CN118387844A - Simple preparation method of nitride powder - Google Patents
Simple preparation method of nitride powder Download PDFInfo
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- CN118387844A CN118387844A CN202410399202.1A CN202410399202A CN118387844A CN 118387844 A CN118387844 A CN 118387844A CN 202410399202 A CN202410399202 A CN 202410399202A CN 118387844 A CN118387844 A CN 118387844A
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- 239000000843 powder Substances 0.000 title claims abstract description 21
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000654 additive Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000011282 treatment Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract 2
- 239000007787 solid Substances 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- -1 alcohol compound Chemical class 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000005121 nitriding Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 13
- 239000011701 zinc Substances 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 8
- AKJVMGQSGCSQBU-UHFFFAOYSA-N zinc azanidylidenezinc Chemical group [Zn++].[N-]=[Zn].[N-]=[Zn] AKJVMGQSGCSQBU-UHFFFAOYSA-N 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 4
- 150000001298 alcohols Chemical class 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000006117 anti-reflective coating Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0722—Preparation by direct nitridation of aluminium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0728—After-treatment, e.g. grinding, purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
技术领域Technical Field
本发明涉及一种氮化物制备方法，尤其涉及一种氮化物粉体的简易制备方法。The invention relates to a method for preparing nitride, and in particular to a simple method for preparing nitride powder.
背景技术Background technique
氮化物包括离子型氮化物、共价型氮化物和金属型氮化物，氮化锌作为金属型氮化物的重要成员之一，因其具有良好的光电性能、电子迁移率和电子饱和度高，在光电二极管、阳极材料、防反射涂层等领域具有广泛的应用前景。Nitrides include ionic nitrides, covalent nitrides and metallic nitrides. Zinc nitride, as one of the important members of metallic nitrides, has broad application prospects in photodiodes, anode materials, anti-reflective coatings and other fields due to its good photoelectric properties, electron mobility and high electron saturation.
目前，制备氮化物粉体的方法有溶剂热法、自蔓延高温合成法等。溶剂热法需要用毒性高的溶剂，且反应时间较长；自蔓延高温合成法对设备的要求高，且很难控制反应过程。因此，寻找一种低成本、操作简单、步骤少、不使用有毒有害反应原料、同时保证产品纯度的氮化物粉体的制备方法具有重要意义。At present, the methods for preparing nitride powders include solvothermal method, self-propagating high temperature synthesis method, etc. The solvothermal method requires highly toxic solvents and has a long reaction time; the self-propagating high temperature synthesis method has high requirements for equipment and it is difficult to control the reaction process. Therefore, it is of great significance to find a method for preparing nitride powders that is low-cost, simple to operate, has few steps, does not use toxic and harmful reaction raw materials, and ensures product purity.
中国CN202110008385.6号专利介绍一种氮化锌粉体材料的制备方法，包括以锌板为起始原料，通过将锌板淹没在盐酸中超声波清洗的方式除去锌板表面的氧化锌杂质，再用去离子水进行多次冲洗，然后在真空中采用蒸馏的方法提纯锌，以此获得高纯锌；由于上述获得的高纯锌不是颗粒状的，还需要在专门的制粒设备中在氩气、高温条件下将高纯锌熔化制成锌锭；获得的高纯锌粒还需要在一定温度下进行进一步的干燥处理，且在干燥处理前需要多次较长时间反复的超声波清洗；通过以上步骤才能实现氮化锌粉体的制备。上述发明中，因盐酸具有腐蚀性，如果以锌粉为原料，由于原料表面积的增加会加大对锌的腐蚀，降低最终产品的收率，所以以锌板为原料。China's patent CN202110008385.6 introduces a method for preparing zinc nitride powder material, including using zinc plate as the starting material, removing zinc oxide impurities on the surface of the zinc plate by submerging the zinc plate in hydrochloric acid and ultrasonic cleaning, then rinsing it with deionized water for multiple times, and then purifying zinc by distillation in a vacuum to obtain high-purity zinc; since the high-purity zinc obtained above is not granular, it is also necessary to melt the high-purity zinc in a special granulation equipment under argon and high temperature conditions to make zinc ingots; the obtained high-purity zinc particles also need to be further dried at a certain temperature, and ultrasonic cleaning is required for multiple long-term repeated cleaning before drying; the above steps can realize the preparation of zinc nitride powder. In the above invention, because hydrochloric acid is corrosive, if zinc powder is used as the raw material, the increase in the surface area of the raw material will increase the corrosion of zinc and reduce the yield of the final product, so zinc plate is used as the raw material.
发明内容Summary of the invention
本发明的目的在于提供一种氮化物粉体的简易制备方法，该方法直接使用常规商业锌粉作为原料，且无需盐酸处理、真空蒸馏、氩气下加热获取锌粒、超声波清洗等任何处理，工艺流程步骤和设备少且要求低、操作容易、只需使用醇类化合物作为添加剂与金属锌粉混合，而且醇添加剂起到了对反应前驱物的分散作用，有效避免材料制备过程中干扰因素的影响，保证制备结果的可控性。The purpose of the present invention is to provide a simple preparation method of nitride powder. The method directly uses conventional commercial zinc powder as a raw material, and does not require any treatment such as hydrochloric acid treatment, vacuum distillation, heating under argon to obtain zinc particles, ultrasonic cleaning, etc. The process steps and equipment are few and the requirements are low, the operation is easy, and only alcohol compounds need to be used as additives to mix with metal zinc powder. The alcohol additive plays a dispersing role on the reaction precursor, effectively avoiding the influence of interfering factors in the material preparation process, and ensuring the controllability of the preparation results.
