CN105731459A - Preparation method of nano chromium carbide powder - Google Patents
Preparation method of nano chromium carbide powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims description 44
- 229910003470 tongbaite Inorganic materials 0.000 title claims description 27
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 title claims description 17
- 238000002360 preparation method Methods 0.000 title claims description 8
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 24
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 24
- 239000002243 precursor Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- 239000004471 Glycine Substances 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 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 description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 description 16
- 239000011651 chromium Substances 0.000 description 13
- 239000002994 raw material Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 238000003763 carbonization Methods 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 229910000423 chromium oxide Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 229910000922 High-strength low-alloy steel Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- JOSWYUNQBRPBDN-UHFFFAOYSA-P ammonium dichromate Chemical compound [NH4+].[NH4+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O JOSWYUNQBRPBDN-UHFFFAOYSA-P 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003966 growth inhibitor Substances 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Carbon And Carbon Compounds (AREA)
Abstract
本发明涉及一种纳米碳化铬粉末的制备方法,属于纳米粉末制备技术领域。工艺过程为:(1)将硝酸铬、甘氨酸和碳源按照一定比例配成溶液;(2)加热并搅拌,溶液挥发、浓缩后分解,得到前驱体粉末;(3)将前驱体粉末于600~1000℃温度范围内,在一定保护气氛下反应0.5?3小时。本发明工艺简单,成本低,易于产业化生产,得到的碳化铬粉末颗粒粒度小于100nm,分散性好。
The invention relates to a preparation method of nano chromium carbide powder, which belongs to the technical field of nano powder preparation. The process is as follows: (1) make a solution of chromium nitrate, glycine and carbon source according to a certain ratio; (2) heat and stir, the solution is volatilized, concentrated and then decomposed to obtain the precursor powder; (3) the precursor powder is heated at 600 Within the temperature range of ~1000°C, react in a certain protective atmosphere for 0.5 to 3 hours. The invention has the advantages of simple process, low cost and easy industrial production, and the particle size of the obtained chromium carbide powder is less than 100nm, and the dispersibility is good.
Description
技术领域technical field
本发明属于纳米粉末制备技术领域,具体涉及一种纳米碳化铬粉末的生产方法。The invention belongs to the technical field of nano powder preparation, and in particular relates to a production method of nano chromium carbide powder.
背景技术Background technique
碳化铬(Cr3C2)因具有高熔点、高硬度、高耐磨性、抑制晶粒长大以及提高材料抗氧化性和抗腐蚀性等优越性能而广泛应用于粉末冶金、电子,催化剂、高温涂层材料等诸多工业生产领域。在硬质合金生产中,碳化铬用于WC硬质合金晶粒长大抑制剂。随着超细硬质合金的应用,对纳米碳化铬的要求越来越紧迫。碳化铬除用于硬质合金生产中的添加剂细化硬质外,也用于制备热喷涂粉末用于高温部件的耐磨防护。在冶炼高强度低合金钢、高强度耐磨钢等一些特种钢时,添加Cr3C2能有效促进它们的晶粒细化、晶粒强化,并且阻碍其位错的延伸和迁移,阻碍晶界的迁移从而提高钢的强度、硬度、铺度、耐磨性、耐蚀性、延伸性等性能,大大提高钢的综合性能。此外,纳米Cr3C2也大量应用于抗磨耗薄膜和半导体薄膜等材料制备。Chromium carbide (Cr 3 C 2 ) is widely used in powder metallurgy, electronics, catalysts, High temperature coating materials and many other industrial production fields. In cemented carbide production, chromium carbide is used as WC cemented carbide grain growth inhibitor. With the application of ultra-fine cemented carbide, the requirements for nano-chromium carbide are becoming more and more urgent. Chromium carbide is not only used as an additive in the production of cemented carbide to refine the hardness, but also used to prepare thermal spray powder for wear protection of high temperature components. When smelting some special steels such as high-strength low-alloy steel and high-strength wear-resistant steel, the addition of Cr 3 C 2 can effectively promote their grain refinement and grain strengthening, and hinder the extension and migration of dislocations, hinder the The migration of the boundary improves the strength, hardness, pavement, wear resistance, corrosion resistance, elongation and other properties of the steel, and greatly improves the comprehensive performance of the steel. In addition, nano-Cr 3 C 2 is also widely used in the preparation of materials such as wear-resistant films and semiconductor films.
