CN101857775B - Lithium niobate crystal polishing solution and preparation method thereof - Google Patents
Lithium niobate crystal polishing solution and preparation method thereof Download PDFInfo
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- 238000005498 polishing Methods 0.000 title claims abstract description 67
- 239000013078 crystal Substances 0.000 title claims abstract description 37
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 48
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 239000007800 oxidant agent Substances 0.000 claims abstract description 15
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 11
- 239000013543 active substance Substances 0.000 claims abstract description 10
- 239000012452 mother liquor Substances 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims description 23
- 150000001412 amines Chemical class 0.000 claims description 16
- 239000000084 colloidal system Substances 0.000 claims description 12
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 11
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- CEJLBZWIKQJOAT-UHFFFAOYSA-N dichloroisocyanuric acid Chemical group ClN1C(=O)NC(=O)N(Cl)C1=O CEJLBZWIKQJOAT-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 229910013641 LiNbO 3 Inorganic materials 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 150000002191 fatty alcohols Chemical class 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000008139 complexing agent Substances 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 230000000087 stabilizing effect Effects 0.000 claims description 3
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 claims description 3
- 239000003085 diluting agent Substances 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- -1 polyoxyethylene vinyl ether Polymers 0.000 claims description 2
- 239000002585 base Substances 0.000 claims 3
- 239000003513 alkali Substances 0.000 claims 1
- 230000003746 surface roughness Effects 0.000 abstract description 4
- 235000012431 wafers Nutrition 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000007517 polishing process Methods 0.000 description 4
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- BVTJGGGYKAMDBN-UHFFFAOYSA-N Dioxetane Chemical compound C1COO1 BVTJGGGYKAMDBN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
一种铌酸锂晶体抛光液及制备方法，其特征是，包括以下成分及其重量百分含量：二氧化硅为5～50，pH值调节剂为0.5～5，醚醇类活性剂为0.02～2，氧化剂为0.5～5，分散剂为0.1～10，去离子水为余量；所述二氧化硅以硅溶胶的状态加入或者以所述二氧化硅的硅溶胶为母液配制抛光液。所述抛光液是一种操作简单，制备方便，并且化学作用强、抛光效率高、表面粗糙度低、无划伤的、可专用于铌酸锂晶体的抛光液。A lithium niobate crystal polishing liquid and a preparation method thereof, characterized in that it comprises the following components and their weight percentages: 5-50 for silicon dioxide, 0.5-5 for a pH regulator, and 0.02 for an ether alcohol active agent ~2, the oxidizing agent is 0.5~5, the dispersant is 0.1~10, and deionized water is the balance; the silicon dioxide is added in the state of silica sol or the polishing liquid is prepared by using the silica sol of silicon dioxide as the mother liquor. The polishing liquid is simple to operate, convenient to prepare, has strong chemical action, high polishing efficiency, low surface roughness, no scratches, and can be specially used for lithium niobate crystals.
Description
技术领域 technical field
本发明涉及化学机械抛光技术领域，特别是一种铌酸锂晶体抛光液及制备方法。所述铌酸锂晶体的分子式为LiNbO3，简称LN。在表面超精密加工方面，铌酸锂晶片的抛光性能不同于硅片的抛光性能，也就是说，用于硅片的抛光液不能用作铌酸锂晶片的抛光液The invention relates to the technical field of chemical mechanical polishing, in particular to a lithium niobate crystal polishing liquid and a preparation method thereof. The molecular formula of the lithium niobate crystal is LiNbO 3 , referred to as LN. In terms of surface ultra-precision machining, the polishing performance of lithium niobate wafers is different from that of silicon wafers, that is, the polishing fluid used for silicon wafers cannot be used as a polishing fluid for lithium niobate wafers
背景技术 Background technique
铌酸锂晶体(分子式LiNbO3，简称LN)是一种具有铁电、压电、热电、电光、声电和光折变效应等多种性质的功能材料。由于它具有较高的机电耦合系数、优良的温度稳定性、低声学传输损耗等特点，所以广泛用于制作高频、宽带表面滤波器件中，而且其优良的电压、电光、非线性光学特性，使得它在超声器件、光开关、调制器、滤波器、二次谐波发生和光参量振荡器等方面获得应用。随着科学技术的不断发展，这种具有延迟温度系数小、机电耦合系数大、体波抑制深的优质LN晶体将会具有更广阔的国内、国际市场。Lithium niobate crystal (molecular formula LiNbO 3 , referred to as LN) is a functional material with various properties such as ferroelectric, piezoelectric, pyroelectric, electro-optic, acoustoelectric and photorefractive effects. Because of its high electromechanical coupling coefficient, excellent temperature stability, and low acoustic transmission loss, it is widely used in the production of high-frequency, broadband surface filter devices, and its excellent voltage, electro-optic, and nonlinear optical properties , making it widely used in ultrasonic devices, optical switches, modulators, filters, second harmonic generation and optical parametric oscillators. With the continuous development of science and technology, this kind of high-quality LN crystal with small delay temperature coefficient, large electromechanical coupling coefficient and deep body wave suppression will have a broader domestic and international market.
