion agent: 1%; Catalyzer: 2.5%; Deionized water: 50.5%; Choose abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water raw material for standby;
Described abrasive material is a norbide, and purity is 98%, and granularity is 2 μ m; Described oxygenant is a potassium permanganate; Described stablizer is a tartrate; Described dispersion agent is a water glass; Described catalyzer is a phosphoric acid.
2) by above-mentioned mass percent abrasive material is joined in the deionized water, ultrasonic stirring 15min fully disperses abrasive material in deionized water, be mixed with suspension;
3) in suspension, add above-mentioned oxygenant, catalyzer, heat ultrasonic stirring 10min simultaneously, promote the dissolving and the dispersion of all kinds of SOLVENTS by above-mentioned mass percent.
4) add stablizer and dispersion agent by above-mentioned mass percent in this solution, ultrasonic stirring 10min can make polishing fluid.
Embodiment 2:
A kind of preparation method who is used for the polishing fluid of ultra-precise low-damage polish of large size diamond wafer, it comprises the steps:
1) by the shared mass percent of each raw material is: abrasive material: oxygenant 10%: stablizer 30%: 3%; Dispersion agent: 1%; Catalyzer: 4.5%; Deionized water: 51.5%; Choose abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water raw material for standby;
Described abrasive material is a titanium dioxide, and purity is 99%, and granularity is 10 μ m; Described oxygenant is ammonium persulphate and hydrogen peroxide; Described stablizer is tartrate and water glass, and tartrate, the shared mass percent of water glass respectively account for 1.5%; Described dispersion agent is a Sodium hexametaphosphate 99; Described catalyzer is sulfuric acid and ferrous sulfate, and sulfuric acid, the shared mass percent of ferrous sulfate respectively account for 2.25%.
2) by above-mentioned mass percent abrasive material is joined in the deionized water, ultrasonic stirring 30min makes abrasive material fully disperse in deionized water, is mixed with suspension;
3) in suspension, add above-mentioned oxygenant, catalyzer, heat ultrasonic stirring 10min simultaneously, promote the dissolving and the dispersion of all kinds of SOLVENTS by above-mentioned mass percent.
4) add stablizer and dispersion agent by above-mentioned mass percent in this solution, ultrasonic stirring 10min can make polishing fluid.
Embodiment 3:
A kind of preparation method who is used for the polishing fluid of ultra-precise low-damage polish of large size diamond wafer, it comprises the steps:
1) by the shared mass percent of each raw material is: abrasive material: oxygenant 15%: stablizer 23%: 5%; Dispersion agent: 1%; Catalyzer: 3.5%; Deionized water: 52.5%; Choose abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water raw material for standby;
Described abrasive material is a silicon carbide, and purity is 99%, and granularity is 2 μ m; Described oxygenant is a potassium bichromate; Described stablizer is a citric acid; Described dispersion agent is a Sodium hexametaphosphate 99; Described catalyzer is phosphoric acid and iron nitrate.
2) by above-mentioned mass percent abrasive material is joined in the deionized water, ultrasonic stirring 15min makes abrasive material fully disperse in deionized water, is mixed with suspension;
3) in suspension, add above-mentioned oxygenant, catalyzer, heat ultrasonic stirring 10min simultaneously, promote the dissolving and the dispersion of all kinds of SOLVENTS by above-mentioned mass percent.
4) add stablizer and dispersion agent by above-mentioned mass percent in this solution, ultrasonic stirring 10min can make polishing fluid.
Embodiment 4:
A kind of preparation method who is used for the polishing fluid of ultra-precise low-damage polish of large size diamond wafer, it comprises the steps:
1) by the shared mass percent of each raw material is: abrasive material: oxygenant 20%: stablizer 10%: 3%; Dispersion agent: 10%; Catalyzer: 5%; Deionized water: 52%; Choose abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water raw material for standby;
Described abrasive material is a norbide, and purity is 98%, and granularity is 2 μ m; Described oxygenant is a chromium trioxide; Described stablizer is a citric acid, and the shared mass percent of citric acid respectively accounts for 1.5%; Described dispersion agent is a water glass; Described catalyzer is a sulfuric acid.