目前Cr3C2粉末的制备方法主要有:“氧化物+碳”球磨还原法、喷雾干燥还原、气体还原法、高能球磨法等。在公开号CN1176224A中,汪兆全等以氧化铬和炭黑为主要原料,按照一定比例,一定技术路线,生产处含碳量12%以上,碳化率高于99.9%的Cr3C2粉末。该方法中原始粉末粒度粗,不利于碳化反应进行,且碳化温度高,能源耗费大,产物粒度难以达到要求,不能满足工业应用。在公开号CN1724349A中,吴恩熙等以氧化铬为铬源,溶于浓度为10%-20%的有机溶剂中,后采用离心喷雾干燥,得到含有铬以及游离有机物前驱物粉末。前驱体在保护气氛中,先550℃焙烧,在通混合气体900-1000℃碳化,得到Cr3C2粉末。该方法工艺过程复杂,采用混合气体碳化,成本较高。在公开号CN100357187C中,郝俊杰等以重铬酸铵、水合肼、酚醛树脂、纳米炭黑为原料,首先合成非晶纳米Cr2O3,后配置酚醛树脂乙醇溶液,将两者混合,球磨(2-8h)干燥,干燥后真空碳化,碳化后粉末球磨筛分,获得所需要求粉末。该方法新颖,但原料与工艺复杂,不利于大规模生产。在公开号CN101955184A中,赵志伟等以纳米Cr2O3为铬源,碳质为还原剂,酒精或丙酮做球磨介质。将原料放入球磨罐,经球磨(2-6h)干燥(0.5~2h)后得到混合料,混合料在保护气氛下,于800~1100℃,进行碳热还原得到纳米碳化铬粉末。该方法工艺过程复杂,时间周期长,不利于工业化推广。At present, the preparation methods of Cr 3 C 2 powder mainly include: "oxide + carbon" ball milling reduction method, spray drying reduction method, gas reduction method, high-energy ball milling method, etc. In the publication number CN1176224A, Wang Zhaoquan and others used chromium oxide and carbon black as the main raw materials, according to a certain proportion and a certain technical route, produced Cr 3 C 2 powder with a carbon content of more than 12% and a carbonization rate higher than 99.9%. In this method, the particle size of the original powder is coarse, which is not conducive to the carbonization reaction, and the carbonization temperature is high, the energy consumption is large, and the particle size of the product is difficult to meet the requirements, which cannot meet the industrial application. In the publication number CN1724349A, Wu Enxi et al. used chromium oxide as a chromium source, dissolved it in an organic solvent with a concentration of 10%-20%, and then used centrifugal spray drying to obtain a precursor powder containing chromium and free organic matter. The precursor is first calcined at 550°C in a protective atmosphere, and then carbonized at 900-1000°C by passing a mixed gas to obtain Cr 3 C 2 powder. The process of this method is complex, carbonization with mixed gas is used, and the cost is relatively high. In the publication number CN100357187C, Hao Junjie and others used ammonium dichromate, hydrazine hydrate, phenolic resin, and nano-carbon black as raw materials to first synthesize amorphous nano-Cr 2 O 3 , and then configure phenolic resin ethanol solution, mix the two, and ball mill (2-8h) drying, vacuum carbonization after drying, powder ball milling and sieving after carbonization to obtain the required powder. The method is novel, but the raw materials and process are complex, which is not conducive to large-scale production. In the publication number CN101955184A, Zhao Zhiwei et al. used nano-Cr 2 O 3 as the chromium source, carbonaceous as the reducing agent, and alcohol or acetone as the ball milling medium. The raw materials are put into a ball mill tank, and the mixture is obtained after ball milling (2-6h) and drying (0.5-2h). The mixture is subjected to carbothermal reduction at 800-1100°C under a protective atmosphere to obtain nano-chromium carbide powder. The process of the method is complicated and the time period is long, which is unfavorable for industrial promotion.
发明内容Contents of the invention
本发明提供一种简单、高效、低成本制备高质量纳米碳化铬的方法。The invention provides a simple, efficient and low-cost method for preparing high-quality nano-chromium carbide.
