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 CN 200810012181 CN200810012181A CN101302403B CN 101302403 B CN101302403 B CN 101302403B CN 200810012181 CN200810012181 CN 200810012181 CN 200810012181 A CN200810012181 A CN 200810012181A CN 101302403 B CN101302403 B CN 101302403B
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polishing
abrasive
deionized water
catalyst
diamond wafer
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CN 200810012181
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CN101302403A (en )
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康仁科
苑泽伟
董伯先
金洙吉
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大连理工大学
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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 beimproved 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

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 For ultra-precision large-size diamond wafer polishing liquid low-damage polishing and preparation

方法 method

技术领域 FIELD

[0001] 本发明属于超硬材料抛光技术领域,特别涉及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。 [0001] The present invention belongs to the technical field of polishing a superhard material, and particularly relates to a polishing liquid and a method for preparing a large-sized ultra precision diamond wafer for polishing low damage.

背景技术 Background technique

[0002] 金刚石晶圆不仅具有高的硬度和耐磨性,而且具有优良的电绝缘性、导热性、透光性和声学及力学特性,被视为21世纪最有发展前途的新材料,在高新技术领域和国防尖端技术领域都有广泛的应用。 [0002] diamond wafer not only has high hardness and wear resistance, and excellent electrical insulation, thermal conductivity, light transmittance and acoustic and mechanical properties of new materials is considered the most promising in the 21st century, defense and high-tech fields cutting-edge technology has a wide range of applications. 但由于受晶体相生长机理的制约,随着晶圆厚度的增加,其表面粗糙度和晶粒大小也会增大到几个微米甚至几十个微米,必须采用精密加工方法将其表面粗糙度降低到纳米量级,并达到一定的面型精度,才能投入使用。 However, due to the constraints of the crystal growth mechanism phase, with increasing thickness of the wafer, the surface roughness and grain size will increase to several tens of microns or even microns, precision machining method must be used to surface roughness down to the nanometer level, and to a certain type of surface accuracy can be put into use. 特别在高新技术领域应用时,不仅要求金刚石晶圆具有极小的表面粗糙度,同时还对其面型精度和表面完整性提出了很高的要求。 When a particular application in the field of high-tech, not only requires a very small diamond wafer having a surface roughness, but also its surface integrity Surface Accuracy and high demands made. 目前金刚石晶圆抛光平坦化技术的相对滞后,尤其是大尺寸CVD金刚石晶圆的超精密无损伤抛光平坦化技术已成为金刚石晶圆在高新技术领域得到广泛应用的瓶颈问题。 Currently polished diamond wafer planarization is lagging behind technology, especially the ultra-precision polishing large size without injury CVD diamond wafer planarization technology has become the bottleneck of diamond wafers are widely used in high-tech fields.

[0003] 由于金刚石是目前已知的硬度最高且高化学惰性的材料,使得现有的抛光技术很难实现大尺寸金刚石晶圆的超精密无损伤表面加工。 [0003] Since diamond is the highest known hardness and high chemical inertness of the material, such that the prior art polishing is difficult to achieve a large-sized diamond wafer without damaging the surface of the ultra-precision machining. 例如,激光束抛光、离子束抛光等抛光技术,目前主要针对小尺寸(Φ < 1英寸)的金刚石晶圆,而且设备复杂、成本高,很难用于产业化生产;热化学抛光技术和电火花抛光技术,虽然目前已能够实现大尺寸金刚石晶圆抛光平坦化,但其抛光表面粗糙度Ra仅能达到几百纳米水平,而且对加工表面带来损伤和污染;传统的机械抛光技术虽然能够实现纳米级抛光,但抛光效率极低,而且容易在加工表面留下划痕等损伤。 For example, polishing the laser beam, an ion beam polishing polishing, mainly for small size (Φ <1 inch) diamond wafer, and complex equipment, and high cost, it is difficult for industrial production; electrical and thermal chemical polishing techniques spark polishing technology, although now possible to realize a large-sized diamond wafer planarizing polishing, but the polishing surface roughness Ra can only reach the level of several hundred nanometers, but also brings damage and contamination of the machined surface; although the conventional mechanical polishing technique capable of achieve nano polishing, but the polishing efficiency is very low, but also easy to leave damage such as scratches in the machined surface. 化学机械抛光(CMP)作为一种基于化学与机械复合作用原理的超精密加工技术,是目前实现大尺寸硅片超光滑无损伤表面加工的最理想的加工方法,在IC制造领域得到广泛应用。 Chemical mechanical polishing (CMP) as an ultra-precision machining technology is based on the principle of mechanical and chemical action of the composite, the processing is the best way to implement a large-sized wafer without damage to ultra-smooth surface finish, it is widely used in IC manufacturing.