2) by above-mentioned mass percent abrasive material is joined in the deionized water, ultrasonic stirring 30min makes abrasive material fully disperse in deionized water, is mixed with suspension;
3) in suspension, add above-mentioned oxygenant, catalyzer, heat ultrasonic stirring 10min simultaneously, promote the dissolving and the dispersion of all kinds of SOLVENTS by above-mentioned mass percent.
4) add stablizer and dispersion agent by above-mentioned mass percent in this solution, ultrasonic stirring 10min can make polishing fluid.
Embodiment 5:
A kind of preparation method who is used for the polishing fluid of ultra-precise low-damage polish of large size diamond wafer, it comprises the steps:
1) by the shared mass percent of each raw material is: abrasive material: oxygenant 6%: stablizer 30%: 2%; Dispersion agent: 8%; Catalyzer: 20%; Deionized water: 34%; Choose abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water raw material for standby;
Described abrasive material is a diamond particles, and purity is 99%, and granularity is 0.5 μ m; Described oxygenant is a potassium permanganate; Described stablizer is a citric acid; Described catalyzer is a phosphoric acid.
2) by above-mentioned mass percent abrasive material is joined in the deionized water, ultrasonic stirring 20min makes abrasive material fully disperse in deionized water, is mixed with suspension;
3) in suspension, add above-mentioned oxygenant, catalyzer, heat ultrasonic stirring 10min simultaneously, promote the dissolving and the dispersion of all kinds of SOLVENTS by above-mentioned mass percent.
4) add stablizer and dispersion agent by above-mentioned mass percent in this solution, ultrasonic stirring 15min can make polishing fluid.
Embodiment 6:
A kind of preparation method who is used for the polishing fluid of ultra-precise low-damage polish of large size diamond wafer, it comprises the steps:
1) by the shared mass percent of each raw material is: abrasive material: oxygenant 10%: stablizer 28%: 1.4%; Dispersion agent: 3%; Catalyzer: 2.7%; Deionized water: 54.9%; Choose abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water raw material for standby;
Described abrasive material is a norbide, and purity is 98%, and granularity is 2 μ m; Described oxygenant is a potassium ferrate; Described stablizer is a potassium primary phosphate; Described dispersion agent is a Sodium hexametaphosphate 99; Described catalyzer is a phosphoric acid.
2) by above-mentioned mass percent abrasive material is joined in the deionized water, ultrasonic stirring 20min makes abrasive material fully disperse in deionized water, is mixed with suspension;
3) in suspension, add above-mentioned oxygenant, catalyzer, heat ultrasonic stirring 10min simultaneously, promote the dissolving and the dispersion of all kinds of SOLVENTS by above-mentioned mass percent.
4) add stablizer and dispersion agent by above-mentioned mass percent in this solution, ultrasonic stirring 15min can make polishing fluid.
Embodiment 7:
A kind of preparation method who is used for the polishing fluid of ultra-precise low-damage polish of large size diamond wafer, it comprises the steps:
1) by the shared mass percent of each raw material is: abrasive material: oxygenant 7%: stablizer 15%: 3.5%; Dispersion agent: 8%; Catalyzer: 4%; Deionized water: 62.5%; Choose abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water raw material for standby;
Described abrasive material is a diamond, and purity is 99%, and granularity is 10 μ m; Described oxygenant is a potassium permanganate; Described stablizer is oilstone acid; Described dispersion agent is a Sodium hexametaphosphate 99; Described catalyzer is a phosphoric acid.
2) by above-mentioned mass percent abrasive material is joined in the deionized water, ultrasonic stirring 20min makes abrasive material fully disperse in deionized water, is mixed with suspension;
3) in suspension, add above-mentioned oxygenant, catalyzer, heat ultrasonic stirring 10min simultaneously, promote the dissolving and the dispersion of all kinds of SOLVENTS by above-mentioned mass percent.
4) add stablizer and dispersion agent by above-mentioned mass percent in this solution, ultrasonic stirring 15min can make polishing fluid.
