CN115676830A - A kind of preparation method of zirconium carbide powder - Google Patents
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- 239000000843 powder Substances 0.000 title claims abstract description 39
- 229910026551 ZrC Inorganic materials 0.000 title claims abstract description 35
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 35
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 7
- 229930006000 Sucrose Natural products 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000005720 sucrose Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 22
- 230000015572 biosynthetic process Effects 0.000 abstract description 10
- 238000003786 synthesis reaction Methods 0.000 abstract description 10
- 238000009826 distribution Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 14
- 238000001308 synthesis method Methods 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000000713 high-energy ball milling Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052936 alkali metal sulfate Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
Description
技术领域technical field
本发明涉及碳化锆粉体制备应用技术领域，具体说是一种碳化锆粉体的制备方法。The invention relates to the technical field of preparation and application of zirconium carbide powder, in particular to a preparation method of zirconium carbide powder.
背景技术Background technique
ZrC 是具有高熔点（3550℃）、高硬度（25GPa）、强耐磨及耐腐蚀性以及优良的导电导热性能，被广泛应用于刀具切削、电子元器件、高温结构材料等领域。此外，ZrC 具有低中子吸收截面和良好的抗辐射性能使其在核反应堆核心材料领域也有重要应用。ZrC has a high melting point (3550°C), high hardness (25GPa), strong wear resistance and corrosion resistance, and excellent electrical and thermal conductivity, and is widely used in tool cutting, electronic components, high-temperature structural materials and other fields. In addition, ZrC has a low neutron absorption cross-section and good radiation resistance, so it is also important in the field of nuclear reactor core materials.
公开号为CN102491327B的中国专利公开了一种碳化锆粉体及其制备方法。其技术方案是：先以8～22wt%的二氧化锆或氧氯化锆、65～80wt%的碱金属硫酸盐、1～3wt%的炭黑和10～20wt%的铝粉为原料，混合均匀；再将混合均匀的原料置于管式电炉内，在惰性气体气氛下以2～8℃/min的升温速率升至950～1150℃，保温1～6小时；然后将所得产物放入浓度为0.5～3mol/L的H2SO4溶液中浸泡2～8小时，过滤，用去离子水清洗至清洗液的pH值为7.0，最后在110℃条件下干燥10～24小时，即得碳化锆粉体。本发明具有原料价格低廉、合成过程简单、合成过程易于控制和具有很大产业化前景的特点；所制备的碳化锆粉体活性高，纯度高，粉体颗粒粒径分布均匀，粒径为80～300nm。此专利存在着制备碳化锆粉体的成本高，且制备出的碳化锆粉体颗粒比较大，粉体颗粒分散性比较差的缺陷。The Chinese patent with publication number CN102491327B discloses a zirconium carbide powder and a preparation method thereof. The technical scheme is: firstly, 8-22wt% of zirconium dioxide or zirconium oxychloride, 65-80wt% of alkali metal sulfate, 1-3wt% of carbon black and 10-20wt% of aluminum powder are used as raw materials, and mixed homogeneously; then put the uniformly mixed raw materials in a tube electric furnace, raise the temperature to 950-1150°C at a rate of 2-8°C/min under an inert gas atmosphere, and keep it warm for 1-6 hours; then put the obtained product into a concentration Soak in 0.5-3mol/L H 2 SO 4 solution for 2-8 hours, filter, wash with deionized water until the pH of the cleaning solution is 7.0, and finally dry at 110°C for 10-24 hours to obtain carbonization Zirconium powder. The invention has the characteristics of low raw material price, simple synthesis process, easy control of the synthesis process and great industrialization prospect; the prepared zirconium carbide powder has high activity, high purity, uniform particle size distribution, and a particle size of 80 ~300nm. This patent has the defects that the cost of preparing zirconium carbide powder is high, and the particles of the prepared zirconium carbide powder are relatively large, and the dispersibility of powder particles is relatively poor.
目前国内外对于ZrC制备的传统方法有：直接合成法、自蔓延高温合成法、高能球磨法、溶胶-凝胶法、碳热还原法等等。直接合成法制得的ZrC粉体颗粒粗大，自蔓延高温合成法的合成过程不易控制，容易影响产品性能，高能球磨法过程中容易引入杂质，溶胶-凝胶法生产的粉体颗粒细小，但是生产过程复杂，不适合大批量生产，碳热还原法的生产工艺简单，但生产出来的产品纯度不高。At present, the traditional methods for ZrC preparation at home and abroad include: direct synthesis method, self-propagating high temperature synthesis method, high energy ball milling method, sol-gel method, carbothermal reduction method and so on. The ZrC powder produced by the direct synthesis method has coarse particles, the synthesis process of the self-propagating high-temperature synthesis method is difficult to control, and it is easy to affect the product performance. Impurities are easily introduced during the high-energy ball milling process. The process is complicated and not suitable for mass production. The production process of the carbothermal reduction method is simple, but the purity of the produced product is not high.