[0004] 虽然目前也有针对金刚石膜的化学机械抛光方法,但由于采用ΚΝ03+Κ0Η或NaN03+KN03+LiN03等混合熔融物作为氧化剂,所需抛光温度达324〜360°C,存在能源消耗大、抛光液蒸发损失大、难以保证抛光液成分的稳定性等问题,尤其随着金刚石晶圆尺寸的增大,高温引起的抛光盘变形和金刚石晶圆翘曲变形等问题更加突出。 [0004] Although there are a method for chemical mechanical polishing of the diamond film, but due ΚΝ03 + Κ0Η NaN03 + KN03 + LiN03 or the like as the oxidant mixture melts, the desired temperature of the polishing 324~360 ° C, the presence of energy consumption, the polishing liquid evaporation loss is large, the problem is difficult to ensure stability of the polishing liquid ingredients, etc., especially with the diamond wafer size increases, the deformation due to high temperatures and polishing diamond wafer warpage problem is more prominent. 另外,由于现有抛光液不含添加催化剂、稳定剂、分散剂等抛光液常用成分,存在抛光速率低,抛光液的稳定性差等问题。 Further, since the conventional polishing solution containing no added catalyst, a stabilizer, a dispersing agent was used a polishing composition, there is a low polishing rate, poor stability of the polishing liquid. 现有的抛光工艺与设备无法满足对大尺寸金刚石晶圆的高效低成本超精密加工要求。 The polishing process with the existing equipment can not meet the requirements of ultra-precision machining cost-efficient large-size diamond wafer.

发明内容 SUMMARY

[0005] 本发明要解决的技术问题是提供一种适于大尺寸金刚石晶圆超精密低损伤抛光的抛光液及其制备方法,解决目前金刚石晶圆的化学机械抛光中由于采用以混合熔融物为氧化剂的抛光液而存在的抛光温度高、设备成本大、加工效率低、抛光质量差等问题。 [0005] The present invention is to solve the technical problem of providing a low damage ultraprecision diamond wafer polishing of large size and preparation method thereof adapted to solve the chemical mechanical polishing using diamond wafer due to melt mixing height polishing liquid oxidant exists polishing temperature, high equipment cost, low processing efficiency, poor quality polishing. [0006] 为了实现上述目的,本发明的技术方案是: [0006] To achieve the above object, the technical solution of the present invention is:

[0007] —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、催化剂、分散剂、稳定剂和去离子水,各原料所占质量百分比为: [0007] - large size diamond wafer types for ultra-precision polishing of low damage solution, characterized in that it comprises an abrasive, an oxidizing agent, a catalyst, a dispersing agent, a stabilizing agent, and deionized water, as a percentage by mass of the raw materials :

[0008]磨料:4 〜20%; [0008] Abrasive: 4 ~ 20%;

[0009] 氧化剂:5〜30%; [0009] Antioxidant: 5~30%;

[0010] 稳定剂:1〜5%; [0010] Stabilizer: 1 ~ 5%;

[0011]分散剂:0.1 〜10%; [0011] Dispersant: 0.1 ~ 10%;

[0012] 催化剂:1〜5%; [0012] Catalyst: 1 ~ 5%;

[0013] 去离子水:42〜65% ;各原料质量百分比之和为100% ; [0013] Deionized water: 42~65%; mass percentage of the raw materials is 100%;

[0014] 所述的磨料纯度为98%〜100% ;粒度分布为50nm〜14 μ m。 The abrasive purity [0014] The 98% ~ 100%; particle size distribution 50nm~14 μ m.

