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CN109399582A - It is prepared by the high temperature and pressure of block materials molybdenum nitride - Google Patents

It is prepared by the high temperature and pressure of block materials molybdenum nitride Download PDF

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CN109399582A
CN109399582A CN201910000664.0A CN201910000664A CN109399582A CN 109399582 A CN109399582 A CN 109399582A CN 201910000664 A CN201910000664 A CN 201910000664A CN 109399582 A CN109399582 A CN 109399582A
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molybdenum
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molybdenum nitride
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CN109399582B (en
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王常春
宋乐乐
曲铭镭
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JILIN UNIVERSITY OF CHEMICAL TECHNOLOGY
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Jilin Institute of Chemical Technology
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    • 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
    • C01B21/0615—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 transition metals other than titanium, zirconium or hafnium
    • C01B21/062—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 transition metals other than titanium, zirconium or hafnium with chromium, molybdenum or tungsten
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    • 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
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract

本发明块体材料氮化钼的高温高压制备方法，属于过渡金属氮化物制备的技术领域。制备过程为以钼粉和三聚氰胺为原料，将钼粉和三聚氰胺分别利用液压机压片，做成三明治结构，按合成腔体大小做成圆柱状；将圆柱状原料装入加热容器，放入合成腔体中，在压力为4.0~5.0 GPa、温度为1500~1900℃下保温保压10分钟；最后冷却卸压，制得氮化钼块状材料。本发明工艺流程简单，缩短了制备周期和烧结时间；不产生空气污染和资源浪费；通过优化合成温度、压力和保温时间，可以合成出两种单一相的氮化钼。The high temperature and high pressure preparation method of bulk material molybdenum nitride of the invention belongs to the technical field of transition metal nitride preparation. The preparation process is as follows: molybdenum powder and melamine are used as raw materials, and the molybdenum powder and melamine are respectively pressed by a hydraulic press to form a sandwich structure, which is made into a cylindrical shape according to the size of the synthesis cavity; the cylindrical raw materials are put into a heating container and put into the synthesis cavity. In the body, the pressure is 4.0~5.0 GPa and the temperature is 1500~1900℃ for 10 minutes, and the pressure is finally cooled to release the molybdenum nitride bulk material. The process of the invention is simple, the preparation cycle and sintering time are shortened, air pollution and resource waste are not generated, and two kinds of single-phase molybdenum nitride can be synthesized by optimizing the synthesis temperature, pressure and holding time.

