CN114702033A - A kind of method for removing metal from polycrystalline diamond treated with electrolysis combined with acid - Google Patents
A kind of method for removing metal from polycrystalline diamond treated with electrolysis combined with acid Download PDFInfo
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 90
- 239000010432 diamond Substances 0.000 title claims abstract description 90
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 70
- 239000002184 metal Substances 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000002253 acid Substances 0.000 title claims abstract description 26
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 11
- 239000003792 electrolyte Substances 0.000 claims abstract description 17
- 238000005903 acid hydrolysis reaction Methods 0.000 claims abstract description 7
- 238000010306 acid treatment Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 51
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 4
- 150000002739 metals Chemical class 0.000 abstract description 3
- 230000008646 thermal stress Effects 0.000 abstract description 3
- 239000003082 abrasive agent Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 229910017052 cobalt Inorganic materials 0.000 description 10
- 239000010941 cobalt Substances 0.000 description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 10
- 239000002245 particle Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
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Abstract
本发明公开了一种电解联合酸处理脱除聚晶金刚石中金属的方法，属于超硬材料磨料磨具领域。主要过程分为聚晶金刚石表面净化、聚晶金刚石碱性电解液电解处理、聚晶金刚石酸解金属脱除处理三个部分。本发明操作简单，具有脱除金属效率高、安全、环保等一系列优点，大大提高了脱除金属深度，降低了聚晶金刚石在使用过程中的残余热应力，增强了聚晶金刚石的热稳定性和耐磨性。且和传统酸法脱除金属相比，此发明在室温下进行，避免了高温下强酸溶液挥发的情况，具有较高的实用价值和应用前景。The invention discloses a method for removing metals from polycrystalline diamond by electrolysis combined with acid treatment, and belongs to the field of superhard material abrasives. The main process is divided into three parts: polycrystalline diamond surface purification, polycrystalline diamond alkaline electrolyte electrolytic treatment, and polycrystalline diamond acid hydrolysis metal removal treatment. The invention is simple to operate, has a series of advantages such as high metal removal efficiency, safety and environmental protection, greatly improves the metal removal depth, reduces the residual thermal stress of the polycrystalline diamond during use, and enhances the thermal stability of the polycrystalline diamond. resistance and wear resistance. In addition, compared with the traditional acid method for metal removal, the invention is carried out at room temperature, avoiding the volatilization of the strong acid solution at high temperature, and has higher practical value and application prospect.
Description
技术领域technical field
本发明专利涉及超硬材料磨料磨具领域，是一种电解联合酸处理脱除聚晶金刚石中金属的方法。The patent of the invention relates to the field of superhard material abrasives, and is a method for removing metals from polycrystalline diamond by electrolysis combined with acid treatment.
背景技术Background technique
聚晶金刚石（PCD）是由金刚石微粉与金属触媒在高温高压下烧结而成的，其具有金刚石的高硬度和高耐磨性，由于其良好的性能，所以被广泛应用于石油钻头、刀具等多个行业。随着科学技术的进步与发展，国内外对超硬材料提出了新的要求，尤其是热稳定性。PCD作为超硬材料重要的一部分，提高其热稳定性能使得产品能够更好地满足使用要求是当下我们要解决的重要难题。Polycrystalline diamond (PCD) is made of diamond powder and metal catalyst sintered under high temperature and high pressure. It has the high hardness and high wear resistance of diamond. Because of its good performance, it is widely used in oil drill bits, cutting tools, etc. multiple industries. With the progress and development of science and technology, new requirements have been put forward for superhard materials at home and abroad, especially thermal stability. As an important part of superhard materials, improving the thermal stability of PCD so that the product can better meet the requirements of use is an important problem that we need to solve at present.