[0015] 上述抛光液的制备方法,包括如下步骤: Preparation [0015] The method of the above-described polishing liquid, comprising the steps of:

[0016] 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% ; [0016] 1) Select an abrasive, an oxidizing agent, a stabilizer, a dispersant, deionized water, and the catalyst feed standby, the percentage by mass of the raw materials as follows: Abrasive: 4~20%; oxidant: 5~30%; Stabilizer: 1 ~ 5%; dispersant: 0 1~10%; catalyst: 1 ~ 5%; deionized water: 42~65%; mass percentage of the raw materials is 100%;

[0017] 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; [0017] 2) above was added to the abrasive mass percentage of deionized water, ultrasonic agitation 10~30min, sufficiently so that the abrasive dispersed in deionized water to prepare a suspension;

[0018] 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。 While [0018] 3) adding an oxidizing agent and a catalyst as described above mass percentage in suspension, heating ultrasonic agitation 10~15min, so that various solvents and thoroughly dissolving and dispersing.

[0019] 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, 即可制得抛光液。 [0019] 4) In the above-described percentage by mass was added stabilizers and dispersing agents, ultrasonic agitation 10~15min, the polishing liquid can be prepared.

[0020] 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、金刚石等磨料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。 [0020] The titanium oxide abrasive, when any of the above mixing an abrasive silica, boron carbide, silicon carbide, cubic boron nitride, diamond or a mixture of two, any two or more, as with any ratio.

[0021 ] 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、高氯酸钾等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。 Oxidant [0021] The chromium trioxide is, any one or more of ammonium persulfate, potassium permanganate, potassium dichromate, hydrogen peroxide, potassium ferrate, potassium perchlorate and the like or a mixture of two, any two when the above mixing ratio is arbitrary.

[0022] 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。 [0022] The catalyst is one or two or more, phosphoric, nitric, sulfuric any ferrous sulfate, ferric nitrate mixing arbitrary two or more kinds, arbitrary ratio.

[0023] 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。 Stabilizer [0023], wherein one or two or more of tartaric acid, potassium dihydrogen phosphate, citric acid, maleic acid arbitrary, mixing sodium silicate, arbitrary two or more kinds, arbitrary ratio.

[0024] 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。 Dispersant [0024] The silica sol of sodium hexametaphosphate, calcium activity, any one or two or more of sodium silicate mixture, mixing any two or more arbitrary ratio.

[0025] 本发明的效果和益处是:本发明采用可在低温条件下对金刚石晶圆具有较强氧化剂作用的试剂作为主要成分,可使所需抛光温度降至50〜150°C,有效地解决因抛光温度高而导致的能源消耗大、抛光液蒸发损失大、难以保证抛光液成分的稳定性等问题,尤其对于大尺寸金刚石晶圆的加工中,可有效解决高温引起的大尺寸抛光盘变形和金刚石晶圆翘曲变形等难题,提高金刚石晶圆的面型精度和表面质量,抛光后金刚石晶圆的表面粗糙度可达纳米级。 [0025] The effects and benefits of the present invention are: the present invention reagents may be employed with a strong oxidizing agent at low temperature as a main component of the diamond wafer, the polishing allows the desired temperature was lowered to 50~150 ° C, effectively due to the high temperature of the polishing solution resulting from energy consumption, large evaporation loss of the polishing liquid, the polishing liquid is difficult to ensure stability problems and other components, especially for large size diamond wafer processing, it can effectively solve the large size of polishing due to high temperatures diamond wafer warpage and deformation and other problems, to improve the surface accuracy and surface quality type diamond wafer, the surface roughness of the diamond wafer after polishing can reach nanometer level. 此外,通过采用分散剂和吸附性较强的稳定剂等添加剂,提高抛光液的分散稳定性。 Further, by using a dispersant and a strong adsorption stabilizer additives to improve dispersion stability of the polishing liquid.

附图说明[0026] 图1是抛光前金刚石晶圆表面的500倍扫描电镜照片。 BRIEF DESCRIPTION [0026] FIG. 1 is a scanning electron micrograph of 500-fold diamond wafer front surface polishing.

