WO2016150176A1 - 含钴掺杂二氧化硅纳米复合磨粒溶胶、抛光液及其制备方法 - Google Patents

含钴掺杂二氧化硅纳米复合磨粒溶胶、抛光液及其制备方法 Download PDF

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WO2016150176A1
WO2016150176A1 PCT/CN2015/095184 CN2015095184W WO2016150176A1 WO 2016150176 A1 WO2016150176 A1 WO 2016150176A1 CN 2015095184 W CN2015095184 W CN 2015095184W WO 2016150176 A1 WO2016150176 A1 WO 2016150176A1
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cobalt
sol
nanocomposite
polishing
abrasive
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PCT/CN2015/095184
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French (fr)
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李家荣
马盼
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江苏天恒纳米科技有限公司
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09G—POLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00—Polishing compositions
    • C09G1/02—Polishing compositions containing abrasives or grinding agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives

Definitions

  • the invention relates to a cobalt-containing doped silica nanocomposite abrasive sol, a polishing liquid and a preparation method thereof.
  • Sapphire single crystal namely aluminum oxide single crystal, combines excellent mechanical, optical, chemical, electrical and anti-radiation properties. It has been widely used in high temperature and high voltage resistant devices, optical systems, special windows, wear resistant devices, infrared guidance, Missile fairings and other high-tech fields such as civil, military, and scientific research. It is especially important that the c (0001) plane of the single crystal sapphire becomes the main substrate material of the light emitting diode because of its small mismatch ratio with the lattice coefficient of the semiconductor GaN, high mechanical strength, and good stability. The rapid development of the LED industry puts new demands on the smoothness of the surface of the sapphire substrate, but the single crystal sapphire poses new challenges for precision polishing because of its high hardness and good chemical stability.
  • polishing single crystal sapphire there are many methods for polishing single crystal sapphire. These polishing mainly remove the surface material of the wafer by chemical and mechanical action to obtain a smooth surface without lattice defects. Some of these processing methods are mainly mechanical, such as Mechanical polishing, liquid jet polishing; some are mainly chemical, such as chemical polishing, hydration polishing; or chemical mechanical phase balancing, such as chemical mechanical polishing (CMP). Among them, chemical mechanical polishing is recognized as the only polishing method that can achieve the global polishing effect, and is widely used in the final precision polishing of sapphire because of its advantages of high speed and low cost.
  • mechanical polishing such as Mechanical polishing, liquid jet polishing
  • chemical mechanical phase balancing such as chemical mechanical polishing (CMP).
  • CMP chemical mechanical polishing
  • the object of the present invention is to overcome the deficiencies of the prior art and to provide a cobalt-containing doping.
  • the cobalt-containing doped silica nanocomposite abrasive granule of the invention has a mass ratio of 0.43 wt% of cobalt nitrate solution and 2.5 wt% of silicic acid solution in a mass ratio of 1:1, and simultaneously adds 1 wt% sodium hydroxide.
  • the doping amount is from 0.1% by weight to 5% by weight.
  • the sol system is stable and can be stored stably for more than six months.
  • the doping amount of cobalt hydroxide in the sol is from 0.5 to 1.5% by weight.
  • the nanocomposite abrasive particles in the sol have a particle diameter of 20 to 150 nm.
  • the particle size of the nanocomposite abrasive particles in the sol is 106-123 nm.
  • the preparation method of the cobalt-containing doped silica nanocomposite abrasive sol is as follows: a silicic acid having a pH of 2.5 and a mass fraction of 2.5% is first prepared by a cation exchange method. Under 100 ° C and stirring conditions, silicic acid, 0.43 wt% cobalt nitrate solution and 1 wt% sodium hydroxide were added to the silica seed crystal for growth. The sodium hydroxide controlled the pH of the whole sol system to 10, and controlled nitric acid. The drop rate of the cobalt and silicic acid mixture maintains the equilibrium between the evaporation rate and the droplet acceleration in the sol system.