一种纳米碳化铬粉末的生产方法,其特征在于包括如下步骤:A kind of production method of nanometer chromium carbide powder, it is characterized in that comprising the steps:
a、将硝酸铬、甘氨酸和碳源按照一定比例溶于去离子水中,其中硝酸铬、甘氨酸和碳源的比例按摩尔比计,硝酸铬与甘氨酸比例为1:(1~6),硝酸铬与碳源的比例为1:(0.5~2);a. Dissolve chromium nitrate, glycine and carbon source in deionized water according to a certain ratio, wherein the ratio of chromium nitrate, glycine and carbon source is based on molar ratio, the ratio of chromium nitrate and glycine is 1: (1 ~ 6), chromium nitrate The ratio to carbon source is 1:(0.5~2);
b、将a步骤形成的溶液加热并搅拌,使溶液挥发、浓缩、分解,得到前驱体粉末;b. Heating and stirring the solution formed in step a, volatilizing, concentrating and decomposing the solution to obtain the precursor powder;
c、将b步骤得到的前驱体粉末于600~1000℃温度范围内,在一定保护气氛下反应0.5~3小时,得到纳米碳化铬粉末。c. Reacting the precursor powder obtained in step b in a temperature range of 600-1000° C. under a certain protective atmosphere for 0.5-3 hours to obtain nano-chromium carbide powder.
其中a步骤中加入的碳源为葡萄糖、蔗糖、柠檬酸、麦芽糖和可溶性淀粉。Wherein the carbon source added in step a is glucose, sucrose, citric acid, maltose and soluble starch.
c步骤中的一定气氛为氮气、氩气保护性气氛;The certain atmosphere in the c step is nitrogen, argon protective atmosphere;
其最佳反应温度为700~900℃;最佳反应时间为1~2小时;The optimum reaction temperature is 700-900°C; the optimum reaction time is 1-2 hours;
本发明生产的纳米碳化铬粉末颗粒粒度小于100nm,分散性好。The particle size of the nano chromium carbide powder produced by the invention is less than 100nm, and the dispersibility is good.
该方法具有以下优点:(1)利用液相中各原料之间的氧化还原反应制备前驱体粉末,简便、快捷,可在十几分钟内完成;(2)利用液相混合各原料,可实现碳源与铬源在分子级别上的均匀混合,使粒度细小的碳源、铬源直接接触反应,减少反应物颗粒之间的扩散距离,促进反应进行;(3)前驱物反应活性高,可降低合成反应温度,提高反应速度;(4)所制备碳化铬粉末粒度小,分散性好。The method has the following advantages: (1) The precursor powder is prepared by redox reaction between raw materials in the liquid phase, which is simple and fast, and can be completed within ten minutes; (2) The raw materials are mixed in the liquid phase to achieve The uniform mixing of carbon source and chromium source at the molecular level enables direct contact reaction of fine-grained carbon source and chromium source, reduces the diffusion distance between reactant particles, and promotes the reaction; (3) the precursor has high reactivity and can Reduce the synthesis reaction temperature and increase the reaction speed; (4) The prepared chromium carbide powder has small particle size and good dispersibility.
附图说明Description of drawings
图1为本发明纳米碳化铬的X射线衍射图。Fig. 1 is the X-ray diffraction pattern of nano chromium carbide of the present invention.
图2为本发明纳米碳化铬的透射电镜照片。Fig. 2 is a transmission electron micrograph of nano chromium carbide of the present invention.
具体实施方式detailed description
下面结合实施例对本发明作进一步的阐述,应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后本领域技术人员可以对本发明做各种改动或修改,这些等价同样落于本申请所附权利要求书所限定的范围。The present invention will be further described below in conjunction with the examples. It should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that those skilled in the art may make various changes or modifications to the present invention after reading the teachings of the present invention, and these equivalents also fall within the scope defined by the appended claims of the present application.
实施例1:Example 1:
称取硝酸铬0.025摩尔、甘氨酸0.1摩尔、碳源0.025摩尔,将各种原料溶于去离子水中,配制成混合溶液,将溶液置于可控温电炉上进行加热。溶液在经历挥发、浓缩、分解等一系列反应后,得到前驱体粉末,将前驱体粉末在600℃、氩气气氛的条件下反应3小时,得到纳米碳化铬粉末。Weigh 0.025 moles of chromium nitrate, 0.1 moles of glycine, and 0.025 moles of carbon source, dissolve various raw materials in deionized water to prepare a mixed solution, and place the solution on a temperature-controllable electric furnace for heating. After the solution undergoes a series of reactions such as volatilization, concentration, and decomposition, the precursor powder is obtained, and the precursor powder is reacted for 3 hours at 600°C in an argon atmosphere to obtain nano-chromium carbide powder.
