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 PDF

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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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CN101302403A (en
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金洙吉
苑泽伟
董伯先
康仁科
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Dalian University of Technology
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Abstract

本发明属于超硬材料抛光技术领域,公开了一种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液及制备方法。其特征是采用氧化能力较强的氧化剂包括三氧化铬、过硫酸铵、高锰酸钾、重铬酸钾、双氧水、高铁酸钾、高氯酸钾等作为主要成分,加入适量的磨料配制抛光液,在常温或较低的温度条件下,借助化学和机械复合作用即可实现金刚石晶圆表面材料的微量去除。此外,还通过添加适量的催化剂、稳定剂、分散剂等以提高抛光液的抛光效果。本发明的效果和益处是所制备的抛光液具有抛光效率高、抛光质量好、稳定性良好等优点,能够在常温或低温条件下实现大尺寸金刚石晶圆的超精密低损伤抛光。

Figure 200810012181

The invention belongs to the technical field of superhard material polishing, and discloses a polishing liquid for ultra-precision and low-damage polishing of a large-size diamond wafer and a preparation method thereof. It is characterized by using oxidants with strong oxidizing ability including chromium trioxide, ammonium persulfate, potassium permanganate, potassium dichromate, hydrogen peroxide, potassium ferrate, potassium perchlorate, etc. Under normal temperature or lower temperature conditions, micro-removal of materials on the surface of diamond wafers can be achieved by means of chemical and mechanical composite effects. In addition, the polishing effect of the polishing liquid is improved by adding an appropriate amount of catalyst, stabilizer, dispersant, etc. The effect and benefit of the invention is that the prepared polishing liquid has the advantages of high polishing efficiency, good polishing quality, good stability, etc., and can realize ultra-precision and low-damage polishing of large-sized diamond wafers under normal temperature or low temperature conditions.

Figure 200810012181

Description

The polishing fluid and the preparation method that are used for ultra-precise low-damage polish of large size diamond wafer
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)

1.一种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液,其特征在于,它包括磨料、氧化剂、稳定剂、分散剂、催化剂和去离子水,各原料所占质量百分比为:1. A polishing liquid for ultra-precision and low-damage polishing of large-size diamond wafers is characterized in that it includes abrasives, oxidizers, stabilizers, dispersants, catalysts and deionized water, and the mass percentages of each raw material are: 磨料:4~20%;Abrasive: 4-20%; 氧化剂:5~30%;Oxidant: 5-30%; 稳定剂:1~5%;Stabilizer: 1-5%; 分散剂:0.1~10%;Dispersant: 0.1~10%; 催化剂:1~5%;Catalyst: 1-5%; 去离子水:42~65%;Deionized water: 42-65%; 各原料质量百分比之和为100%;The sum of the mass percentages of each raw material is 100%; 所述的磨料纯度为98%~100%;粒度分布为50nm~14μm;The purity of the abrasive is 98%-100%; the particle size distribution is 50nm-14μm; 所述的分散剂为硅溶胶、六偏磷酸钠、活性磷酸钙、硅酸钠中的任意一种或者两种以上的混合,任意两种以上混合时,为任意配比;The dispersant is any one or a mixture of two or more of silica sol, sodium hexametaphosphate, active calcium phosphate, and sodium silicate. When any two or more are mixed, the ratio is arbitrary; 所述的稳定剂为酒石酸、磷酸二氢钾、柠檬酸、马来酸、硅酸钠中的任意一种或者两种以上的混合,任意两种以上混合时,为任意配比;The stabilizer is any one or a mixture of two or more of tartaric acid, potassium dihydrogen phosphate, citric acid, maleic acid, and sodium silicate. When any two or more are mixed, the ratio is arbitrary; 所述的催化剂为硫酸、磷酸、硝酸、硫酸亚铁、硝酸铁中的任意一种或者两种以上的混合;任意两种以上混合时,为任意配比。The catalyst is any one or a mixture of two or more of sulfuric acid, phosphoric acid, nitric acid, ferrous sulfate, and ferric nitrate; when any two or more are mixed, the ratio is arbitrary. 2.根据权利要求1所述的一种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液,其特征在于:采用在低温条件下对金刚石晶圆具有较强氧化作用的试剂,使所需抛光温度降至50~150℃。 2. a kind of polishing liquid that is used for ultra-precision low-damage polishing of large-size diamond wafer according to claim 1, is characterized in that: adopt the reagent that diamond wafer has stronger oxidizing effect under low temperature condition, make all The polishing temperature needs to be reduced to 50-150°C. the 3.权利要求1所述抛光液的制备方法,其特征在于包括如下步骤:3. the preparation method of polishing liquid described in claim 1 is characterized in that comprising the steps: 1)选取磨料、氧化剂、稳定剂、分散剂、催化剂和去离子水原料备用,各原料所占质量百分比为:磨料:4~20%;氧化剂:5~30%;稳定剂:1~5%;分散剂:0.1~10%;催化剂:1~5%;去离子水:42~65%;各原料质量百分比之和为100%;1) Select abrasives, oxidants, stabilizers, dispersants, catalysts and deionized water as raw materials for standby use. The mass percentages of each raw material are: abrasives: 4-20%; oxidants: 5-30%; stabilizers: 1-5% ; Dispersant: 0.1-10%; Catalyst: 1-5%; Deionized water: 42-65%; The sum of the mass percentages of each raw material is 100%; 2)按上述质量百分比将磨料加入到去离子水中,超声波搅拌10~30min,使得磨料在去离子水中充分分散,配制成悬浮液;2) Add the abrasive into the deionized water according to the above mass percentage, and ultrasonically stir for 10-30 minutes, so that the abrasive is fully dispersed in the deionized water and prepared into a suspension; 3)在悬浮液中按上述质量百分比加入氧化剂和催化剂,进行加热的同时超声波搅拌10~15min,以使各种溶剂充分溶解和分散;3) Add oxidizing agent and catalyst to the suspension according to the above mass percentage, and ultrasonically stir for 10-15 minutes while heating, so as to fully dissolve and disperse various solvents; 4)在该溶液中按上述质量百分比加入稳定剂和分散剂,超声波搅拌10~15min,制得抛光液。4) Add stabilizer and dispersant to the solution according to the above mass percentage, and ultrasonically stir for 10-15 minutes to prepare a polishing solution. 4.根据权利要求3所述的制备方法,其特征在于:所述的氧化剂为三氧化铬、过硫酸铵、高锰酸钾、重铬酸钾、双氧水、高铁酸钾、高氯酸钾中的任意一种或者两种以上的混合;任意两种以上混合时,为任意配比。4. preparation method according to claim 3 is characterized in that: described oxygenant is any in chromium trioxide, ammonium persulfate, potassium permanganate, potassium dichromate, hydrogen peroxide, potassium ferrate, potassium perchlorate A mixture of one or more than two; when any two or more are mixed, it is an arbitrary ratio. 5.根据权利要求3所述的制备方法,其特征在于:所述的磨料为二氧化钛、二氧化硅、碳化硼、碳化硅、立方氮化硼、金刚石中的任意一种或者两种以上的混合;任意两种以上混合时,为任意配比。 5. The preparation method according to claim 3, characterized in that: the abrasive is any one of titanium dioxide, silicon dioxide, boron carbide, silicon carbide, cubic boron nitride, diamond or a mixture of two or more ; When any two or more are mixed, the ratio is arbitrary. the
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