  • the doping reaction time is from 140 minutes to 420 minutes. By controlling the doping reaction time, a silica nanocomposite abrasive sol system with different cobalt doping amounts can be obtained.
  • a polishing liquid composition having a composition and mass percentage as follows:
  • polishing liquid composition composition and mass percentage are as follows:
  • the structure of the nanocomposite abrasive particles in the cobalt-containing doped silica nanocomposite abrasive granule of the present invention is a pure silica seed crystal inside, and the outer layer grown portion is doped with cobalt hydroxide and silica. The part that is together.
  • the outer layer of cobalt hydroxide reacts with the alumina of the sapphire surface to increase the removal rate of sapphire.
  • the hardness of cobalt hydroxide is smaller than that of silica, which can reduce the wear on the surface of sapphire and reduce the surface roughness.
  • the abrasive particles thus designed can achieve the purpose of "high rate, low roughness" polishing at the same time. Polishing the sapphire substrate by using the polishing liquid provided by the invention can effectively improve the surface removal rate of the sapphire and reduce the roughness of the sapphire surface.
  • the cobalt-containing doped silica nanocomposite abrasive granule of the present embodiment was prepared by a coprecipitation method.
  • the preparation process is as follows: firstly, a cation exchange method is used to prepare a pH value of 2.5, then 2.5 wt% of silicic acid, 0.43 wt% of Co(NO3)2 ⁇ 6H2O solution at an equal mass ratio, stirring at 100 ° C, and 1 wt%. Sodium hydroxide is added to the silica seed crystals separately.
  • the cobalt-doped silica nanocomposite abrasive sol was prepared by dropwise addition of 140 minutes, 280 minutes, and 420 minutes, respectively, to a cobalt hydroxide doping amount of 0.5 wt%, 1.0 wt%, and 1.5 wt%.
  • the sol having a cobalt hydroxide doping amount of 0.5% by weight was diluted with deionized water to 3 L, and the solid content was 10%.
  • the composite abrasive grain size of cobalt-doped silica is 106 nm, and the final pH of the sol is 10.
  • a 1% dispersant sodium pyrophosphate and a 0.5% surfactant dodecyl polyoxyethylene ether were added to obtain a polishing liquid.
  • the sol having a cobalt hydroxide doping amount of 1.0 wt% was diluted with deionized water to 3 L, and the solid content was 10%.
  • the composite abrasive grain size of the cobalt-doped silica is 110 nm, and the final pH of the sol is 10.
  • a 1% dispersant sodium pyrophosphate and a 0.5% surfactant dodecyl polyoxyethylene ether were added to obtain a polishing liquid.
  • the sol of 1.5 wt% of cobalt hydroxide was diluted with deionized water to 3 L, and the solid content was 10%.
  • the composite abrasive grain size of the cobalt-doped silica was 123 nm, and the final pH of the sol was 10.5.
  • a 1% dispersant sodium pyrophosphate and a 0.5% surfactant dodecyl polyoxyethylene ether were added to obtain a polishing liquid.
  • the undoped pure silica sol was diluted with deionized water to 3 L, the solid content was 10%, the silica particles were 95 nm, and the pH was 10 after dilution. After filtration through a 350-mesh sieve, a 1% dispersant sodium pyrophosphate and a 0.5% surfactant dodecyl polyoxyethylene ether were added to obtain a polishing liquid.
  • Polishing test using the above polishing liquid to sapphire substrate under certain polishing conditions Light test. Polishing conditions are as follows:
  • Polishing machine UNIPOL-1502 single-side polishing machine
  • Polishing pad polyurethane material, RODEL production
  • the substrate is then washed and dried, and then the surface topography of the substrate is measured.
  • the surface average roughness (Ra) was measured with an Ambios XI-100 surface topographer with a resolution of 0.1 angstrom.
  • the test range was 93.5 ⁇ m '93.5 ⁇ m.
  • the weight of the substrate was weighed using an analytical balance, and the difference in weight before and after polishing divided by the polishing time was the polishing rate.
  • Example 1 The polishing effects of the polishing liquids of the respective examples are shown in Table 1, respectively. It can be seen that the sol containing the cobalt-doped composite abrasive particles (Examples 1, 2, 3) has improved the polishing speed and reduced the surface of the sapphire after polishing the sapphire substrate compared to Comparative Example 1 (pure silica sol). Roughness.
  • Example 1 Example 2 Example 3 Comparative Example 1 Polishing rate mg/h 6.55 8.40 6.75 4.55 Ra, nm 1.538 1.612 1.564 2.541