目前提高PCD热稳定性最有效的方法就是去除金刚石聚晶层中的金属相钴、铝等元素。在PCD的烧结过程中，金属钴作为烧结助剂起催化剂作用，促进金刚石颗粒之间的结合生成D-D键。金属钴的存在之所以会降低聚晶金刚石的稳定性，有两个主要原因，一是所用烧结助剂金属钴与金刚石的热膨胀系数相差较大，由于聚晶金刚石工作条件多为高温条件，因此在工作过程中金刚石晶粒容易脱落从而降低金刚石复合片的性能，二是当温度高于700℃时金刚石会在钴元素的催化作用下转化为石墨使得PCD失效,导致其热稳定性降低。同时金属钴的存在会破坏PCD中形成的Ｄ－Ｄ键，使得PCD在高温条件下出现大规模的磨损、开裂、分层等热损伤，从而降低工具的使用寿命。铝等金属的存在由于热膨胀系数不同也会造成PCD内部热应力，造成内部裂纹、强度硬度下降等问题，从而降低其使用性能。At present, the most effective way to improve the thermal stability of PCD is to remove elements such as cobalt and aluminum in the metal phase of the diamond polycrystalline layer. In the sintering process of PCD, metal cobalt acts as a sintering aid to act as a catalyst, promoting the combination between diamond particles to generate D-D bonds. There are two main reasons why the presence of metal cobalt reduces the stability of polycrystalline diamond. One is that the thermal expansion coefficient of the sintering aid metal cobalt used is quite different from that of diamond. Since the working conditions of polycrystalline diamond are mostly high temperature conditions, so During the working process, the diamond grains are easy to fall off, which reduces the performance of the diamond composite sheet. Second, when the temperature is higher than 700 °C, the diamond will be converted into graphite under the catalysis of cobalt element, which will cause PCD failure and reduce its thermal stability. At the same time, the presence of metallic cobalt will destroy the D-D bond formed in the PCD, causing large-scale thermal damage such as wear, cracking, and delamination of the PCD under high temperature conditions, thereby reducing the service life of the tool. The existence of metals such as aluminum will also cause internal thermal stress in PCD due to different thermal expansion coefficients, resulting in problems such as internal cracks and reduction in strength and hardness, thereby reducing its performance.
为提高PCD产品的使用性能，需除去其中的金属钴、铝等元素。目前已有很多国内外学者对PCD的金属脱除进行了研究，常用的方法为酸法金属脱除。酸金属脱除技术所用酸种类繁多，包括盐酸、硝酸、氢氟酸以及磷酸、硫酸、高氯酸，大多是采用腐蚀性强酸或将几种强酸进行混合作为金属脱除试剂，利用强酸试剂的强氧化性来达到脱除效果。而使用传统酸法存在两个弊端，一方面强酸在高温下挥发对环境产生危害，另一方面脱除深度和效果都不够理想。因此研究一种安全、环保、高效的金属脱除方法尤为关键。In order to improve the performance of PCD products, elements such as metal cobalt and aluminum need to be removed. At present, many domestic and foreign scholars have carried out research on the metal removal of PCD, and the commonly used method is acid metal removal. There are many kinds of acids used in acid metal removal technology, including hydrochloric acid, nitric acid, hydrofluoric acid, phosphoric acid, sulfuric acid, and perchloric acid. Most of them use corrosive strong acids or mix several strong acids as metal removal reagents. Strong oxidizing properties to achieve the removal effect. There are two drawbacks in using the traditional acid method. On the one hand, the volatilization of strong acid at high temperature causes harm to the environment, and on the other hand, the removal depth and effect are not ideal. Therefore, it is particularly critical to develop a safe, environmentally friendly and efficient metal removal method.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于：提供一种电解联合酸处理聚晶金刚石金属脱除的方法，在碱性电解液中对聚晶金刚石表面进行预处理，脱除部分表面金属，使后续酸处理过程中酸溶液能顺利进入到金刚石颗粒缝隙中对金属进行脱除。其原理可靠，操作简单，安全环保，大大提高了脱除深度，降低了聚晶金刚石在使用过程中的残余热应力，增强了聚晶金刚石的热稳定性和耐磨性。且和传统酸法金属脱除相比，此发明在室温下进行，避免了高温下强酸溶液挥发的情况，具有较高的实用价值和应用前景。The object of the present invention is to provide a method for removing metal from polycrystalline diamond by electrolysis combined with acid treatment, pretreating the surface of polycrystalline diamond in an alkaline electrolyte, removing part of the surface metal, and making the acid in the subsequent acid treatment process The solution can smoothly enter into the gaps of the diamond particles to remove the metal. The principle is reliable, the operation is simple, safe and environmentally friendly, the removal depth is greatly improved, the residual thermal stress of the polycrystalline diamond during use is reduced, and the thermal stability and wear resistance of the polycrystalline diamond are enhanced. And compared with the traditional acid method for metal removal, the invention is carried out at room temperature, avoiding the volatilization of the strong acid solution at high temperature, and has higher practical value and application prospect.