[0027] 图2是抛光后金刚石晶圆表面的500倍扫描电镜照片。 [0027] FIG. 2 is a 500 times after polishing SEM photograph of the diamond wafer surface.

具体实施方式 detailed description

[0028] 下面结合技术方案和附图详细叙述本发明的具体实施例。 [0028] below with reference to the accompanying drawings and the technical solutions described in detail specific embodiments of the present invention.

[0029] 本发明的方法中所使用的氧化剂、稳定剂、分散剂、催化剂等药品均为常见药品。 [0029] oxidants, stabilizing agents, dispersing agents, catalysts and other drugs in methods of the invention are used in common drugs. 本发明的方法所用的设备均为常用的已知设备。 The method of the present invention are used in conventional apparatus known devices.

[0030] 实施例1 : [0030] Example 1:

[0031] 一种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液的制备方法,它包括如下步骤: [0031] A method for preparing a large-sized low damage ultra-precision diamond wafer polishing liquid for polishing, comprising the steps of:

[0032] 1)按各原料所占质量百分比为:磨料:18%、氧化剂:25%、稳定剂:3% ;分散剂: ;催化剂:2. 5% ;去离子水:50. 5% ;选取磨料、氧化剂、稳定剂、分散剂、催化剂和去离子 [0032] 1) the percentage by mass of the raw materials is occupied: Abrasive: 18% Antioxidant: 25%, stabilizer: 3%; Dispersant:; catalyst: 25%; Deionized water: 50 5%;. select an abrasive, an oxidizing agent, stabilizing agents, dispersing agents, catalysts, and deionized

水原料备用; Alternate water feed;

[0033] 所述的磨料为碳化硼,纯度为98%,粒度为2μπι;所述的氧化剂为高锰酸钾;所述的稳定剂为酒石酸;所述的分散剂为硅酸钠;所述的催化剂为磷酸。 [0033] The boron carbide abrasive, 98% purity, particle size of 2μπι; the oxidizing agent is potassium permanganate; said stabilizer is tartaric acid; said dispersant is sodium silicate; the the catalyst is phosphoric acid.

[0034] 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15min,使磨料在去离子水中充分分散,配制成悬浮液; [0034] 2) above was added to the abrasive mass percentage of deionized water, ultrasonic stirring 15min, the abrasive dispersed in deionized water sufficient to prepare a suspension;

[0035] 3)在悬浮液中按上述质量百分比加入上述的氧化剂、催化剂,进行加热同时超声波搅拌lOmin,促进各种溶剂的溶解和分散。 [0035] 3) In the above-described suspension was added the aforementioned oxidant mass percent, the catalyst was heated with stirring while ultrasonic lOmin, promote dissolution and dispersion of various solvents.

[0036] 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lOmin,即可制抛光液。 [0036] 4) In the above solution, the mass percentage addition of stabilizers and dispersing agents, ultrasonic agitation lOmin, the polishing liquid can be prepared.

[0037] 实施例2 : [0037] Example 2:

[0038] 一种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液的制备方法,它包括如下步骤: [0038] A method for preparing a large-sized low damage ultra-precision diamond wafer polishing liquid for polishing, comprising the steps of:

[0039] 1)按各原料所占质量百分比为:磨料:10%、氧化剂:30%、稳定剂:3% ;分散剂: ;催化剂:4. 5% ;去离子水:51. 5% ;选取磨料、氧化剂、稳定剂、分散剂、催化剂和去离子 [0039] 1) the percentage by mass of the raw materials is occupied: Abrasive: 10% Antioxidant: 30%, stabilizer: 3%; Dispersant:; catalyst: 45%; Deionized water: 51 5%;. select an abrasive, an oxidizing agent, stabilizing agents, dispersing agents, catalysts, and deionized

水原料备用; Alternate water feed;