Description

It is prepared by the high temperature and pressure of block materials molybdenum nitride
Technical field
The invention belongs to the technical fields of transition metal nitride preparation, are related to the preparation of molybdenum nitride (MoN) high temperature and pressure Method.
Background technique
Transition metal nitride is due to excellent physicochemical property, such as the low compressed coefficient, high hardness, high heat Stability, excellent electromagnetic property, good wear-resisting and corrosion-resistant etc. characteristics, and it is widely used in protective coating, microelectronics system Diffusion barrier, optics decorative coveringn and multifunction horniness material in system.Wherein, molybdenum nitride all shows especially prominent in various performances Out, such as: catalysis characteristics, high rigidity, the low compressed coefficient and the good electric conductivity etc. of very high plus hydrogen desulfuration.
However, the molybdenum nitride of pure phase block materials is difficult to be synthesized by conventional method.Common synthesis molybdenum nitride Method have high-temperature ammonolysis method (using high activity nitrogen source NH3, N2H4Reacted Deng with the oxide of molybdenum or molybdenum), magnetron sputtering and Vapor deposition
The methods of.The transition metal nitride prepared by these methods is long with the reaction time, condition is harsh, at high cost, production Raw exhaust emission and synthetic sample have the shortcomings that impurity.And the transition metal nitride synthesized by conventional method is powder Shape or film are difficult to test the mechanics such as its hardness, conductivity and electric property.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of new molybdenum nitride (MoN).This method is height with melamine Activated nitrogen source utilizes the molybdenum nitride of the direct synthesizing block material of high temperature and high pressure method using metal molybdenum powder as molybdenum source.Utilize this method Be respectively synthesized sodium chloride structure and be carbonized tungsten structure molybdenum nitride, wherein carbonization tungsten structure molybdenum nitride show it is very high Hardness (convergence 21.5 GPa of hardness), can be used for multiplexing function hard material.
The specific technical solution of the present invention is as described below.
A kind of preparation method of new molybdenum nitride (MoN), the melamine and purity for being 99.99% with purity are 99.99% Molybdenum powder as raw material.Molybdenum nitride bulk is made in technical process through raw material briquetting, assembling, high temperature and pressure synthesis, cooling release Material；The raw material briquetting refers to and molybdenum powder and melamine is used cold press respectively by synthetic cavity size using hydraulic press It with a thickness of the disk and diameter of 1 mm is disk of 4 mm with a thickness of 0.75 mm that be pressed into diameter, which be 4 mm,.By two panels trimerization The piece that cyanamide is pressed into is wrapped in a piece of disk being pressed into molybdenum powder and forms sandwich structure as reaction raw materials.The assembling, It is that the cylindric raw material of sandwich structure is packed into heating container, is put into synthetic cavity；The high temperature and pressure synthesis, is to press Power is 4.0 ~ 5.0 GPa, temperature is heat-insulation pressure keeping 10 minutes at 1500 ~ 1900 DEG C；The cooling release is off energization and adds Block is assembled after heat naturally cools to room temperature, then release.
Experiment of the invention can be completed on the type cubic hinge press of domestic SPD-6 × 600.The experimental results showed that synthesis Size, the temperature of pressure are an important factor for influencing the different phase structure molybdenum nitrides of synthesis.Work as it can be seen from embodiment 1 ~ 2 The nitride that temperature generates when increasing is by a cube opposite hexagonal phase conversion.The preparation condition of synthesis pure phase cubic phase molybdenum nitride is: Synthesis pressure is 5.0 GPa, and synthesis temperature range is 1500 DEG C, heat-insulation pressure keeping 10 minutes.Synthesize pure phase hexagonal phase molybdenum nitride Preparation condition is: synthesis pressure is 4.0 ~ 5.0 GPa, and synthesis temperature is 1800 DEG C, heat-insulation pressure keeping 10 minutes.
In order to guarantee the uniformity of the synthetic cavity temperature in the process of synthetic sample, the heating method that this method uses It is switched on the heating of graphite-pipe heater-type；In order to guarantee that sample does not react with the graphite-pipe for generating heat, the chamber of synthetic sample Body is protected using hexagonal boron nitride.
Present invention process process is simple；Do not generate air pollution；The nitridation molybdenum material of pure phase can be synthesized；By adjusting temperature Degree and pressure can get out of phase molybdenum nitride, and can improve the purity of molybdenum nitride by adjusting temperature and pressure, prepare Material be block materials, be conducive to the test of its mechanical property and electric property.The method of the present invention substantially reduces tradition side The manufacturing cycle of method and the time of sintering, the block materials of synthesis are conducive to optimize its physical and mechanical property.
