技术领域technical field
本发明涉及蓝宝石研磨技术领域，特别是一种高效碳化硼研磨液及其配制方法。The invention relates to the technical field of sapphire grinding, in particular to a high-efficiency boron carbide grinding liquid and a preparation method thereof.
背景技术Background technique
蓝宝石玻璃，类似钢玉成分,硬度为9,它的优点是较普通玻璃硬度更高，有着很好的热特性，极好的电气特性和介电特性，并且防化学腐蚀，它耐高温，导热好，硬度高，透红外，化学稳定性好，因此，常用它来代替其它光学材料制作光学元件、透红外线光学窗片等，被广泛地应用于红外及远红外军用装备方面，并用于制作高档手表的表镜和手机触摸屏。Sapphire glass, similar to corundum, has a hardness of 9. Its advantages are higher hardness than ordinary glass, good thermal properties, excellent electrical and dielectric properties, and chemical corrosion resistance. It is resistant to high temperature and conducts heat. Good, high hardness, infrared transmission, and good chemical stability. Therefore, it is often used to replace other optical materials to make optical elements, infrared optical windows, etc. It is widely used in infrared and far infrared military equipment, and is used to make high-grade The mirror of the watch and the touch screen of the mobile phone.
在蓝宝石加工行业内，A向和M向蓝宝石加工难度大于C向蓝宝石，一般碳化硼研磨液加工时间长，去除速率低，机械损耗大，增加了机器和人工成本。In the sapphire processing industry, A-direction and M-direction sapphires are more difficult to process than C-direction sapphires. Generally, the processing time of boron carbide abrasives is long, the removal rate is low, and the mechanical loss is large, which increases the cost of machines and labor.
中国专利(专利申请号为201110097782.1)公开的“蓝宝石衬底片粗磨研磨液及其配制方法”，其“蓝宝石衬底片粗磨研磨液”是由碳化硼、水和悬浮液组成,碳化硼、水和悬浮液的重量比＝2∶4∶1,所述悬浮液由分散剂、悬浮剂和防锈剂组成,分散剂、悬浮剂和防锈剂的重量比＝2∶5∶1,所述分散剂为高分子有机醇,所述悬浮剂为高分子化合物,所述防锈剂为碱。Chinese patent (patent application No. 201110097782.1) discloses "Sapphire Substrate Rough Grinding Liquid and Its Preparation Method", and its "Sapphire Substrate Rough Grinding Liquid" is composed of boron carbide, water and suspension, boron carbide, water The weight ratio=2:4:1 to the suspension, the suspension is made up of dispersant, suspending agent and antirust agent, the weight ratio=2:5:1 of dispersant, suspending agent and antirust agent, the described The dispersant is high molecular organic alcohol, the suspending agent is high molecular compound, and the antirust agent is alkali.
另一中国专利(专利申请号为201410102575.4)公开的“一种碳化硼精磨助磨剂及其使用方法”，该研磨液所述各材料按以下重量组份：分子量200-10000聚乙二醇40-70份、碳化硼10-15份、氢氧化钠5-10份、EDTA二钠1-3份、甘油1-3份、磷酸脂3-5份、烷基醇酰胺0.5-2份、余量为去离子水。Another Chinese patent (patent application number is 201410102575.4) discloses "a boron carbide fine grinding grinding aid and its use method". 40-70 parts, 10-15 parts of boron carbide, 5-10 parts of sodium hydroxide, 1-3 parts of disodium EDTA, 1-3 parts of glycerin, 3-5 parts of phosphate ester, 0.5-2 parts of alkanolamide, The balance is deionized water.
还有中国专利(专利申请号为201510645217.2)公开的“一种高效硅晶片研磨液”，该助磨剂使用醇胺类物质、酰胺类物质、无机盐、消泡剂和任选的水进行混合而制得，所述碳化硼精磨助磨剂在对碳化硼进行精磨时加入，能够提高浆料的固含量，提高磨矿效率，并使得到的碳化硼的粒径分布集中。There is also "a high-efficiency silicon wafer grinding liquid" disclosed in the Chinese patent (patent application number 201510645217.2). The grinding aid is mixed with alcohol amines, amides, inorganic salts, defoamers and optional water. The boron carbide fine grinding grinding aid is added when the boron carbide is finely ground, which can increase the solid content of the slurry, improve the grinding efficiency, and concentrate the particle size distribution of the obtained boron carbide.