发明内容Contents of the invention
针对现有技术中的问题，本发明提供了一种碳化锆粉体的制备方法，本发明的方法实施成本低，且合成工艺简单，过程易于控制，制备出的ZrC粉体颗粒细小达到纳米级，粉体颗粒分散性好，粒径分布均匀。Aiming at the problems in the prior art, the present invention provides a method for preparing zirconium carbide powder. The method of the present invention has low implementation cost, simple synthesis process, easy control of the process, and the prepared ZrC powder particles are as fine as nanometers. , The powder particles have good dispersibility and uniform particle size distribution.
本发明解决其技术问题所采用的技术方案是：一种碳化锆粉体的制备方法，该方法具体包括以下步骤：The technical solution adopted by the present invention to solve its technical problem is: a kind of preparation method of zirconium carbide powder, and this method specifically comprises the following steps:
步骤一：以硝酸锆（Zr(NO3)4·5H2O）作为锆源，以蔗糖作为碳源，锆源的摩尔数以锆源中锆元素的摩尔数计；碳源的摩尔数以碳源中碳元素的摩尔数计，按照锆源与碳源的摩尔比为1:3、1:4、1:5混合制成水溶液；Step 1: Zirconium nitrate (Zr(NO 3 ) 4 5H 2 O) is used as the zirconium source, sucrose is used as the carbon source, and the number of moles of the zirconium source is calculated by the number of moles of zirconium element in the zirconium source; the number of moles of the carbon source is calculated by In terms of moles of carbon elements in the carbon source, the molar ratio of the zirconium source to the carbon source is 1:3, 1:4, 1:5 and mixed to make an aqueous solution;
步骤二：将上述水溶液置入高压反应釜中进行水热反应，反应温度为170～250度，反应时间为15h～25h，之后进行干燥得到水热产物；Step 2: Put the above aqueous solution into a high-pressure reactor for hydrothermal reaction, the reaction temperature is 170-250 degrees, the reaction time is 15h-25h, and then dry to obtain a hydrothermal product;
步骤三：将水热产物进行加热，加热温度为1300～1600度，保温时间为1～2h，随炉冷却，加热过程中惰性气体保护，最后经研磨得到碳化锆粉体。本发明实施成本低，且合成工艺简单，过程易于控制，制备出的ZrC粉体颗粒细小。Step 3: Heating the hydrothermal product, the heating temperature is 1300-1600 degrees, the holding time is 1-2 hours, cooling with the furnace, protected by inert gas during the heating process, and finally grinding to obtain zirconium carbide powder. The implementation cost of the invention is low, the synthesis process is simple, the process is easy to control, and the prepared ZrC powder particles are fine.
本发明的进一步技术改进在于：步骤二中将上述水溶液置入高压反应釜中进行水热反应，反应温度为200度，反应时间为20h，粉体颗粒分散性好，粒径分布均匀尺寸达到纳米级。The further technical improvement of the present invention is: in step 2, the above aqueous solution is placed in a high-pressure reactor for hydrothermal reaction, the reaction temperature is 200 degrees, the reaction time is 20h, the powder particles have good dispersibility, and the particle size distribution is uniform and the size reaches nanometers. class.
本发明的进一步技术改进在于：步骤二中水溶液进行水热反应后，再进行干燥的方式为真空干燥，温度60度，时间为9小时。The further technical improvement of the present invention is: after the aqueous solution undergoes hydrothermal reaction in step 2, the drying method is vacuum drying at a temperature of 60 degrees and a time of 9 hours.
本发明的进一步技术改进在于：步骤三中将水热产物进行加热，加热温度为1500度，保温时间：1.5h。The further technical improvement of the present invention is: in step 3, the hydrothermal product is heated, the heating temperature is 1500 degrees, and the holding time: 1.5h.
本发明的有益效果：Beneficial effects of the present invention:
本发明的方法实施成本低，且合成工艺简单，过程易于控制，制备出的ZrC粉体颗粒细小，粉体颗粒分散性好，粒径分布均匀，本发明具有良好的社会效益，适合推广使用。The method of the invention has low implementation cost, simple synthesis process, and easy control of the process. The prepared ZrC powder particles are fine, the powder particles have good dispersibility, and the particle size distribution is uniform. The invention has good social benefits and is suitable for popularization and use.
具体实施方式Detailed ways
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施方式，进一步阐述本发明。In order to make the technical means, creative features, goals and effects achieved by the present invention easy to understand, the present invention will be further described below in conjunction with specific embodiments.