Detailed description of the invention
Fig. 1: raw material and assembling schematic diagram of the invention；
Fig. 2: nitridation molybdenum compound X-ray diffraction pattern prepared by embodiment 1；
Fig. 3: nitridation molybdenum compound X-ray diffraction pattern prepared by embodiment 2；
Fig. 4: nitridation molybdenum compound X-ray diffraction pattern prepared by embodiment 3；
Fig. 5: nitridation molybdenum compound X-ray diffraction pattern prepared by embodiment 4；
Fig. 6: nitridation molybdenum compound X-ray diffraction pattern prepared by embodiment 5.
Specific embodiment
Embodiment 1:
Using purity be 99.99% melamine and purity be 99.99% molybdenum as raw material.It is big by synthetic cavity using hydraulic press It is small that by molybdenum powder and melamine, with cold press, to be pressed into diameter be 4 mm with a thickness of the disk and diameter of 1 mm is 4 mm thickness respectively Degree is the disk of 0.75 mm.Two panels is wrapped in the piece that melamine is pressed into and a piece of forms Sanming City with the disk that molybdenum powder is pressed into The sample for controlling structure is packed into synthetic cavity.It assembles and uses Graphite thermal tube in cavity, do thermal insulation material with pyrophillite, utilize six Angle boron nitride protects cavity, and (assembling schematic diagram is as shown in Figure 1) synthesis pressure is 5.0 GPa, and synthesis temperature is 1500 DEG C, protects The warm dwell time is 10 minutes, stops release after sample cooled to room temperature after heating, the molybdenum nitride tool that this condition is prepared The X-ray diffraction patterns of body are shown in Fig. 2.
Embodiment 2
Using raw material same as Example 1, assembling same as Example 1 will be used after powder sample compression moulding, closed It is 5.0 GPa at pressure, synthesis temperature is 1800 DEG C, and the pressure-maintaining and heat-preservation time 10 minutes, sample naturally cooled to after stopping heating Release after room temperature, this condition prepare the molybdenum nitride (c-MoN) of cubic phase phase and the mixed phase of hexagonal phase molybdenum nitride (p-MoN). In conjunction with above embodiments 1 it is found that increasing the molybdenum nitride that temperature is conducive to synthesize hexagonal phase.Specific X-ray diffraction patterns are shown in Fig. 3.
Embodiment 3
Using raw material same as Example 1, assembling same as Example 1, synthesis pressure are used after powder sample compression moulding Power is 5.0 GPa, and synthesis temperature is 1900 DEG C, the pressure-maintaining and heat-preservation time 10 minutes, stops sample cooled to room temperature after heating Release afterwards.Synthesize under this condition substantially identical as the sample in embodiment 2.Specific X-ray diffraction patterns are shown in Fig. 4.Thus it says The bright molybdenum nitride for increasing temperature and cannot synthesizing the hexagonal phase of pure phase.Its reason may be that the molybdenum nitride of the hexagonal phase of synthesis hinders The diffusion of nitrogen of high activity.It can be examined by reducing pressure and reducing the thickness of sample, as a result see embodiment 4 and embodiment 5。
Embodiment 4
Using raw material same as Example 1, assembling same as Example 1, synthesis pressure are used after powder sample compression moulding Power is 4 GPa, and synthesis temperature is 1800 DEG C, the pressure-maintaining and heat-preservation time 10 minutes, is stopped after heating after sample cooled to room temperature Release.Synthesize the molybdenum nitride of the hexagonal phase of pure phase under this condition.Specific X-ray diffraction patterns are shown in Fig. 5.
Embodiment 5
Using raw material same as Example 1, molybdenum powder and melamine are used respectively by synthetic cavity size using hydraulic press It is 4 mm with a thickness of the disk and diameter of 0.7 mm is disk of 4 mm with a thickness of 0.75 mm that cold press, which is pressed into diameter,.By two Piece is wrapped in the sample loading synthesis chamber that a piece of disk being pressed into molybdenum powder forms sandwich structure with the piece that melamine is pressed into In body.It assembles and uses Graphite thermal tube in cavity, do thermal insulation material with pyrophillite, protect cavity, synthesis using hexagonal boron nitride Pressure is 5.0 GPa, and synthesis temperature is 1800 DEG C, and the heat-insulation pressure keeping time is 10 minutes, and sample naturally cools to after stopping heating Release after room temperature, the molybdenum nitride that this condition is prepared are that the specific X-ray diffraction patterns of pure phase hexagonal phase molybdenum nitride are shown in Fig. 6.
Above said content, only a specific embodiment of the invention cannot be limited the scope of implementation of the present invention, greatly with it All equivalent changes and improvement carried out according to present patent application range should all still belong to the range that the invention patent covers.