随着光电子技术的高速发展，新型高性能、高精密、高集成的光电子系统不断涌现，对抛光技术提出了更高的要求。为保证器件的性能，对晶体表面的完整性及精度提出了严格要求，即表面无缺陷、无变质层，晶体结构完整，表面超光滑。目前化学机械抛光(ChemicalMechanical Polishing，简称CMP)技术是获得光滑无损伤表面最有效的方法之一。采用抛光液的化学作用和磨料的机械去除作用相结合的抛光方法，可以高效率获得高质量的抛光表面。但是，由于铌酸锂晶体的硬度较低(莫氏5)，因此在加工过程中容易产生划伤、塌边等缺陷，且具有韧性高，加工速度慢；对温度具有敏感性，易产生微畴反转；尤其易产生角度很小的尖劈碎晶，从而产生砂道、潜划伤等缺陷，在后继使用过程中可能会造成较大损失。因此，系统研究铌酸锂晶片抛光加工工艺，以及铌酸锂晶体专用型抛光液的研发，变的更加迫切！本发明正是鉴于此需求，通过一系列抛光实验，确定了实用有效的铌酸锂晶体抛光液及制备方法。With the rapid development of optoelectronic technology, new high-performance, high-precision, and highly integrated optoelectronic systems are emerging, which put forward higher requirements for polishing technology. In order to ensure the performance of the device, strict requirements are put forward for the integrity and precision of the crystal surface, that is, there is no defect on the surface, no metamorphic layer, the crystal structure is complete, and the surface is ultra-smooth. At present, chemical mechanical polishing (CMP) technology is one of the most effective methods to obtain a smooth and damage-free surface. The polishing method combining the chemical action of the polishing liquid and the mechanical removal of the abrasive can obtain a high-quality polished surface with high efficiency. However, due to the low hardness of lithium niobate crystals (Mohs 5), defects such as scratches and edge collapse are prone to occur during processing, and they have high toughness and slow processing speed; they are sensitive to temperature and prone to micro Domain inversion; in particular, it is easy to produce wedge crystals with small angles, resulting in defects such as sand roads and latent scratches, which may cause greater losses in the subsequent use process. Therefore, it is more urgent to systematically study the polishing process of lithium niobate wafers and the development of special polishing fluid for lithium niobate crystals! In view of this requirement, the present invention determines a practical and effective lithium niobate crystal polishing liquid and a preparation method through a series of polishing experiments.
发明内容 Contents of the invention
本发明针对在铌酸锂晶体抛光过程中，抛光速率低，易出现划伤，塌边等问题，提供一种铌酸锂晶体抛光液及制备方法。所述抛光液是一种操作简单，制备方便，并且化学作用强、抛光效率高、表面粗糙度低、无划伤的、可专用于铌酸锂晶体的抛光液。The invention provides a lithium niobate crystal polishing liquid and a preparation method aiming at the problems of low polishing rate, easy scratches, edge collapse and the like during the polishing process of lithium niobate crystals. The polishing liquid is simple to operate, convenient to prepare, has strong chemical action, high polishing efficiency, low surface roughness, no scratches, and can be specially used for lithium niobate crystals.