实施例2:Example 2:
称取硝酸铬0.025摩尔、甘氨酸0.025摩尔、碳源0.0125摩尔,将各种原料溶于去离子水中,配制成混合溶液,将溶液置于可控温电炉上进行加热。溶液在经历挥发、浓缩、分解等一系列反应后,得到前驱体粉末,将前驱体粉末在900℃,氩气气氛的条件下反应2小时,得到纳米碳化铬粉末。Weigh 0.025 mol of chromium nitrate, 0.025 mol of glycine, and 0.0125 mol of carbon source, dissolve various raw materials in deionized water, prepare a mixed solution, and place the solution on a temperature-controllable electric furnace for heating. After the solution undergoes a series of reactions such as volatilization, concentration, and decomposition, the precursor powder is obtained, and the precursor powder is reacted at 900 ° C for 2 hours under the conditions of argon atmosphere to obtain nano-chromium carbide powder.
实施例3:Example 3:
称取硝酸铬0.025摩尔、甘氨酸0.1摩尔、碳源0.0375摩尔溶于蒸馏水中,配制成溶液,将溶液置于可控温电炉上进行加热。溶液在经历挥发、浓缩、分解等一系列过程后发生反应,得到前驱体粉末,将前驱体粉末在800℃、氮气气氛的条件下于炉中反应1.5小时,得到纳米碳化铬粉末。Weigh 0.025 mol of chromium nitrate, 0.1 mol of glycine, and 0.0375 mol of carbon source and dissolve them in distilled water to prepare a solution, and heat the solution on a temperature-controllable electric furnace. The solution reacts after undergoing a series of processes such as volatilization, concentration, and decomposition to obtain a precursor powder. The precursor powder is reacted in a furnace at 800°C and nitrogen atmosphere for 1.5 hours to obtain nano-chromium carbide powder.
实施例4:Example 4:
称取硝酸铬0.025摩尔、甘氨酸0.15摩尔、碳源0.05摩尔溶于去离子水中,配制成混合溶液,将溶液置于可控温电炉上进行加热。溶液在经历挥发、浓缩、分解等一系列过程后发生反应,得到前驱体粉末,将前驱体粉末在900℃、氩气气氛的条件下于炉中反应1小时,得到纳米碳化铬粉末。Weigh 0.025 moles of chromium nitrate, 0.15 moles of glycine, and 0.05 moles of carbon source and dissolve them in deionized water to prepare a mixed solution, and heat the solution on a temperature-controllable electric furnace. The solution reacts after undergoing a series of processes such as volatilization, concentration, and decomposition to obtain a precursor powder. The precursor powder is reacted in a furnace at 900°C and an argon atmosphere for 1 hour to obtain nano-chromium carbide powder.
实施例5:Example 5:
称取硝酸铬0.025摩尔、甘氨酸0.1摩尔、碳源0.05摩尔溶于去离子水中,配制成混合溶液,将溶液置于可控温电炉上进行加热。溶液在经历挥发、浓缩、分解等一系列过程后发生反应,得到前驱体粉末,将前驱体粉末在1000℃、氩气氛条件下于炉中反应0.5小时,得到纳米碳化铬粉末。Weigh 0.025 mol of chromium nitrate, 0.1 mol of glycine, and 0.05 mol of carbon source and dissolve them in deionized water to prepare a mixed solution, and place the solution on a temperature-controllable electric furnace for heating. The solution reacts after undergoing a series of processes such as volatilization, concentration, and decomposition to obtain a precursor powder. The precursor powder is reacted in a furnace at 1000°C and an argon atmosphere for 0.5 hours to obtain nano-chromium carbide powder.
实施例6:Embodiment 6:
称取硝酸铬0.025摩尔、甘氨酸0.125摩尔、碳源0.0375摩尔溶于去离子水中,配制成混合溶液,将溶液置于可控温电炉上进行加热。溶液在经历挥发、浓缩、分解等一系列过程后发生反应,得到前驱体粉末,将前驱体粉末在1000℃、氮气气氛条件下于炉中反应0.5小时,得到纳米碳化铬粉末。Weigh 0.025 moles of chromium nitrate, 0.125 moles of glycine, and 0.0375 moles of carbon source and dissolve them in deionized water to prepare a mixed solution, and heat the solution on a temperature-controllable electric furnace. The solution reacts after undergoing a series of processes such as volatilization, concentration, and decomposition to obtain a precursor powder. The precursor powder is reacted in a furnace at 1000°C under a nitrogen atmosphere for 0.5 hours to obtain nano-chromium carbide powder.
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