实施例1Example 1
一种碳化锆粉体的制备方法，该方法具体包括以下步骤：A preparation method of zirconium carbide powder, the method specifically comprises the following steps:
步骤一：以硝酸锆（Zr(NO3)4·5H2O）作为锆源，以蔗糖作为碳源，锆源的摩尔数以锆源中锆元素的摩尔数计；碳源的摩尔数以碳源中碳元素的摩尔数计，按照锆源与碳源的摩尔比为1:3、1:4、1:5混合制成水溶液；Step 1: Zirconium nitrate (Zr(NO 3 ) 4 5H 2 O) is used as the zirconium source, sucrose is used as the carbon source, and the number of moles of the zirconium source is calculated by the number of moles of zirconium element in the zirconium source; the number of moles of the carbon source is calculated by In terms of moles of carbon elements in the carbon source, the molar ratio of the zirconium source to the carbon source is 1:3, 1:4, 1:5 and mixed to make an aqueous solution;
步骤二：将上述水溶液置入高压反应釜中进行水热反应，反应温度为200度，反应时间为20h，之后进行真空干燥，温度60度，时间为9小时，得到水热产物,粉体颗粒分散性好，粒径分布均匀；Step 2: Put the above aqueous solution into a high-pressure reactor for hydrothermal reaction, the reaction temperature is 200 degrees, the reaction time is 20 hours, and then vacuum-dried at a temperature of 60 degrees, and the time is 9 hours, to obtain hydrothermal products, powder particles Good dispersion and uniform particle size distribution;
步骤三：将水热产物进行加热，加热温度为1500度，保温时间为1.5h，随炉冷却，加热过程中惰性气体保护，最后经研磨得到碳化锆粉体，本发明实施成本低，且合成工艺简单，过程易于控制，制备出的ZrC粉体颗粒细小。Step 3: Heating the hydrothermal product, the heating temperature is 1500 degrees, the holding time is 1.5h, cooling with the furnace, protected by an inert gas during the heating process, and finally grinding to obtain zirconium carbide powder. The implementation cost of the present invention is low, and the synthetic The process is simple, the process is easy to control, and the prepared ZrC powder has fine particles.
实施例2Example 2
一种碳化锆粉体的制备方法，该方法具体包括以下步骤：A preparation method of zirconium carbide powder, the method specifically comprises the following steps:
步骤一：以硝酸锆（Zr(NO3)4·5H2O）作为锆源，以蔗糖作为碳源，锆源的摩尔数以锆源中锆元素的摩尔数计；碳源的摩尔数以碳源中碳元素的摩尔数计，按照锆源与碳源的摩尔比为1:3、1:4、1:5混合制成水溶液；Step 1: Zirconium nitrate (Zr(NO 3 ) 4 5H 2 O) is used as the zirconium source, sucrose is used as the carbon source, and the number of moles of the zirconium source is calculated by the number of moles of zirconium element in the zirconium source; the number of moles of the carbon source is calculated by In terms of moles of carbon elements in the carbon source, the molar ratio of the zirconium source to the carbon source is 1:3, 1:4, 1:5 and mixed to make an aqueous solution;
步骤二：将上述水溶液置入高压反应釜中进行水热反应，反应温度为180度，反应时间为19h，之后进行干燥得到水热产物；Step 2: Put the above-mentioned aqueous solution into a high-pressure reactor for hydrothermal reaction, the reaction temperature is 180 degrees, the reaction time is 19 hours, and then dried to obtain a hydrothermal product;
步骤三：将水热产物进行加热，加热温度为1400度，保温时间为1h，随炉冷却，加热过程中惰性气体保护，最后经研磨得到碳化锆粉体，本发明实施成本低，且合成工艺简单，过程易于控制，制备出的ZrC粉体颗粒细小。Step 3: Heating the hydrothermal product, the heating temperature is 1400 degrees, the holding time is 1h, cooling with the furnace, protected by inert gas during the heating process, and finally the zirconium carbide powder is obtained by grinding. The implementation cost of the present invention is low, and the synthesis process is Simple, the process is easy to control, and the prepared ZrC powder has fine particles.