本发明的技术方案如下：Technical scheme of the present invention is as follows:
一种铌酸锂晶体抛光液，其特征是，包括以下成分及其重量百分含量：二氧化硅为5～50，pH值调节剂为0.5～5，醚醇类活性剂为0.02～2，氧化剂为0.5～5，分散剂为0.1～10，去离子水为余量；所述二氧化硅以硅溶胶的状态加入或者以所述二氧化硅的硅溶胶为母液配制抛光液。A lithium niobate crystal polishing liquid, characterized in that it comprises the following components and their weight percentages: 5-50 for silicon dioxide, 0.5-5 for a pH regulator, 0.02-2 for an ether alcohol active agent, The oxidizing agent is 0.5-5, the dispersant is 0.1-10, and deionized water is the balance; the silicon dioxide is added in the state of silica sol or the polishing liquid is prepared by using the silica sol of silicon dioxide as a mother liquor.
所述硅溶胶中二氧化硅胶团颗粒的粒径为30～150nm，所述二氧化硅胶团颗粒在所述硅溶胶中的重量百分含量为1～50。The particle diameter of the silica colloid particles in the silica sol is 30-150 nm, and the weight percentage of the silica colloid particles in the silica sol is 1-50.
所述硅溶胶中二氧化硅胶团颗粒的粒径为40～70nm，所述二氧化硅胶团颗粒在所述硅溶胶中的重量百分含量为1～50。The particle size of the silica colloid particles in the silica sol is 40-70 nm, and the weight percentage of the silica colloid particles in the silica sol is 1-50.
所述pH值调节剂包括KOH和有机胺碱的混合液，所述KOH和有机胺碱的重量比为1～5∶1；所述KOH参与以下化学反应：KOH+LiNbO3→LiOH+KNbO3；所述有机胺碱不仅具有稳定抛光液pH值的作用，而且具有络合剂的作用。The pH regulator includes a mixed solution of KOH and an organic amine base, the weight ratio of the KOH and the organic amine base is 1-5:1; the KOH participates in the following chemical reaction: KOH+LiNbO 3 →LiOH+KNbO 3 ; The organic amine base not only has the effect of stabilizing the pH value of the polishing solution, but also has the effect of complexing agent.
所述有机胺碱包括以下物质中的一种或多种：乙二胺，三乙胺，氢氧化四乙基胺。The organic amine base includes one or more of the following substances: ethylenediamine, triethylamine, tetraethylamine hydroxide.
所述醚醇类活性剂包括以下物质中的一种或多种：非离子表面活性剂，脂肪醇聚氧乙烯醚，壬基酚聚氧乙烯醚，烷基酚聚氧乙烯醚，阴离子聚丙烯酸盐。The ether alcohol active agent includes one or more of the following substances: nonionic surfactant, fatty alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, anionic polyacrylic acid Salt.
所述氧化剂为二氯异氰尿酸钠，其分子式为C3Cl2N3O3Na；所述二氯异氰尿酸钠也被称为优氯净。The oxidizing agent is sodium dichloroisocyanurate, whose molecular formula is C 3 Cl 2 N 3 O 3 Na; the sodium dichloroisocyanurate is also called euchlorozine.
所述分散剂包括以下物质中的一种或多种：聚乙二醇，聚乙烯醇，聚丙烯酸盐。The dispersant includes one or more of the following substances: polyethylene glycol, polyvinyl alcohol, polyacrylate.
一种铌酸锂晶体抛光液的制备方法，其特征是，包括以下步骤：A kind of preparation method of lithium niobate crystal polishing fluid is characterized in that, comprises the following steps:
(1)根据上述抛光液的成分及其重量百分含量备料；(1) prepare materials according to the composition of the above-mentioned polishing liquid and the weight percentage thereof;
(2)将硅溶胶和去离子水进行混合，或者以硅溶胶为母液，向母液中加入去离子水，形成硅溶胶稀释液；(2) mixing silica sol and deionized water, or using silica sol as mother liquor, adding deionized water to mother liquor to form silica sol dilution;
(3)在搅拌的条件下，向硅溶胶稀释液中依次加入醚醇类表面活性剂、分散剂、氧化剂和pH值调节剂。(3) Add ether alcohol surfactant, dispersant, oxidizing agent and pH regulator to the silica sol diluent sequentially under the condition of stirring.