技术方案Technical solutions
为实现本发明之目的，采用以下技术方案予以实现：For realizing the purpose of the present invention, adopt following technical scheme to realize:
a、聚晶金刚石表面净化处理，其具体过程为：先用丙酮溶液溶解聚晶金刚石表面有机溶剂，再用乙醇溶液清洗残留的丙酮溶液，最后将洗净的聚晶金刚石烘干备用；a. Purifying the surface of the polycrystalline diamond, the specific process is: first dissolve the organic solvent on the surface of the polycrystalline diamond with an acetone solution, then clean the residual acetone solution with an ethanol solution, and finally dry the cleaned polycrystalline diamond for use;
b、聚晶金刚石碱性电解液电解处理，其具体过程为：将处理后的聚晶金刚石放入定制的电解池中电解处理，电解液是由Na2CO3、KOH、H2O组成的混合溶液，Na2CO3溶液和KOH溶液比例为1：1到1：3之间，（Na2CO3，KOH）和H2O的比例为1：20到1：50之间，以聚晶金刚石为阳极，金属铜片为阴极，确定电压在0.5v到1.5v之间，确定电解时间在24h到48小时之间；b. Electrolytic treatment of polycrystalline diamond with alkaline electrolyte, the specific process is as follows: put the treated polycrystalline diamond into a customized electrolytic cell for electrolytic treatment, and the electrolyte is composed of Na 2 CO 3 , KOH and H 2 O Mixed solutions, the ratio of Na 2 CO 3 solution and KOH solution is between 1:1 and 1:3, and the ratio of (Na 2 CO 3 , KOH) and H 2 O is between 1:20 and 1:50. Crystal diamond is the anode, metal copper sheet is the cathode, the voltage is determined to be between 0.5v and 1.5v, and the electrolysis time is determined to be between 24h and 48 hours;
c、聚晶金刚石酸解金属脱除处理，其具体过程为：将电解处理过的聚晶金刚石放入配置好的酸性金属脱除液中金属脱除处理，酸性金属脱除液是由硫酸（98 wt%）、过氧化氢（30 wt%）组成的混合液，体积比为1:5到1：10之间，将配置好的金属脱除液和聚晶金刚石放入未密封的聚四氟乙烯容器中进行反应,金属脱除时间为 24h到48 h之间。c. Polycrystalline diamond acid hydrolysis metal removal treatment, the specific process is as follows: put the electrolytically treated polycrystalline diamond into the prepared acid metal removal solution for metal removal treatment, and the acid metal removal solution is made of sulfuric acid ( 98 wt%), hydrogen peroxide (30 wt%), the volume ratio is between 1:5 and 1:10, put the prepared metal removal solution and polycrystalline diamond into the unsealed polytetrafluoroethylene The reaction was carried out in a vinyl fluoride container, and the metal removal time was between 24 h and 48 h.
本发明中步骤a中聚晶金刚石表面净化处理优选过程为：将聚晶金刚石样品（含钴量5%到10%之间）放入装有丙酮溶液的烧杯中，在超声清洗机中清洗样品表面10 min到20min，再将丙酮溶液处理过的聚晶金刚石放入装有酒精溶液的烧杯中，在超声清洗机中清洗10 min到20 min中，清洗过后的聚晶金刚石样品在烘箱中烘干备用，设置温度为60℃到80℃之间，时间为5h到10h之间。In the present invention, the preferred process for purifying the surface of the polycrystalline diamond in step a is as follows: put the polycrystalline diamond sample (containing between 5% and 10% of cobalt) into a beaker containing an acetone solution, and clean the sample in an ultrasonic cleaning machine For 10 to 20 minutes on the surface, put the polycrystalline diamond treated with acetone solution into a beaker with alcohol solution, clean it in an ultrasonic cleaner for 10 to 20 minutes, and dry the cleaned polycrystalline diamond in an oven. For dry use, set the temperature between 60°C and 80°C and the time between 5h and 10h.