发明内容Contents of the invention
本发明所要解决的技术问题是提供一种使用寿命长、稳定性好、能够提高A向和M向蓝宝石研磨速率、且所加工产品的表面平整度好的研磨液，并提供其配制方法。The technical problem to be solved by the present invention is to provide a long service life, good stability, can improve the grinding rate of A-direction and M-direction sapphire, and the surface smoothness of processed products is good, and provide its preparation method.
为解决上述技术问题，本发明所采取的技术方案是发明一种高效碳化硼研磨液，包括以下重量份的原料：In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is to invent a kind of high-efficiency boron carbide grinding liquid, comprising the raw materials of following parts by weight:
碳化硼微粉5-25分散剂1-2水性增稠剂0.5-1Boron carbide powder 5-25 dispersant 1-2 water-based thickener 0.5-1
防沉剂0.5-1增效剂0.5-5防锈剂0.5-1Anti-sedimentation agent 0.5-1 Synergist 0.5-5 Anti-rust agent 0.5-1
基底液65-92份；Base liquid 65-92 parts;
所述基底液采用纯水、异丙醇、多元醇中的一种或多种混合而成，当为多种时，各组分的配比为等重量份或其它比例。The base liquid is prepared by mixing one or more of pure water, isopropanol, and polyhydric alcohol. When there are more than one, the proportion of each component is equal parts by weight or other ratios.
所述的碳化硼微粉的粒径为5-45微米，莫氏硬度为9。The boron carbide micropowder has a particle size of 5-45 microns and a Mohs hardness of 9.
所述的分散剂为松油醇、聚氧乙烯醚、壬基酚聚氧乙烯醚、三乙醇胺中的一种或多种混合而成，当为多种时，各组分的配比为等重量份或其它比例。The dispersant is formed by mixing one or more of terpineol, polyoxyethylene ether, nonylphenol polyoxyethylene ether, and triethanolamine. When there are more than one, the proportion of each component is equal to parts by weight or other ratios.
所述的水性增稠剂为工业明胶、聚丙烯酸钠、聚丙烯酰胺、羧甲基纤维素纳中的一种或多种混合而成，当为多种时，各组分的配比为等重量份或其它比例。The water-based thickener is mixed with one or more of industrial gelatin, sodium polyacrylate, polyacrylamide, and sodium carboxymethyl cellulose. When there are multiple types, the proportion of each component is equal to parts by weight or other ratios.
所述的防沉剂为硅酸镁铝、柠檬酸钠、膨润土、气相二氧化硅中的一种或多种混合而成，当为多种时，各组分的配比为等重量份或其它比例。The anti-settling agent is formed by mixing one or more of magnesium aluminum silicate, sodium citrate, bentonite, and fumed silica. When there are more than one, the proportion of each component is equal parts by weight or other proportions.
所述的增效剂为氮氮二甲基甲酰胺、氮氮二甲基乙二胺、氮氮二甲基乙醇胺、氮氮二甲基乙酰胺中的一种或多种混合而成，当为多种时，各组分的配比为等重量份或其它比例。The synergist is a mixture of one or more of nitrogen nitrogen dimethylformamide, nitrogen nitrogen dimethylethylenediamine, nitrogen nitrogen dimethylethanolamine, nitrogen nitrogen dimethylacetamide, when When there are multiple types, the proportioning of each component is equal parts by weight or other proportions.
所述的防锈剂为二甲基硅油、矿物质油、食用油、工业白油中的一种或多种混合而成，当为多种时，各组分的配比为等重量份或其它比例。The antirust agent is formed by mixing one or more of simethicone oil, mineral oil, edible oil, and industrial white oil. other proportions.