[0040] 所述的磨料为二氧化钛,纯度为99%,粒度为10 μ m ;所述的氧化剂为过硫酸铵和双氧水;所述的稳定剂为酒石酸和硅酸钠,酒石酸、硅酸钠所占质量百分比各占1. 5%;所述的分散剂为六偏磷酸钠;所述的催化剂为硫酸和硫酸亚铁,硫酸、硫酸亚铁所占质量百分比各占2. 25%。 [0040] The abrasive material is titanium dioxide having a purity of 99%, a particle size of 10 μ m; the oxidizing agent is ammonium persulfate and hydrogen peroxide; said stabilizer is tartaric acid and sodium tartrate, sodium silicate representing each accounted for 1.5% percent by mass; dispersing agent is the sodium hexametaphosphate; the catalyst is sulfuric acid and ferrous sulfate, ferrous sulfate share each accounted for 2.25% by mass percentage.

[0041] 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30min,使得磨料在去离子水中充分分散,配制成悬浮液; [0041] 2) above was added to the abrasive mass percentage of deionized water, ultrasonic stirring 30min, sufficiently so that the abrasive dispersed in deionized water to prepare a suspension;

[0042] 3)在悬浮液中按上述质量百分比加入上述的氧化剂、催化剂,进行加热同时超声波搅拌lOmin,促进各种溶剂的溶解和分散。 [0042] 3) In the above-described suspension was added the aforementioned oxidant mass percent, the catalyst was heated with stirring while ultrasonic lOmin, promote dissolution and dispersion of various solvents.

[0043] 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lOmin,即可制得抛光液。 [0043] 4) In the above-described percentage by mass was added stabilizers and dispersing agents, ultrasonic agitation lOmin, the polishing liquid can be prepared.

[0044] 实施例3 : [0044] Example 3:

[0045] 一种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液的制备方法,它包括如下步骤: [0045] A method for preparing a large-sized low damage ultra-precision diamond wafer polishing liquid for polishing, comprising the steps of:

[0046] 1)按各原料所占质量百分比为:磨料:15%、氧化剂:23%、稳定剂:5% ;分散剂: ;催化剂:3. 5% ;去离子水:52. 5% ;选取磨料、氧化剂、稳定剂、分散剂、催化剂和去离子 [0046] 1) the percentage by mass of the raw materials is occupied: Abrasive: 15% Antioxidant: 23%, stabilizers: 5%; dispersant:; Catalyst: 3 5%; Deionized water: 52 5%;. select an abrasive, an oxidizing agent, stabilizing agents, dispersing agents, catalysts, and deionized

水原料备用; Alternate water feed;

[0047] 所述的磨料为碳化硅,纯度为99%,粒度为2 μ m ;所述的氧化剂为重铬酸钾;所述的稳定剂为柠檬酸;所述的分散剂为六偏磷酸钠;所述的催化剂为磷酸和硝酸铁。 [0047] The abrasive is silicon carbide with a purity of 99%, a particle size of 2 μ m; the oxidizing agent is potassium dichromate; said stabilizer is citric acid; the dispersing agent is hexametaphosphoric acid sodium; phosphoric acid and the catalyst is ferric nitrate.

[0048] 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15min,使得磨料在去离子水中充分分散,配制成悬浮液; [0048] 2) above was added to the abrasive mass percentage of deionized water, ultrasonic stirring 15min, sufficiently so that the abrasive dispersed in deionized water to prepare a suspension;

[0049] 3)在悬浮液中按上述质量百分比加入上述的氧化剂、催化剂,进行加热同时超声波搅拌lOmin,促进各种溶剂的溶解和分散。 [0049] 3) In the above-described suspension was added the aforementioned oxidant mass percent, the catalyst was heated with stirring while ultrasonic lOmin, promote dissolution and dispersion of various solvents.

[0050] 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lOmin,即可制得抛光液。 [0050] 4) In the above-described percentage by mass was added stabilizers and dispersing agents, ultrasonic agitation lOmin, the polishing liquid can be prepared.