Be under 60 ℃ the condition, to adopt the polishing fluid of press embodiment 1 preparation at polish temperature, on precise grinding polisher, carried out polishing and tested.Fig. 2 for polishing after the stereoscan photograph (500 times of magnifications) on the diamond wafer surface that obtains, a small amount of stain is a CVD diamond wafer inherent growth defect among Fig. 2.Fig. 1 is 500 times of stereoscan photographs of polishing diamond crystal column surface not.
Claims (5)
1. a polishing fluid that is used for ultra-precise low-damage polish of large size diamond wafer is characterized in that, it comprises abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water, and the shared mass percent of each raw material is:
Abrasive material: 4～20%;
Oxygenant: 5～30%;
Stablizer: 1～5%;
Dispersion agent: 0.1～10%;
Catalyzer: 1～5%;
Deionized water: 42～65%;
Each raw materials quality per-cent sum is 100%;
Described abrasive material purity is 98%～100%; Size-grade distribution is 50nm～14 μ m;
Described dispersion agent is any one or the two or more mixing in silicon sol, Sodium hexametaphosphate 99, active calcium phosphate, the water glass, during any two or more mixing, is any proportioning;
Described stablizer is any one or the two or more mixing in tartrate, potassium primary phosphate, citric acid, toxilic acid, the water glass, during any two or more mixing, is any proportioning;
Described catalyzer is any one or the two or more mixing in sulfuric acid, phosphoric acid, nitric acid, ferrous sulfate, the iron nitrate; During any two or more mixing, be any proportioning.
2. a kind of polishing fluid that is used for ultra-precise low-damage polish of large size diamond wafer according to claim 1, it is characterized in that: adopt under cold condition diamond wafer is had reagent than strong oxidation, make required polish temperature reduce to 50～150 ℃.
3. the preparation method of the described polishing fluid of claim 1 is characterized in that comprising the steps:
1) choose abrasive material, oxygenant, stablizer, dispersion agent, catalyzer and deionized water raw material for standby, the shared mass percent of each raw material is: abrasive material: 4～20%; Oxygenant: 5～30%; Stablizer: 1～5%; Dispersion agent: 0.1～10%; Catalyzer: 1～5%; Deionized water: 42～65%; Each raw materials quality per-cent sum is 100%;
2) by above-mentioned mass percent abrasive material is joined in the deionized water, ultrasonic stirring 10～30min makes abrasive material fully disperse in deionized water, is mixed with suspension;
3) add oxygenant and catalyzer by above-mentioned mass percent in suspension, ultrasonic stirring 10～15min when heating is so that all kinds of SOLVENTS fully dissolves and disperses;
4) add stablizer and dispersion agent by above-mentioned mass percent in this solution, ultrasonic stirring 10～15min makes polishing fluid.
4. preparation method according to claim 3 is characterized in that: described oxygenant is any one or the two or more mixing in chromium trioxide, ammonium persulphate, potassium permanganate, potassium bichromate, hydrogen peroxide, potassium ferrate, the potassium perchlorate; During any two or more mixing, be any proportioning.
5. preparation method according to claim 3 is characterized in that: described abrasive material is any one or the two or more mixing in titanium dioxide, silicon-dioxide, norbide, silicon carbide, cubic boron nitride, the diamond; During any two or more mixing, be any proportioning.
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| CN2008100121814A CN101302403B (en) | 2008-07-03 | 2008-07-03 | Polishing solution for ultra-precise low-damage polish of large size diamond wafer and preparation thereof |
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| CN102464944B (en) * | 2010-11-05 | 2015-05-20 | 安集微电子（上海）有限公司 | Chemical-mechanical polishing liquid and its application method |
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| CN115011258A (en) * | 2022-07-20 | 2022-09-06 | 黄河三角洲京博化工研究院有限公司 | Double-component polishing solution, preparation method thereof and silicon wafer polishing method |
| CN115851137A (en) * | 2022-12-20 | 2023-03-28 | 青岛福禄泰科表面材料科技有限公司 | Polishing solution for semiconductor material and preparation method thereof |
| CN118165701B (en) * | 2024-05-11 | 2024-07-26 | 山东天岳先进科技股份有限公司 | Grinding liquid for diamond and grinding method for diamond substrate |
| CN118143760B (en) * | 2024-05-11 | 2024-07-05 | 山东天岳先进科技股份有限公司 | Surface treatment method of diamond substrate |
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