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

本发明提供了一种含钴掺杂二氧化硅纳米复合磨粒溶胶，由质量百分数为0.43wt％的硝酸钴溶液和2.5wt％的硅酸溶液按1:1的质量比，同时加入1wt％氢氧化钠，通过共沉淀法沉淀在二氧化硅晶种上反应制成，所述的溶胶中的纳米复合磨粒呈均匀球形，所述的含钴掺杂二氧化硅纳米复合磨粒溶胶中的氢氧化钴掺杂量为0.1wt％-5wt％。采用本发明提供的抛光液对蓝宝石基片进行抛光，可以有效地提高蓝宝石表面去除率，降低蓝宝石表面的粗糙度。

Description

含钴掺杂二氧化硅纳米复合磨粒溶胶、抛光液及其制备方法 技术领域
本发明涉及一种含钴掺杂二氧化硅纳米复合磨粒溶胶、抛光液及其制备方法。
背景技术
蓝宝石单晶即三氧化二铝单晶，综合了优良的机械、光学、化学、电学以及抗辐射性能，已广泛应用于耐高温高压器件、光学系统、特种窗口、耐磨损器件、红外制导、导弹整流罩等民用、军事、科研高科技领域。尤为重要的是单晶蓝宝石c(0001)面因为与半导体GaN的晶格系数失配率较小、机械强度高、稳定性好等优势成为发光二极管的主要衬底材料。LED行业的迅猛发展对蓝宝石衬底表面的光滑度提出了新的要求，但单晶蓝宝石因为其硬度高，化学稳定性好等特点对精密抛光提出了新的挑战。
目前应用于单晶蓝宝石抛光的方法有很多，这些抛光主要以化学和机械作用将晶片表面材料去除，以获得光洁无晶格缺陷的表面，在这些加工方法中有的以机械作用为主，如机械抛光、液体喷射抛光；有的以化学作用为主，如化学抛光、水合抛光；或化学机械相平衡起作用，如化学机械抛光(CMP)。其中化学机械抛光是公认的唯一一种可以取得全局抛光效果的抛光方法，并且因为去其除速率快、成本低的优势广泛应用于蓝宝石最终的精密抛光中。目前在蓝宝石抛光的实际应用中，通常采用二氧化硅、氧化铝等传统无机磨粒，其对蓝宝石的抛光速率和表面粗糙度上已不能很好的满足工业需求。已报道的复合磨粒也都大多是通过高温煅烧再溶解之后得到复合氧化物磨粒，而在煅烧过程中颗粒的团聚会增大抛光基片的表面粗糙度。
发明内容
本发明的发明目的在于克服现有技术的不足之处，提供一种含钴掺杂 二氧化硅纳米复合磨粒、抛光液及其制备方法。
本发明的含钴掺杂二氧化硅纳米复合磨粒溶胶，由质量百分数为0.43wt％的硝酸钴溶液和2.5wt％的硅酸溶液按1:1的质量比，同时加入1wt％氢氧化钠，通过共沉淀法沉淀在二氧化硅晶种上反应制成，所述的溶胶中的纳米复合磨粒呈均匀球形，所述的钴掺杂二氧化硅纳米复合磨粒溶胶中的氢氧化钴掺杂量为0.1wt％-5wt％。溶胶体系稳定，可以稳定存放六个月以上。
优选地，
所述的溶胶中的氢氧化钴掺杂量为0.5-1.5wt％。
所述的溶胶中纳米复合磨粒的粒径为20-150纳米。
优选地，
所述的溶胶中纳米复合磨粒的粒径为106-123纳米。
所述的含钴掺杂二氧化硅纳米复合磨粒溶胶的制备方法如下：先用阳离子交换法制备pH值为2.5、质量分数为2.5％的硅酸。在100℃和搅拌条件下，硅酸、0.43wt％的硝酸钴溶液和1wt％氢氧化钠分别加入二氧化硅晶种中进行生长,氢氧化钠控制整个溶胶体系pH值保持在10，控制硝酸钴和硅酸混合物的滴加速度保持溶胶体系中蒸发速度和滴加速度相平衡。
优选地，
所述的掺杂反应时间为140分钟-420分钟。通过控制掺杂反应时间，可制得不同钴掺杂量的二氧化硅纳米复合磨粒溶胶体系。
一种抛光液组合物，组成及质量百分含量如下：
Figure PCTCN2015095184-appb-000001
Figure PCTCN2015095184-appb-000002