[0051] 实施例4: [0051] Example 4:

[0052] 一种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液的制备方法,它包括如下步骤: [0052] A method for preparing a large-sized low damage ultra-precision diamond wafer polishing liquid for polishing, comprising the steps of:

[0053] 1)按各原料所占质量百分比为:磨料:20%、氧化剂:10%、稳定剂:3% ;分散剂: 10% ;催化剂:5% ;去离子水:52% ;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; [0053] 1) the percentage by mass of the raw materials is occupied: Abrasive: 20% Antioxidant: 10%, stabilizer: 3%; Dispersant: 10%; Catalyst: 5%; Deionized water: 52%; selecting abrasive , oxidizing agents, stabilizing agents, dispersing agents, catalysts and deionized water feed standby;

[0054] 所述的磨料为碳化硼,纯度为98%,粒度为2μπι ;所述的氧化剂为三氧化铬;所述的稳定剂为柠檬酸,柠檬酸所占质量百分比各占1. 5% ;所述的分散剂为硅酸钠;所述的催化剂为硫酸。 [0054] The boron carbide abrasive, 98% purity, particle size of 2μπι; the oxidizing agent is chromium trioxide; said stabilizer is citric acid, citric acid mass percentage share of each accounted for 1.5% ; said dispersant is sodium silicate; the catalyst is sulfuric acid.

[0055] 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30min,使得磨料在去离子水中充分分散,配制成悬浮液; [0055] 2) above was added to the abrasive mass percentage of deionized water, ultrasonic stirring 30min, sufficiently so that the abrasive dispersed in deionized water to prepare a suspension;

[0056] 3)在悬浮液中按上述质量百分比加入上述的氧化剂、催化剂,进行加热同时超声波搅拌lOmin,促进各种溶剂的溶解和分散。 [0056] 3) In the above-described suspension was added the aforementioned oxidant mass percent, the catalyst was heated with stirring while ultrasonic lOmin, promote dissolution and dispersion of various solvents.

[0057] 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lOmin,即可制得抛光液。 [0057] 4) In the above-described percentage by mass was added stabilizers and dispersing agents, ultrasonic agitation lOmin, the polishing liquid can be prepared.

[0058] 实施例5 : [0058] Example 5:

[0059] 一种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液的制备方法,它包括如下步骤: [0059] A method for preparing a large-sized low damage ultra-precision diamond wafer polishing liquid for polishing, comprising the steps of:

[0060] 1)按各原料所占质量百分比为:磨料:6%、氧化剂:30%、稳定剂:2% ;分散剂: 8% ;催化剂:20% ;去离子水:34% ;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; [0060] 1) the percentage by mass of the raw materials is occupied: Abrasive: 6%, the oxidizing agent: 30%, stabilizers: 2%; dispersant: 8%; Catalyst: 20%; Deionized water: 34%; selecting abrasive , oxidizing agents, stabilizing agents, dispersing agents, catalysts and deionized water feed standby;

[0061] 所述的磨料为金刚石颗粒,纯度为99%,粒度为0. 5μπι ;所述的氧化剂为高锰酸钾;所述的稳定剂为柠檬酸;所述的催化剂为磷酸。 [0061] The diamond abrasive particles, a purity of 99% particle size of 0. 5μπι; the oxidizing agent is potassium permanganate; said stabilizer is citric acid; the catalyst is phosphoric acid.

[0062] 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20min,使得磨料在去离子水中充分分散,配制成悬浮液; [0062] 2) above was added to the abrasive mass percentage of deionized water, ultrasonic stirring 20min, sufficiently so that the abrasive dispersed in deionized water to prepare a suspension;

[0063] 3)在悬浮液中按上述质量百分比加入上述的氧化剂、催化剂,进行加热同时超声波搅拌lOmin,促进各种溶剂的溶解和分散。 [0063] 3) In the above-described suspension was added the aforementioned oxidant mass percent, the catalyst was heated with stirring while ultrasonic lOmin, promote dissolution and dispersion of various solvents. [0064] 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15min,即可制得抛光液。 [0064] 4) In the above-described percentage by mass was added stabilizers and dispersing agents, ultrasonic stirring 15min, the polishing liquid can be prepared.