本发明的目的是通过以下技术方案实现的：The objective of the present invention is achieved through the following technical solutions:
一种氮化物粉体的简易制备方法，包括以下步骤：A simple method for preparing nitride powder comprises the following steps:
（1）取一定量的醇类化合物作为添加剂；(1) Taking a certain amount of alcohol compound as an additive;
（2）将醇类化合物与金属锌粉以一定比例通过研磨使二者混合均匀；(2) Grinding the alcohol compound and the metallic zinc powder in a certain proportion to uniformly mix the two;
（3）将步骤（2）得到的所述混合物通过气固法氮化；(3) nitriding the mixture obtained in step (2) by a gas-solidification method;
（4）将步骤（3）得到的所述产物研磨、干燥即可。(4) Grind and dry the product obtained in step (3).
优选的，步骤（1）中，所述醇类化合物添加剂包括甲醇、丙三醇中的一种。Preferably, in step (1), the alcohol compound additive includes one of methanol and propylene glycol.
可选的，步骤（2）中，所述锌粉为常规商业锌粉即可，可直接使用，无需其它处理。Optionally, in step (2), the zinc powder can be conventional commercial zinc powder and can be used directly without further treatment.
优选的，步骤（2）中，所述醇类化合物添加剂与锌粉的摩尔比例为1:0.12~1:0.43。Preferably, in step (2), the molar ratio of the alcohol compound additive to the zinc powder is 1:0.12 to 1:0.43.
本发明的优点与效果是：The advantages and effects of the present invention are:
1.本发明通过利用醇类化合物添加剂与金属粉末混合，通过醇添加剂辅助金属粉末的反应，不仅提高了产品的分散性，避免了产物颗粒在后续反应过程中发生团聚，而且还可大大提高产品的纯度，纯度可高达98%，相对于不使用醇类化合物添加剂的工艺，本工艺的产物纯度可提高了高达52%以上；1. The present invention uses alcohol compound additives to mix with metal powders, and uses the alcohol additives to assist the reaction of the metal powders, which not only improves the dispersibility of the product and avoids the agglomeration of product particles in the subsequent reaction process, but also greatly improves the purity of the product, which can be as high as 98%. Compared with the process without using alcohol compound additives, the product purity of this process can be increased by more than 52%;
2.本发明具有工艺简单、原料易得、操作容易、成本低廉，污染小优点。在保证产品纯度的基础上简化了制备工艺，减少了设备数量和对设备的要求，同时提高了产品的分散性，在氮化物粉体制备领域具有广阔的应用前景。2. The present invention has the advantages of simple process, readily available raw materials, easy operation, low cost and little pollution. On the basis of ensuring the purity of the product, the preparation process is simplified, the number of equipment and the requirements for equipment are reduced, and the dispersibility of the product is improved, which has broad application prospects in the field of nitride powder preparation.
具体实施方式Detailed ways
下面结合实施例，对本发明的一些实施方式作详细说明。Some implementation modes of the present invention are described in detail below in conjunction with examples.
实施例一Embodiment 1
选取甲醇作为醇类添加剂；Methanol is selected as the alcohol additive;
将甲醇添加剂与金属锌粉以摩尔比1:0.32通过研磨使二者混合均匀；Methanol additive and metallic zinc powder were mixed uniformly by grinding at a molar ratio of 1:0.32;
将步骤2）得到的所述混合物在流动气氛为NH3、流速为300sccm中加热3小时；The mixture obtained in step 2) is heated in a flowing atmosphere of NH3 at a flow rate of 300 sccm for 3 hours;
将步骤3）得到的所述产物研磨、干燥。The product obtained in step 3) is ground and dried.
实施例二Embodiment 2
选取丙三醇作为醇类添加剂；Selecting glycerol as the alcohol additive;
将丙三醇添加剂与金属锌粉以摩尔比1:0.18通过研磨使二者混合均匀；Grind the glycerol additive and the metallic zinc powder in a molar ratio of 1:0.18 to mix the two uniformly;
将步骤2）得到的所述混合物在流动气氛为NH3、流速为300sccm中加热3小时；The mixture obtained in step 2) is heated in a flowing atmosphere of NH3 at a flow rate of 300 sccm for 3 hours;
将步骤3）得到的所述产物研磨、干燥。The product obtained in step 3) is ground and dried.
对比例一Comparative Example 1
在不借助任何醇类添加剂的情况下，对金属锌粉进行研磨；Grinding metallic zinc powder without any alcohol additives;
将步骤1）得到的所述混合物在流动气氛为NH3、流速为300sccm中加热3小时；The mixture obtained in step 1) is heated in a flowing atmosphere of NH3 at a flow rate of 300 sccm for 3 hours;
将步骤2）得到的所述产物研磨、干燥；Grinding and drying the product obtained in step 2);
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims (4)
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| CN202410399202.1A CN118387844A (en) | 2024-04-03 | 2024-04-03 | Simple preparation method of nitride powder |
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