以上各组成的质量百分含量之和为100％。
优选地，
所述的抛光液组合物，组成及质量百分含量如下：
Figure PCTCN2015095184-appb-000003
以上各组成的质量百分含量之和为100％。
本发明的含钴掺杂二氧化硅纳米复合磨粒溶胶中的纳米复合磨粒的结构为内部为纯的二氧化硅晶种，外层长大的部分为氢氧化钴和二氧化硅掺杂在一起的部分。外层氢氧化钴和蓝宝石表层的氧化铝发生化学反应，从而提高对蓝宝石的去除率。同时氢氧化钴硬度比二氧化硅小，可以降低对蓝宝石表面的磨损，降低表面粗糙度。这样设计的磨粒可同时达到“高速率、低粗糙度”抛光的目的。采用本发明提供的抛光液对蓝宝石基片进行抛光，可以有效地提高蓝宝石表面去除率，降低蓝宝石表面的粗糙度。
具体实施方式
下面用一些实例对本发明的实施方案作进一步说明，但本发明不受这些具体实施例的限制。
实施例1
本实施例的含钴掺杂二氧化硅纳米复合磨粒溶胶采用共沉淀法制备。制备过程为：先用阳离子交换法制备pH值为2.5，然后2.5wt％的硅酸、0.43wt％的Co(NO3)2·6H2O溶液以等质量比，在100℃搅拌条件下，和1wt％氢氧化钠一起分别加入二氧化硅晶种中。氢氧化钠控制整个溶胶体系pH 值保持在10，控制硝酸钴和硅酸混合物的滴加速度保持溶胶体系中蒸发速度和滴加速度相平衡。分别滴加140分钟，280分钟，420分钟，制得氢氧化钴掺杂量为0.5wt％，1.0wt％，1.5wt％的含钴掺杂二氧化硅纳米复合磨粒溶胶。
实施例2
将氢氧化钴掺杂量为0.5wt％的溶胶加去离子水稀释到3L，固含量为10％。钴掺杂二氧化硅的复合磨粒粒径为106纳米，溶胶最终pH值为10。用350目的滤筛过滤之后，加入1％分散剂焦磷酸钠、0.5％表面活性剂十二烷基聚氧乙烯醚，得抛光液。
实施例3
氢氧化钴掺杂量为1.0wt％的溶胶加去离子水稀释到3L，固含量为10％。钴掺杂二氧化硅的复合磨粒粒径为110纳米，溶胶最终pH值为10。用350目的滤筛过滤之后，加入1％分散剂焦磷酸钠、0.5％表面活性剂十二烷基聚氧乙烯醚，得抛光液。
实施例4
氢氧化钴掺杂量为1.5wt％的溶胶加去离子水稀释到3L，固含量为10％。钴掺杂二氧化硅的复合磨粒粒径为123纳米，溶胶最终pH值为10.5。用350目的滤筛过滤之后，加入1％分散剂焦磷酸钠、0.5％表面活性剂十二烷基聚氧乙烯醚，得抛光液。
对照例1
未掺杂的纯硅溶胶加去离子水稀释到3L，固含量为10％，二氧化硅颗粒为95纳米，稀释后pH值为10。用350目的滤筛过滤之后，加入1％分散剂焦磷酸钠、0.5％表面活性剂十二烷基聚氧乙烯醚，得抛光液。
抛光试验：使用上述各抛光液在一定抛光条件下对蓝宝石基片进行抛 光试验。抛光条件如下：
抛光机：UNIPOL-1502单面抛光机
工件：直径为50.8mm的蓝宝石c(0001)面
抛光垫：聚氨酯材料、RODEL生产
抛光压力：6公斤
下盘转速：60rpm
抛光时间：120分钟
抛光后，接着洗涤和干燥基片，然后测量基片的表面形貌特征。表面平均粗糙度(Ra)用AmbiosXI-100表面形貌仪测试，其分辨力为0.1埃。测试范围为93.5μm′93.5μm。基片重量用分析天平称量，抛光前后重量差除以抛光时间为抛光速率。
各实施例抛光液的抛光效果分别见表1。可见，与对照例1(纯硅溶胶)相比，含有钴掺复合磨粒的溶胶(实施例1、2、3)对蓝宝石基片抛光之后，均提高了抛光速度，并降低了蓝宝石表面的粗糙度。
表1各实施例抛光液对蓝宝石基片的抛光效果
  实施例1 实施例2 实施例3 对照例1
抛光速率mg/h 6.55 8.40 6.75 4.55
Ra，nm 1.538 1.612 1.564 2.541