本发明的技术效果如下：Technical effect of the present invention is as follows:
本发明是一种化学机械抛光液，主要应用于铌酸锂晶体的超精密加工，能够获得纳米级超光滑表面，其中含有研磨颗粒和水，其还含有下述成分中的一种或多种：聚乙二醇脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚等抛光助剂。该抛光液的配制方法简单，例如：取30％硅溶胶母液，用去离子水稀释，在搅拌的条件下，加入一定比例的氧化剂(0.5～5％)、分散剂(0.1～10％)、表面活性剂(0.02～2％)、pH值调节剂(0.5～5)，混合搅拌均匀。在相应的抛光工艺条件下进行抛光，可实现铌酸锂晶片的超精密加工，满足了不同应用领域对铌酸锂晶体表面质量的要求。本发明具有成本低、效率高、表面质量好、易清洗以及低腐蚀性等优点。The invention is a chemical mechanical polishing liquid, which is mainly used in the ultra-precision processing of lithium niobate crystals, and can obtain nano-scale ultra-smooth surfaces, which contains abrasive particles and water, and also contains one or more of the following components : Polyethylene glycol fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether and other polishing aids. The preparation method of the polishing liquid is simple, for example: take 30% silica sol mother liquid, dilute it with deionized water, add a certain proportion of oxidant (0.5-5%), dispersant (0.1-10%), Surfactant (0.02-2%), pH regulator (0.5-5), mixed and stirred evenly. Polishing under the corresponding polishing process conditions can realize ultra-precision machining of lithium niobate wafers, and meet the requirements of different application fields for the surface quality of lithium niobate crystals. The invention has the advantages of low cost, high efficiency, good surface quality, easy cleaning and low corrosion.
具体实施方式 Detailed ways
一种铌酸锂晶体抛光液，包括以下成分及其重量百分含量：二氧化硅为5～50，pH值调节剂为0.5～5，醚醇类活性剂为0.02～2，氧化剂为0.5～5，分散剂为0.1～10，去离子水为余量；所述二氧化硅以硅溶胶的状态加入。所述硅溶胶中二氧化硅胶团颗粒的粒径为30～150nm，所述二氧化硅胶团颗粒在所述硅溶胶中的重量百分含量为1～50。所述硅溶胶中二氧化硅胶团颗粒的粒径为40～70nm，所述二氧化硅胶团颗粒在所述硅溶胶中的重量百分含量为1～50。所述pH值调节剂包括KOH和有机胺碱的混合液，所述KOH和有机胺碱的重量比为1～5∶1；所述KOH参与以下化学反应：KOH+LiNbO3→LiOH+KNbO3；所述有机胺碱不仅具有稳定抛光液pH值的作用，而且具有络合剂的作用。所述有机胺碱包括以下物质中的一种或多种：乙二胺，三乙胺，氢氧化四乙基胺。所述醚醇类活性剂包括以下物质中的一种或多种：非离子表面活性剂，脂肪醇聚氧乙烯醚，壬基酚聚氧乙烯醚，烷基酚聚氧乙烯醚，阴离子聚丙烯酸盐。所述氧化剂为二氯异氰尿酸钠，其分子式为C3Cl2N3O3Na；所述二氯异氰尿酸钠也被称为优氯净。所述分散剂包括以下物质中的一种或多种：聚乙二醇，聚乙烯醇，聚丙烯酸盐。A lithium niobate crystal polishing liquid, comprising the following components and their weight percentages: 5-50 for silicon dioxide, 0.5-5 for a pH regulator, 0.02-2 for an ether alcohol active agent, and 0.5-2 for an oxidant 5. The dispersant is 0.1-10, and the balance is deionized water; the silicon dioxide is added in the state of silica sol. The particle diameter of the silica colloid particles in the silica sol is 30-150 nm, and the weight percentage of the silica colloid particles in the silica sol is 1-50. The particle diameter of the silica colloid particles in the silica sol is 40-70 nm, and the weight percentage of the silica colloid particles in the silica sol is 1-50. The pH regulator includes a mixed solution of KOH and an organic amine base, the weight ratio of the KOH and the organic amine base is 1-5:1; the KOH participates in the following chemical reaction: KOH+LiNbO 3 →LiOH+KNbO 3 ; The organic amine base not only has the effect of stabilizing the pH value of the polishing solution, but also has the effect of complexing agent. The organic amine base includes one or more of the following substances: ethylenediamine, triethylamine, tetraethylamine hydroxide. The ether alcohol active agent includes one or more of the following substances: nonionic surfactant, fatty alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, anionic polyacrylic acid Salt. The oxidizing agent is sodium dichloroisocyanurate, whose molecular formula is C 3 Cl 2 N 3 O 3 Na; the sodium dichloroisocyanurate is also called euchlorozine. The dispersant includes one or more of the following substances: polyethylene glycol, polyvinyl alcohol, polyacrylate.