实施例3Example 3
一种碳化锆粉体的制备方法，该方法具体包括以下步骤：A preparation method of zirconium carbide powder, the method specifically comprises the following steps:
步骤一：以硝酸锆（Zr(NO3)4·5H2O）作为锆源，以蔗糖作为碳源，锆源的摩尔数以锆源中锆元素的摩尔数计；碳源的摩尔数以碳源中碳元素的摩尔数计，按照锆源与碳源的摩尔比为1:3、1:4、1:5混合制成水溶液；Step 1: Zirconium nitrate (Zr(NO 3 ) 4 5H 2 O) is used as the zirconium source, sucrose is used as the carbon source, and the number of moles of the zirconium source is calculated by the number of moles of zirconium element in the zirconium source; the number of moles of the carbon source is calculated by In terms of moles of carbon elements in the carbon source, the molar ratio of the zirconium source to the carbon source is 1:3, 1:4, 1:5 and mixed to make an aqueous solution;
步骤二：将上述水溶液置入高压反应釜中进行水热反应，反应温度为190度，反应时间为21h，之后进行干燥得到水热产物；Step 2: Put the above aqueous solution into a high-pressure reactor for hydrothermal reaction, the reaction temperature is 190 degrees, the reaction time is 21 hours, and then dried to obtain a hydrothermal product;
步骤三：将水热产物进行加热，加热温度为1600度，保温时间为2h，随炉冷却，加热过程中惰性气体保护，最后经研磨得到碳化锆粉体，本发明实施成本低，且合成工艺简单，过程易于控制，制备出的ZrC粉体颗粒细小Step 3: Heating the hydrothermal product, the heating temperature is 1600 degrees, the holding time is 2 hours, cooling with the furnace, inert gas protection during the heating process, and finally grinding to obtain zirconium carbide powder. The implementation cost of the present invention is low, and the synthesis process Simple, easy to control the process, the prepared ZrC powder particles are fine
本发明的方法实施成本低，且合成工艺简单，过程易于控制，制备出的ZrC粉体颗粒细小达到纳米级，粉体颗粒分散性好，粒径分布均匀，本发明具有良好的社会效益，适合推广使用。The implementation cost of the method of the present invention is low, and the synthesis process is simple, the process is easy to control, the prepared ZrC powder particles are as fine as nanometers, the powder particles have good dispersibility, and the particle size distribution is uniform. The present invention has good social benefits and is suitable for Promotional use.
对比例comparative example
以硝酸锆（Zr(NO3)4·5H2O）作为锆源，以蔗糖作为碳源，锆源的摩尔数以锆源中锆元素的摩尔数计；碳源的摩尔数以碳源中碳元素的摩尔数计。按照锆源与碳源的摩尔比为1:3进行混合制成水溶液，将水溶液置入高压反应釜中进行水热反应，反应温度200度，反应时间20h，之后进行干燥（干燥方式为真空干燥，温度60度，时间12小时）得到水热产物。将水热产物进行加热，加热温度：1200度，保温时间：2h，随炉冷却，最后经研磨得到最终产物，但是经XRD检测分析，最终产物为氧化锆。Zirconium nitrate (Zr(NO 3 ) 4 5H 2 O) was used as the zirconium source, sucrose was used as the carbon source, and the moles of the zirconium source were calculated as the moles of zirconium element in the zirconium source; the moles of the carbon source were calculated as the carbon source The number of moles of carbon element. Mix according to the molar ratio of zirconium source and carbon source to 1:3 to make an aqueous solution, put the aqueous solution into a high-pressure reactor for hydrothermal reaction, the reaction temperature is 200 degrees, the reaction time is 20h, and then dried (the drying method is vacuum drying , temperature 60 degrees, time 12 hours) to obtain hydrothermal products. Heating the hydrothermal product, heating temperature: 1200 degrees, holding time: 2h, cooling with the furnace, and finally grinding to obtain the final product, but the final product is zirconia through XRD detection and analysis.
以上显示和描述了本发明的基本原理、主要特征和优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施方式和说明书中的描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入本发明要求保护的范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。The basic principles, main features and advantages of the present invention have been shown and described above. Those skilled in the industry should understand that the present invention is not limited by the above-mentioned embodiments, and the descriptions in the above-mentioned embodiments and specification only illustrate the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also There are various changes and improvements, and these changes and improvements all fall within the scope of protection of the present invention. The protection scope of the present invention is defined by the appended claims and their equivalents.
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| CN103626179A (en) * | 2013-11-19 | 2014-03-12 | 陕西科技大学 | Method for preparing nanometer zirconium carbide powder |
| CN107721429A (en) * | 2017-11-15 | 2018-02-23 | 中国科学院福建物质结构研究所 | Zirconium carbide silicon carbide composite powder body material and preparation method thereof |
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| CN102515164A (en) * | 2011-11-30 | 2012-06-27 | 北京科技大学 | Preparation method of zirconium carbide ceramic powder |
| CN103626179A (en) * | 2013-11-19 | 2014-03-12 | 陕西科技大学 | Method for preparing nanometer zirconium carbide powder |
| CN107721429A (en) * | 2017-11-15 | 2018-02-23 | 中国科学院福建物质结构研究所 | Zirconium carbide silicon carbide composite powder body material and preparation method thereof |
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