与此同时，还提供一种高效碳化硼研磨液的配制方法，其配制步骤如下：At the same time, a preparation method of high-efficiency boron carbide grinding liquid is also provided, and the preparation steps are as follows:
A、先用纯水将碳化硼微粉清洗2-3次，洗去杂质离子，滤干，得滤干碳化硼微粉；A. First, clean the boron carbide micropowder with pure water for 2-3 times, wash away impurity ions, and filter dry to obtain boron carbide micropowder;
B、再将滤干碳化硼微粉与基底液混合均匀，用300-500目筛网过滤，去除大颗粒杂质，得混合液；B. Mix the dried boron carbide micropowder with the base solution evenly, filter with a 300-500 mesh screen to remove large particles of impurities, and obtain a mixed solution;
C、向混合液中加入分散剂和防沉剂，并置入密闭高速分散罐中，以1000-1200转/分钟的转速分散3-7min，得初混液；C. Add dispersant and anti-sedimentation agent to the mixed solution, put it into a closed high-speed dispersion tank, and disperse at a speed of 1000-1200 rpm for 3-7 minutes to obtain the initial mixed solution;
D、继续向密闭高速分散罐中的初混液中依次加入水性增稠剂、增效剂和防锈剂，以800-1000转/分钟的转速分散10-15min，即得高效碳化硼研磨液。D. Continue to add water-based thickener, synergist and anti-rust agent to the initial mixture in the closed high-speed dispersion tank, and disperse at a speed of 800-1000 rpm for 10-15 minutes to obtain a high-efficiency boron carbide grinding liquid.
本发明的高效碳化硼研磨液，由于加入了增效剂，应用在蓝宝石A向或M向研磨工艺中，使得研磨过程中研磨液与蓝宝石片表面发生化学反应，加速了研磨过程，提高了研磨速率，据测试，平均去除率达到4.5μm/min；使得蓝宝石晶片表面平整度大大提高，TTV≤1μm。The high-efficiency boron carbide grinding liquid of the present invention is applied in the A-direction or M-direction grinding process of sapphire due to the addition of a synergist, so that the chemical reaction between the grinding liquid and the surface of the sapphire sheet occurs during the grinding process, which accelerates the grinding process and improves the grinding efficiency. According to the test, the average removal rate reaches 4.5μm/min; the surface flatness of the sapphire wafer is greatly improved, and TTV≤1μm.
同时，本发明的高效碳化硼研磨液中还加入分散剂和防沉剂，使得碳化硼微粉能够长时间均匀地悬浮在基底液当中，进而提高了碳化硼研磨液的使用寿命，其应用在蓝宝石研磨加工中，可以连续加工6-8h，从而降低了蓝宝石的加工成本。At the same time, a dispersant and an anti-sedimentation agent are also added to the high-efficiency boron carbide grinding liquid of the present invention, so that the boron carbide micropowder can be uniformly suspended in the base liquid for a long time, thereby improving the service life of the boron carbide grinding liquid, which is used in sapphire During the grinding process, it can be processed continuously for 6-8 hours, thereby reducing the processing cost of sapphire.
另外，在配制方法中，还特别限定了各组成原料的添加顺序，即：先添加基底液，再添加分散剂和防沉剂，其次添加水性增稠剂和增效剂，最后添加防锈剂，因而，本发明的高效碳化硼研磨液的稳定性好，连续加工12-15盘，每盘的良率≥90％，大大提高了加工效率，降低了返工成本。In addition, in the preparation method, the order of adding the raw materials is also specially limited, that is: first add the base liquid, then add the dispersant and anti-sedimentation agent, then add the water-based thickener and synergist, and finally add the rust inhibitor , Therefore, the high-efficiency boron carbide grinding liquid of the present invention has good stability, can process 12-15 disks continuously, and the yield rate of each disk is ≥ 90%, which greatly improves the processing efficiency and reduces the cost of rework.
具体实施方式detailed description
以下结合实施例，对本发明作进一步的说明。下面的说明是采用例举的方式，但本发明的保护范围不应局限于此。Below in conjunction with embodiment, the present invention will be further described. The following description is by way of example, but the protection scope of the present invention should not be limited thereto.
下面的表1提供10组实施例，表中的数据为所用原料的重量份。The following Table 1 provides 10 groups of examples, and the data in the table are parts by weight of raw materials used.