本发明中步骤c中酸性金属脱除液的配置优选过程为：将硫酸（98 wt%）沿着烧杯壁或者玻璃棒缓慢注入装有过氧化氢（30 wt%）的烧杯中，浓硫酸密度大，如果先加浓硫酸，水会在浓硫酸表面形成一层水层，表面水迅速沸腾，十分危险。In the present invention, the preferred process for configuring the acidic metal removal liquid in step c is as follows: slowly inject sulfuric acid (98 wt%) into the beaker containing hydrogen peroxide (30 wt%) along the beaker wall or glass rod, and the concentration of concentrated sulfuric acid is If the concentrated sulfuric acid is added first, the water will form a layer of water on the surface of the concentrated sulfuric acid, and the surface water will boil rapidly, which is very dangerous.
本发明的有益效果是：The beneficial effects of the present invention are:
1.采用丙酮溶液可以有效清除聚晶金刚石表面的有机溶剂，确保后续电解液和酸性金属脱除液可以更大程度上进入到金刚石颗粒缝隙间；1. The use of acetone solution can effectively remove the organic solvent on the surface of the polycrystalline diamond, ensuring that the subsequent electrolyte and acid metal removal solution can enter the gap between the diamond particles to a greater extent;
2.而通过碱性电解液金属脱除预处理可以将聚晶金刚石表面金属脱除干净，且电解金属脱除速度快，效率高，为下一步酸性金属脱除液进入金刚石颗粒间隙进一步金属脱除提供了更好的条件；2. The metal removal on the surface of polycrystalline diamond can be cleaned by the alkaline electrolyte metal removal pretreatment, and the electrolytic metal removal speed is fast and the efficiency is high, which is the next step for the acidic metal removal solution to enter the diamond particle gap for further metal removal. In addition to providing better conditions;
3.通过电解联合酸反复处理，不但可以对聚晶金刚石表面金属进行脱除，且对聚晶金刚石内部金刚石颗粒间残余的金属也能起到很有效的脱除效果，极大的增强了聚晶金刚石的热稳定性和力学性能。3. Through the repeated treatment of electrolysis and acid, not only the metal on the surface of the polycrystalline diamond can be removed, but also the residual metal between the diamond particles inside the polycrystalline diamond can also be removed effectively, which greatly enhances the polycrystalline diamond. Thermal stability and mechanical properties of crystalline diamond.