[0065] 实施例6 : [0065] Example 6:

[0066] 一种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液的制备方法,它包括如下步骤: [0066] A method for preparing a large-sized low damage ultra-precision diamond wafer polishing liquid for polishing, comprising the steps of:

[0067] 1)按各原料所占质量百分比为:磨料:10%、氧化剂:28%、稳定剂:1.4% •'分散剂:3% ;催化剂:2. 7% ;去离子水:54. 9% ;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; [0067] 1) the percentage by mass of the raw materials is occupied: Abrasive: 10% Antioxidant: 28%, stabilizers: 1.4% • 'Dispersant: 3%; Catalyst: 2 7%; Deionized water: 54. 9%; selecting an abrasive, an oxidizing agent, a stabilizer, a dispersant, a catalyst material and deionized water reserve;

[0068] 所述的磨料为碳化硼,纯度为98%,粒度为2μπι;所述的氧化剂为高铁酸钾;所述的稳定剂为磷酸二氢钾;所述的分散剂为六偏磷酸钠;所述的催化剂为磷酸。 [0068] The boron carbide abrasive, 98% purity, particle size of 2μπι; the oxidizing agent is potassium ferrate; potassium dihydrogen phosphate as the stabilizer; the dispersing agent is sodium hexametaphosphate ; said catalyst is phosphoric acid.

[0069] 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20min,使得磨料在去离子水中充分分散,配制成悬浮液; [0069] 2) above was added to the abrasive mass percentage of deionized water, ultrasonic stirring 20min, sufficiently so that the abrasive dispersed in deionized water to prepare a suspension;

[0070] 3)在悬浮液中按上述质量百分比加入上述的氧化剂、催化剂,进行加热同时超声波搅拌lOmin,促进各种溶剂的溶解和分散。 [0070] 3) In the above-described suspension was added the aforementioned oxidant mass percent, the catalyst was heated with stirring while ultrasonic lOmin, promote dissolution and dispersion of various solvents.

[0071] 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15min,即可制得抛光液。 [0071] 4) In the above-described percentage by mass was added stabilizers and dispersing agents, ultrasonic stirring 15min, the polishing liquid can be prepared.

[0072] 实施例7 : [0072] Example 7:

[0073] —种用于大尺寸金刚石晶圆超精密低损伤抛光的抛光液的制备方法,它包括如下步骤: [0073] - preparation of ultra-precision large diamond wafer polishing of low damage species for liquid, comprising the steps of:

[0074] 1)按各原料所占质量百分比为:磨料:7%、氧化剂:15%、稳定剂:3.5%;分散剂: 8% ;催化剂:4% ;去离子水:62. 5% ;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; [0074] 1) the percentage by mass of the raw materials is occupied: Abrasive: 7%, the oxidizing agent: 15%, stabilizers: 3.5%; dispersant: 8%; Catalyst: 4%; Deionized water: 625.%; select an abrasive, an oxidizing agent, a stabilizer, a dispersant, deionized water, and the catalyst feed standby;

[0075] 所述的磨料为金刚石,纯度为99%,粒度为10 μ m;所述的氧化剂为高锰酸钾;所述的稳定剂为油石酸;所述的分散剂为六偏磷酸钠;所述的催化剂为磷酸。 [0075] The diamond abrasive, 99% purity, a particle size of 10 μ m; the oxidizing agent is potassium permanganate; Whetstone said stabilizer is an acid; said dispersant is sodium hexametaphosphate ; said catalyst is phosphoric acid.

[0076] 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20min,使得磨料在去离子水中充分分散,配制成悬浮液; [0076] 2) above was added to the abrasive mass percentage of deionized water, ultrasonic stirring 20min, sufficiently so that the abrasive dispersed in deionized water to prepare a suspension;

[0077] 3)在悬浮液中按上述质量百分比加入上述的氧化剂、催化剂,进行加热同时超声波搅拌lOmin,促进各种溶剂的溶解和分散。 [0077] 3) In the above-described suspension was added the aforementioned oxidant mass percent, the catalyst was heated with stirring while ultrasonic lOmin, promote dissolution and dispersion of various solvents.

[0078] 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15min,即可制得抛光液。 [0078] 4) In the above-described percentage by mass was added stabilizers and dispersing agents, ultrasonic stirring 15min, the polishing liquid can be prepared.

