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.
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.