一种铌酸锂晶体抛光液的制备方法，其特征是，包括以下步骤：(1)根据上述抛光液的成分及其重量百分含量备料；(2)将硅溶胶和去离子水进行混合，或者以硅溶胶为母液，向母液中加入去离子水，形成硅溶胶稀释液；(3)在搅拌的条件下，向硅溶胶稀释液中依次加入醚醇类表面活性剂、分散剂、氧化剂和pH值调节剂。A kind of preparation method of lithium niobate crystal polishing fluid is characterized in that, comprises the following steps: (1) according to the composition of above-mentioned polishing fluid and its weight percent content preparation; (2) silica sol and deionized water are mixed, Or take silica sol as mother liquor, add deionized water in mother liquor, form silica sol dilution; (3) under the condition of stirring, add ether alcohol surfactant, dispersant, oxidizing agent and pH regulator.
本发明是为了解决在铌酸锂晶体抛光过程中，抛光速率低，易出现划伤，塌边等问题，从而公开了一种操作简单，制备方便，化学作用强、抛光效率高、表面粗糙度低、无划伤的铌酸锂晶体专用抛光液。The invention aims to solve the problems of low polishing rate, prone to scratches and edge collapse during the polishing process of lithium niobate crystals, thereby disclosing a method with simple operation, convenient preparation, strong chemical action, high polishing efficiency and excellent surface roughness. Low and scratch-free polishing fluid for lithium niobate crystals.
本发明铌酸锂晶体抛光液，其特征是，所属的抛光液成分和重量百分比组成如下：Lithium niobate crystal polishing liquid of the present invention is characterized in that, the belonging polishing liquid composition and weight percent composition are as follows:
硅溶胶5～50； pH值调节剂0.5～5 醚醇类活性剂0.02～2Silica sol 5~50; pH adjuster 0.5~5 Ether alcohol active agent 0.02~2
氧化剂0.5～5； 分散剂0.1～10 去离子水余量。Oxidant 0.5-5; Dispersant 0.1-10 Deionized water balance.
本发明所述硅溶胶是粒径40～70nm的二氧化硅溶胶，其浓度为1～50％。The silica sol in the present invention is a silica sol with a particle diameter of 40-70 nm, and its concentration is 1-50%.
本发明所述的pH调节剂为KOH溶液和有机胺碱的混合液，KOH和有机胺碱的比例为1～5∶1。The pH regulator of the present invention is a mixed liquid of KOH solution and organic amine base, and the ratio of KOH and organic amine base is 1-5:1.
本发明所述的醚醇类活性剂是非离子活性剂，如非离子表面活性剂，脂肪醇聚氧乙烯醚(0～10)、壬基酚聚氧乙烯醚、烷基酚聚氧乙烯醚、阴离子聚丙烯酸盐中的一种。The ether alcohol active agent described in the present invention is nonionic active agent, as nonionic surfactant, fatty alcohol polyoxyethylene ether (0～10), nonylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, One of the anionic polyacrylates.
本发明铌酸锂晶体抛光液的制备方法，包括以下步骤(组分为重量百分比)：The preparation method of lithium niobate crystal polishing liquid of the present invention comprises the following steps (component is weight percent):
(1)将粒径40～70nm的硅溶胶用去离子水稀释，去离子水含量75～80％；(1) Dilute the silica sol with a particle size of 40-70nm with deionized water, and the deionized water content is 75-80%;
(2)在搅拌的条件下，向其中加入0.02～2％的醚醇类表面活性剂；(2) under the condition of stirring, add 0.02～2% ether alcohol surfactant wherein;
(3)在搅拌的条件下，向其中加入0.5～5％的氧化剂；(3) under the condition of stirring, add 0.5～5% oxidizing agent thereinto;
(4)在搅拌的条件下，向其中加入0.5～5％pH值调节剂，搅拌均匀即可使用。(4) Under the condition of stirring, add 0.5-5% pH regulator thereinto, stir evenly and use it immediately.