Claims (4)

1.一种氮化钼的高温高压制备方法，是以钼粉、三聚氰胺为原料，经原料压块、组装、高温高压合成、冷却卸压的工艺过程制得氮化钼块状材料；所述的原料压块，是指利用液压机按合成腔体大小将原料做成具有三明治结构（两片三聚氰胺包裹一片钼）的圆柱状；所述的组装，是将块状圆柱状原料装入加热容器，放入合成腔体中；所述的高温高压合成，是在压力为4.0~5.0 GPa、温度为1500~1900 ℃下保温保压10分钟；所述的冷却卸压，是停止通电加热后组装块自然冷却至常温，然后卸压。1. A high temperature and high pressure preparation method for molybdenum nitride, which uses molybdenum powder and melamine as raw materials, and obtains molybdenum nitride bulk material through the process of raw material briquetting, assembly, high temperature and high pressure synthesis, and cooling and pressure relief; The raw material briquetting refers to using a hydraulic press to make the raw material into a cylindrical shape with a sandwich structure (two pieces of melamine wrap a piece of molybdenum) according to the size of the synthesis cavity; the assembly is to put the block cylindrical raw material into a heating container, Put it into the synthesis cavity; the high-temperature and high-pressure synthesis is to maintain the pressure for 10 minutes at a pressure of 4.0 to 5.0 GPa and a temperature of 1500 to 1900 ° C; the cooling and pressure relief is to assemble the block after stopping the power-on heating. Cool to room temperature naturally, and then release the pressure. 2.根据权利要求1所述的氮化钼的高温高压制备方法，其特征是，所述的原料压块，将钼粉和三聚氰胺分别用冷压机压制成直径为4 mm厚度为1 mm的圆片和直径为4 mm厚度为0.75 mm的圆片；将两片用三聚氰胺压成的片包裹着一片用钼粉压成的圆片形成三明治结构的样品装入合成腔体当中；所述的高温高压合成，是在压力为4.0~5.0 GPa、温度为1500~1900 ℃下保温保压10分钟。2. the high-temperature and high-pressure preparation method of molybdenum nitride according to claim 1, is characterized in that, described raw material briquetting, molybdenum powder and melamine are respectively pressed into a diameter of 4 mm and a thickness of 1 mm with a cold press. Discs and discs with a diameter of 4 mm and a thickness of 0.75 mm; two sheets made of melamine are wrapped around a sheet made of molybdenum powder to form a sandwich structure sample into the synthesis cavity; the said High temperature and high pressure synthesis is carried out under the pressure of 4.0~5.0 GPa and the temperature of 1500~1900 ℃ for 10 minutes. 3.一种氮化钼的高温高压制备方法，所述的氮化钼是氯化钠结构的立方相氮化钼；以钼粉和三聚氰胺为原料，经原料压块、组装、高温高压合成、冷却卸压的工艺过程制得立方相的氮化钼材料；所述的原料压块，是指利用液压机按合成腔体大小将原料做成具有三明治结构（两片三聚氰胺包裹一片钼）的圆柱状；所述的组装，是将块状圆柱状原料装入加热容器，放入合成腔体中；所述的高温高压合成，是在压力为5.0 GPa、温度为1500 ℃下保温保压10分钟；所述的冷却卸压，是停止通电加热后组装块自然冷却至常温，然后卸压。3. a high temperature and high pressure preparation method of molybdenum nitride, the molybdenum nitride is a cubic phase molybdenum nitride of sodium chloride structure; using molybdenum powder and melamine as raw materials, through raw material briquetting, assembly, high temperature and high pressure synthesis, The cubic phase molybdenum nitride material is obtained by the process of cooling and pressure relief; the raw material briquetting refers to using a hydraulic press to make the raw material into a cylindrical shape with a sandwich structure (two pieces of melamine wrap a piece of molybdenum) according to the size of the synthesis cavity. ; Described assembling is to pack the block cylindrical raw material into the heating container and put it into the synthesis cavity; the described high temperature and high pressure synthesis is to maintain pressure for 10 minutes at a pressure of 5.0 GPa and a temperature of 1500 °C; The cooling pressure relief means that the assembly block is naturally cooled to normal temperature after the heating is stopped, and then the pressure is relieved. 4.一种氮化钼的高温高压制备方法，所述的氮化钼是碳化钨结构的六角相氮化钼；以钼粉和三聚氰胺为原料，经原料压块、组装、高温高压合成、冷却卸压的工艺过程制得立方相的氮化钼材料；所述的原料压块，将钼粉和三聚氰胺分别用冷压机压制成直径为4 mm厚度为0.7 mm的圆片和直径为4 mm厚度为0.75 mm的圆片；将两片用三聚氰胺压成的片包裹着一片用钼粉压成的圆片形成三明治结构的样品装入合成腔体当中；所述的组装，是将块状圆柱状原料装入加热容器，放入合成腔体中；所述的高温高压合成，是在压力为5.0 GPa、温度为1800 ℃下保温保压10分钟；所述的冷却卸压，是停止通电加热后组装块自然冷却至常温，然后卸压。4. A high-temperature and high-pressure preparation method for molybdenum nitride, wherein the molybdenum nitride is a hexagonal molybdenum nitride of tungsten carbide structure; using molybdenum powder and melamine as raw materials, through raw material briquetting, assembly, high-temperature and high-pressure synthesis, cooling Molybdenum nitride material of cubic phase is obtained in the process of decompression; for the raw material briquette, molybdenum powder and melamine are respectively pressed into circular sheets with a diameter of 4 mm and a thickness of 0.7 mm and a diameter of 4 mm by cold pressing. A disc with a thickness of 0.75 mm; two sheets made of melamine are wrapped around a sheet made of molybdenum powder to form a sandwich structure sample and put into the synthesis cavity; the assembly is to assemble the block cylindrical The raw materials are put into the heating container and put into the synthesis cavity; the high-temperature and high-pressure synthesis is carried out at a pressure of 5.0 GPa and a temperature of 1800 °C for 10 minutes under heat preservation and pressure; After the assembly block is naturally cooled to room temperature, and then the pressure is released.
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