Claims (8)

  1. 含钴掺杂二氧化硅纳米复合磨粒溶胶，其特征在于，由质量百分数为0.43wt％的硝酸钴溶液和2.5wt％的硅酸溶液按1:1的质量比，同时加入1wt％氢氧化钠，通过共沉淀法沉淀在二氧化硅晶种上反应制成，所述的溶胶中的纳米复合磨粒呈均匀球形，所述的溶胶中的氢氧化钴掺杂量为0.1wt％-5wt％。
  2. 根据权利要求2所述的含钴掺杂二氧化硅纳米复合磨粒溶胶，其特征在于，所述的溶胶中的氢氧化钴掺杂量为0.5-1.5wt％。
  3. 根据权利要求1所述的含钴掺杂二氧化硅纳米复合磨粒溶胶，其特征在于，所述的溶胶中纳米复合磨粒的粒径为20-150纳米。
  4. 根据权利要求3所述的含钴掺杂二氧化硅纳米复合磨粒溶胶，其特征在于，所述的溶胶中纳米复合磨粒的粒径为106-123纳米。
  5. 如权利要求1-4中任意一种含钴掺杂二氧化硅纳米复合磨粒溶胶的制备方法，其特征在于，步骤如下：先用阳离子交换法制备pH值为2.5、质量分数为2.5％的硅酸。在100℃和搅拌条件下，硅酸、0.43wt％的硝酸钴溶液和1wt％氢氧化钠分别加入二氧化硅晶种中进行生长,氢氧化钠控制整个溶胶体系pH值保持在10，控制硝酸钴和硅酸混合物的滴加速度保持溶胶体系中蒸发速度和滴加速度相平衡。
  6. 根据权利要求5所述的含钴掺杂二氧化硅纳米复合磨粒溶胶的制备方法，其特征在于，所述的掺杂反应时间为140分钟-420分钟。
  7. 含有如权利要求1-4中任意一种含钴掺杂二氧化硅纳米复合磨粒溶胶的抛光液组合物，其特征在于，组成及质量百分含量如下：
    Figure PCTCN2015095184-appb-100001
    以上各组成的质量百分含量之和为100％。
  8. 根据权利要求7所述的抛光液组合物，其特征在于，组成及质量百分含量如下：
    Figure PCTCN2015095184-appb-100002
    以上各组成的质量百分含量之和为100％。
PCT/CN2015/095184 2015-03-23 2015-11-20 含钴掺杂二氧化硅纳米复合磨粒溶胶、抛光液及其制备方法 WO2016150176A1 (zh)

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