本发明具有如下优点：The present invention has the following advantages:
1.选用复合碱，KOH和有机胺碱，KOH能够增强抛光液的化学作用，发生的反应方程式为：KOH+LiNbO3→LiOH+KNbO3 1. Choose compound base, KOH and organic amine base, KOH can enhance the chemical action of polishing liquid, the reaction equation is: KOH+LiNbO 3 →LiOH+KNbO 3
有机胺碱作为抛光液pH调节剂，能够很好的保持溶液的pH值稳定，确保化学作用的一致稳定，从而实现抛光速率的稳定，同时还能起到络合剂的作用，有助于抛光产物从晶体表面脱离，提高了抛光效率。Organic amine base is used as the pH regulator of the polishing solution, which can keep the pH value of the solution stable and ensure the consistency and stability of the chemical action, so as to achieve the stability of the polishing rate. The product is detached from the crystal surface, improving the polishing efficiency.
2.选用表面活性剂，增强了高低选择比，大大降低了表面张力、减少了损伤层，提高了质量传输速率，增强运输过程，达到高平整高光洁表面。2. The use of surfactants enhances the high-low selectivity ratio, greatly reduces surface tension, reduces damaged layers, improves mass transmission rate, enhances the transportation process, and achieves a high-level, high-gloss surface.
3.本发明为碱性抛光液，具有对抛光设备无腐蚀，对环境无污染，稳定性好。3. The present invention is an alkaline polishing liquid, which has no corrosion to polishing equipment, no pollution to the environment, and good stability.
4.选用纳米SiO2溶胶作为抛光液磨料，其粒径小(40～70nm)，硬度低(对LN晶体低损伤)，分散性好(易清洗)，提高了抛光表面的一致性，能够达到高速率高平整低损伤抛光、污染小，解决了目前金刚石磨料硬度大易划伤、易沉淀等诸多弊端。4. Nano-SiO 2 sol is selected as the polishing liquid abrasive, which has small particle size (40-70nm), low hardness (low damage to LN crystal), good dispersion (easy to clean), improves the consistency of the polished surface, and can achieve High-speed, high-level, low-damage polishing, low pollution, solves many disadvantages of the current diamond abrasives, such as high hardness, easy scratching, and easy precipitation.
下面通过实施例的方式进一步说明本发明，但并不因此将本发明限制在所属的实施例范围之中。The present invention is further illustrated below by means of examples, but the present invention is not limited to the scope of the examples.
本发明抛光液实施例1～实施例4的成分和含量如下：The composition and content of polishing liquid embodiment 1～embodiment 4 of the present invention are as follows:
以实施例1来描述本发明的制备过程：Describe the preparation process of the present invention with embodiment 1:
取570g的二氧化硅胶体，粒径为40～50nm，固含量为20％，在不断搅拌下，依次加入氧化剂二氯异氰尿酸钠(俗称优氯净)1.5g，表面活性剂脂肪醇聚氧乙烯醚0.5g，分散剂聚乙二醇(PEG2000)2.0g，去离子水1400g，最后加入KOH，调节溶液pH＝10.0，便制得了本发明的抛光液。用配好的抛光液进行抛光实验，在Logitech PM5精密研磨抛光机上，对2inch铌酸锂晶片进行实验，压力350g/cm2，抛光盘转速是60r/min，抛光液流量5ml/min。用ZYG05022测抛光后的铌酸锂晶片表面的粗糙度，测量结果为8.574埃，采用SartorisuCP225D型精密电子天平(精度0.01mg)，对抛光前后晶片称重计算器材料去除率为673nm/min。Take 570g of colloidal silica, the particle size is 40-50nm, and the solid content is 20%. Under continuous stirring, add 1.5g of oxidizing agent sodium dichloroisocyanurate (commonly known as Youchlorozine) and surfactant fatty alcohol polysaccharide. Oxyethylene ether 0.5g, dispersant polyethylene glycol (PEG2000) 2.0g, deionized water 1400g, and finally KOH was added to adjust the pH of the solution to 10.0 to prepare the polishing solution of the present invention. The polishing experiment was carried out with the prepared polishing liquid. On the Logitech PM5 precision grinding and polishing machine, the experiment was carried out on the 2inch lithium niobate wafer, the pressure was 350g/cm 2 , the rotational speed of the polishing disc was 60r/min, and the flow rate of the polishing liquid was 5ml/min. The surface roughness of the polished lithium niobate wafer was measured with ZYG05022, and the measurement result was 8.574 angstroms. The Sartorisu CP225D precision electronic balance (accuracy 0.01mg) was used, and the material removal rate of the wafer weighing calculator before and after polishing was 673nm/min.
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