具体实施方式Detailed ways
该发明以下结合具体实施例进行进一步描述：The invention is further described below in conjunction with specific embodiments:
实施例1：Example 1:
a、聚晶金刚石表面净化处理，其具体过程为：将聚晶金刚石样品（含钴量5%）放入装有丙酮溶液的烧杯中，在超声清洗机中清洗样品表面10 min，再将丙酮溶液处理过的聚晶金刚石放入装有酒精溶液的烧杯中，在超声清洗机中清洗10 min，清洗过后的聚晶金刚石样品在烘箱中烘干备用，设置温度为60℃，时间为5h；a. Polycrystalline diamond surface purification treatment, the specific process is: put the polycrystalline diamond sample (containing 5% cobalt) into a beaker containing acetone solution, clean the surface of the sample in an ultrasonic cleaner for 10 min, and then acetone The solution-treated polycrystalline diamond was placed in a beaker containing an alcohol solution, cleaned in an ultrasonic cleaner for 10 min, and the cleaned polycrystalline diamond sample was dried in an oven for use at a temperature of 60°C and a time of 5h;
b、聚晶金刚石碱性电解液电解处理，其具体过程为：将处理后的聚晶金刚石放入定制的电解池中电解处理，电解液是由Na2CO3、KOH、H2O组成的混合溶液，Na2CO3溶液和KOH溶液比例为1:1，（Na2CO3，KOH）和H2O的比例为1：20，以聚晶金刚石为阳极，金属铜片为阴极，确定电压在0.5v，确定电解时间在24h；b. Electrolytic treatment of polycrystalline diamond with alkaline electrolyte, the specific process is as follows: put the treated polycrystalline diamond into a customized electrolytic cell for electrolytic treatment, and the electrolyte is composed of Na 2 CO 3 , KOH and H 2 O Mixed solution, the ratio of Na 2 CO 3 solution and KOH solution is 1:1, the ratio of (Na 2 CO 3 , KOH) and H 2 O is 1:20, using polycrystalline diamond as anode and metal copper sheet as cathode, determine The voltage is 0.5v, and the electrolysis time is determined to be 24h;
c、聚晶金刚石酸解金属脱除处理，其具体过程为：将电解处理过的聚晶金刚石放入配置好的酸性金属脱除液中金属脱除处理，酸性金属脱除液是由硫酸（98 wt%）、过氧化氢（30 wt%）组成的混合液，体积比为1:5，将配置好的金属脱除液和聚晶金刚石放入未密封的聚四氟乙烯容器中进行反应,金属脱除时间为 24h；c. Polycrystalline diamond acid hydrolysis metal removal treatment, the specific process is as follows: put the electrolytically treated polycrystalline diamond into the prepared acid metal removal solution for metal removal treatment, and the acid metal removal solution is made of sulfuric acid ( 98 wt%) and hydrogen peroxide (30 wt%), with a volume ratio of 1:5, put the prepared metal removal solution and polycrystalline diamond into an unsealed PTFE container for reaction , the metal removal time is 24h;
实施例2：Example 2:
a、聚晶金刚石表面净化处理，其具体过程为：将聚晶金刚石样品（含铝量7%）放入装有丙酮溶液的烧杯中，在超声清洗机中清洗样品表面15min，再将丙酮溶液处理过的聚晶金刚石放入装有酒精溶液的烧杯中，在超声清洗机中清洗15 min，清洗过后的聚晶金刚石样品在烘箱中烘干备用，设置温度为70℃，时间为7h；a. Polycrystalline diamond surface purification treatment, the specific process is: put the polycrystalline diamond sample (containing 7% aluminum) into a beaker with acetone solution, clean the surface of the sample in an ultrasonic cleaner for 15min, and then put the acetone solution The treated polycrystalline diamond was placed in a beaker containing an alcohol solution, cleaned in an ultrasonic cleaner for 15 min, and the cleaned polycrystalline diamond sample was dried in an oven for later use, the temperature was set to 70 °C, and the time was 7 h;
b、聚晶金刚石碱性电解液电解处理，其具体过程为：将处理后的聚晶金刚石放入定制的电解池中电解处理，电解液是由Na2CO3、KOH、H2O组成的混合溶液，Na2CO3溶液和KOH溶液比例为1:2，（Na2CO3，KOH）和H2O的比例为1：30，以聚晶金刚石为阳极，金属铜片为阴极，确定电压在1.0 v，确定电解时间在36 h；b. Electrolytic treatment of polycrystalline diamond with alkaline electrolyte, the specific process is as follows: put the treated polycrystalline diamond into a customized electrolytic cell for electrolytic treatment, and the electrolyte is composed of Na 2 CO 3 , KOH and H 2 O Mixed solution, the ratio of Na 2 CO 3 solution and KOH solution is 1:2, the ratio of (Na 2 CO 3 , KOH) and H 2 O is 1:30, using polycrystalline diamond as anode and metal copper sheet as cathode, determine The voltage is 1.0 v, and the electrolysis time is determined to be 36 h;