[0079] 在抛光温度为60°C的条件下,采用按实施例1制备的抛光液,在精密研磨抛光机上进行了抛光试验。 [0079] In the polishing temperature conditions of 60 ° C, using a polishing liquid prepared according to Example 1, the polishing tests carried out on a precision polishing machine. 图2为抛光后得到的金刚石晶圆表面的扫描电镜照片(放大倍数500 倍),图2中少量黑点为CVD金刚石晶圆固有的生长缺陷。 FIG 2 is a diamond wafer after polishing the surface obtained by scanning electron microscope photograph (magnification 500 times), a small amount of black dots in FIG. 2 CVD diamond wafer is inherent growth defects. 图1是未抛光金刚石晶圆表面的500倍扫描电镜照片。 FIG 1 is a non-polished diamond wafer surface SEM photograph of 500 times.

Claims (5)

  1. 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:磨料:4〜20% ;氧化剂:5〜30% ;稳定剂:1〜5% ;分散剂:0· 1〜·;催化剂:1〜5% ;去离子水:42〜65% ;各原料质量百分比之和为100% ;所述的磨料纯度为98%〜100% ;粒度分布为50nm〜14μπι ; 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;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;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。 A large ultra-precision diamond wafer polishing of low damage solution, characterized in that it comprises an abrasive, an oxidizing agent, stabilizing agents, dispersing agents, catalysts and deionized water, the percentage proportion by mass of the raw materials is: abrasive: 4~20%; oxidant: 5~30%; stabilizer: 1 ~ 5%; dispersant: 1 ~ · 0 ·; catalyst: 1 ~ 5%; deionized water: 42~65%; the quality of the raw materials total percentage is 100%; the abrasive ~ 100%, a purity of 98%; grain size distribution 50nm~14μπι; said dispersant is silica sol, sodium hexametaphosphate, calcium activity, any sodium silicate one or a mixture of two or more, the mixing of any two or more thereof, any ratio; stabilizer according to any one of tartaric acid, potassium dihydrogen phosphate, citric acid, maleic acid, sodium silicate, or mixing two or more kinds, the mixing of any two or more thereof, of any ratio; the catalyst is nitric acid, ferrous sulfate, ferric nitrate in any mixing two or more kinds of sulfuric acid, or; any two when the above mixing ratio is arbitrary.
  2. 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°C。 2. A method according to claim 1 for a large-sized ultra-precision diamond wafer polishing of low damage solution, characterized in that: the use of reagents having a strong oxidizing effect on the diamond wafer at a low temperature, so that the The polishing required temperature was reduced to 50 ~150 ° C.
  3. 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: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% ;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;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;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。 The method of preparing the polishing liquid according to claim 1, characterized by comprising the following steps: 1) Select an abrasive, an oxidizing agent, a stabilizer, a dispersant, deionized water, and the catalyst feed standby, as a percentage by mass of the raw materials: abrasive : 4~20%; oxidant: 5~30%; stabilizer: 1 ~ 5%; dispersant: 0 1~10%; catalyst: 1 ~ 5%; deionized water: 42~65%; the quality of the raw materials total percentage is 100%; 2) above was added to the abrasive mass percentage of deionized water, ultrasonic agitation 10~30min, sufficiently so that the abrasive dispersed in deionized water to prepare a suspension; 3) in the above-described mass suspension while the percentage adding an oxidizing agent and a catalyst, heating ultrasonic agitation 10~15min, so that various solvents and thoroughly dissolving and dispersing; 4) in the solution described above mass percentage addition of stabilizers and dispersing agents, ultrasonic agitation 10~15min, Ltd. I was polishing liquid.
  4. 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. The method of preparation according to claim 3, wherein: said oxidant is chromium trioxide, any ammonium persulfate, potassium permanganate, potassium dichromate, hydrogen peroxide, potassium ferrate, potassium perchlorate in or a mixture of two or more; mixing any two or more arbitrary ratio.
  5. 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。 The production method according to claim 3, wherein: said abrasive is titania, any one of silica, boron carbide, silicon carbide, cubic boron nitride, diamond or a mixture of two or more ; mixing any two or more arbitrary ratio.
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