表1中的各个实施例，其配制步骤如下：Each embodiment in table 1, its preparation steps are as follows:
A、先用纯水将碳化硼微粉清洗2-3次，洗去杂质离子，滤干，得滤干碳化硼微粉；A. First, clean the boron carbide micropowder with pure water for 2-3 times, wash away impurity ions, and filter dry to obtain boron carbide micropowder;
B、再将滤干碳化硼微粉与基底液混合均匀，用400目筛网过滤，去除大颗粒杂质，得混合液；B. Mix the dried boron carbide micropowder with the base liquid evenly, filter with a 400-mesh sieve, remove large particles of impurities, and obtain a mixed liquid;
C、向混合液中加入分散剂和防沉剂，并置入密闭高速分散罐中，以1100转/分钟的转速分散5min，得初混液；C. Add a dispersant and an anti-sedimentation agent to the mixed solution, put it into a closed high-speed dispersion tank, and disperse for 5 minutes at a speed of 1100 rpm to obtain an initial mixed solution;
D、继续向密闭高速分散罐中的初混液中依次加入水性增稠剂、增效剂和防锈剂，以900转/分钟的转速分散12min，即得高效碳化硼研磨液。D. Continue to add water-based thickener, synergist and anti-rust agent to the initial mixture in the closed high-speed dispersion tank in sequence, and disperse at a speed of 900 rpm for 12 minutes to obtain a high-efficiency boron carbide grinding liquid.
表1：实施例1-10所用原料的重量份Table 1: parts by weight of raw materials used in embodiments 1-10
采用上述实施例1配制出的高效碳化硼研磨液，对蓝宝石晶片进行研磨后，蓝宝石晶片表面平整度TTV、平均良率及去除率数据以及研磨过程的工艺条件如下：Adopt the high-efficiency boron carbide lapping liquid that above-mentioned embodiment 1 prepares, after sapphire wafer is ground, the process condition of sapphire wafer surface flatness TTV, average yield and removal rate data and grinding process are as follows:
研磨机：Presi1200；Grinder: Presi1200;
被研磨的晶片：蓝宝石A向4寸片；Polished wafer: sapphire A to 4-inch piece;
被研磨的晶片数量：32pics；The number of wafers to be ground: 32pics;
单位研磨压力：300g/cm2；Unit grinding pressure: 300g/cm2 ;
双面研磨速比：15:30:7:5；Double-sided grinding speed ratio: 15:30:7:5;
研磨时间：25min；Grinding time: 25min;
研磨液流量：400-600ml/min；Grinding fluid flow: 400-600ml/min;
研磨后，对蓝宝石晶片进行超声清洗、烘干、测量厚度。通过测厚仪测量蓝宝石晶片的厚度差来求去除数率，并对所有32pics被研磨的蓝宝石晶片进行测量，求取平均值得到去除率；用平整度测试仪对所有32pics被研磨的蓝宝石晶片进行测量，求取平均值得到平整度。After grinding, the sapphire wafer was ultrasonically cleaned, dried, and its thickness measured. Use a thickness gauge to measure the thickness difference of the sapphire wafer to calculate the removal rate, and measure all 32pics of ground sapphire wafers, and calculate the average value to obtain the removal rate; use a flatness tester to measure all 32pics of ground sapphire wafers Measure and calculate the average value to obtain the flatness.
检测结果显示，蓝宝石晶片经高效碳化硼研磨液研磨后，平均良率为94.5％，平均去除率为4.5μm/min，表面平整度TTV≤1，完全满足蓝宝石A向研磨工艺要求，并大大节省了加工成本。The test results show that after the sapphire wafer is ground by high-efficiency boron carbide grinding fluid, the average yield rate is 94.5%, the average removal rate is 4.5 μm/min, and the surface flatness TTV is ≤ 1, which fully meets the requirements of the sapphire A-direction grinding process and greatly saves processing costs.
采用上述实施例2-10配制出的高效碳化硼研磨液对蓝宝石晶片进行研磨后的效果见下面是表2。The effect of grinding the sapphire wafer with the high-efficiency boron carbide grinding liquid prepared in the above-mentioned Examples 2-10 is shown in Table 2 below.
表2：实施例2-10的研磨效果Table 2: Grinding Effects of Examples 2-10
本发明的高效碳化硼研磨液，适用于蓝宝石晶片加工的粗研磨。The high-efficiency boron carbide grinding fluid of the invention is suitable for rough grinding in sapphire wafer processing.
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| CN201610101314.XACN105505231A (en) | 2016-02-24 | 2016-02-24 | A kind of high-efficiency boron carbide grinding fluid and preparation method thereof |
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| CN201610101314.XACN105505231A (en) | 2016-02-24 | 2016-02-24 | A kind of high-efficiency boron carbide grinding fluid and preparation method thereof |
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| CN201610101314.XAPendingCN105505231A (en) | 2016-02-24 | 2016-02-24 | A kind of high-efficiency boron carbide grinding fluid and preparation method thereof |
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