c、聚晶金刚石酸解金属脱除处理，其具体过程为：将电解处理过的聚晶金刚石放入配置好的酸性金属脱除液中金属脱除处理，酸性金属脱除液是由硫酸（98 wt%）、过氧化氢（30 wt%）组成的混合液，体积比为1:7，将配置好的金属脱除液和聚晶金刚石放入未密封的聚四氟乙烯容器中进行反应,金属脱除时间为 36 h；c. Polycrystalline diamond acid hydrolysis metal removal treatment, the specific process is as follows: put the electrolytically treated polycrystalline diamond into the prepared acid metal removal solution for metal removal treatment, and the acid metal removal solution is made of sulfuric acid ( 98 wt%) and hydrogen peroxide (30 wt%), with a volume ratio of 1:7, put the prepared metal removal solution and polycrystalline diamond into an unsealed PTFE container for reaction , the metal removal time is 36 h;
实施例3：Example 3:
a、聚晶金刚石表面净化处理，其具体过程为：将聚晶金刚石样品（含钴量10%）放入装有丙酮溶液的烧杯中，在超声清洗机中清洗样品表面20 min，再将丙酮溶液处理过的聚晶金刚石放入装有酒精溶液的烧杯中，在超声清洗机中清洗20 min，清洗过后的聚晶金刚石样品在烘箱中烘干备用，设置温度为80℃，时间为10 h；a. Polycrystalline diamond surface purification treatment, the specific process is: put the polycrystalline diamond sample (containing 10% cobalt) into a beaker containing acetone solution, clean the surface of the sample in an ultrasonic cleaner for 20 min, and then acetone The solution-treated polycrystalline diamond was placed in a beaker containing an alcohol solution, cleaned in an ultrasonic cleaner for 20 min, and the cleaned polycrystalline diamond sample was dried in an oven for later use. The set temperature was 80 °C and the time was 10 h. ;
b、聚晶金刚石碱性电解液电解处理，其具体过程为：将处理后的聚晶金刚石放入定制的电解池中电解处理，电解液是由Na2CO3、KOH、H2O组成的混合溶液，Na2CO3溶液和KOH溶液比例为1:3，（Na2CO3，KOH）和H2O的比例为1：50，以聚晶金刚石为阳极，金属铜片为阴极，确定电压在1.5 v，确定电解时间在48 h；b. Electrolytic treatment of polycrystalline diamond with alkaline electrolyte, the specific process is as follows: put the treated polycrystalline diamond into a customized electrolytic cell for electrolytic treatment, and the electrolyte is composed of Na 2 CO 3 , KOH and H 2 O Mixed solution, the ratio of Na 2 CO 3 solution and KOH solution is 1:3, the ratio of (Na 2 CO 3 , KOH) and H 2 O is 1:50, using polycrystalline diamond as anode and metal copper sheet as cathode, determine The voltage is 1.5 V, and the electrolysis time is determined to be 48 h;
c、聚晶金刚石酸解金属脱除处理，其具体过程为：将电解处理过的聚晶金刚石放入配置好的酸性金属脱除液中金属脱除处理，酸性金属脱除液是由硫酸（98 wt%）、过氧化氢（30 wt%）组成的混合液，体积比为1:10，将配置好的金属脱除液和聚晶金刚石放入未密封的聚四氟乙烯容器中进行反应,金属脱除时间为 48 h。c. Polycrystalline diamond acid hydrolysis metal removal treatment, the specific process is as follows: put the electrolytically treated polycrystalline diamond into the prepared acid metal removal solution for metal removal treatment, and the acid metal removal solution is made of sulfuric acid ( 98 wt%) and hydrogen peroxide (30 wt%), with a volume ratio of 1:10, put the prepared metal removal solution and polycrystalline diamond into an unsealed PTFE container for reaction , the metal removal time was 48 h.
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| US5650059A (en) * | 1995-08-11 | 1997-07-22 | Credo Tool Company | Method of making cemented carbide substrate |
| JPH09295224A (en) * | 1996-04-26 | 1997-11-18 | Korea Advanced Inst Of Sci Technol | Method for coating super hard tool with diamond film |
| US20100095602A1 (en) * | 2008-10-20 | 2010-04-22 | Smith International, Inc. | Techniques and materials for the accelerated removal of catalyst material from diamond bodies |
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