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 PDFInfo
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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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- 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
- C01B21/0615—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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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/21—Attrition-index or crushing strength of granulates
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- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
The high temperature and high pressure preparation process of block materials molybdenum nitride of the present invention belongs to the technical field of transition metal nitride preparation.Preparation process is that molybdenum powder and melamine are utilized respectively hydraulic press tabletting, are made into sandwich structure, is sized for by synthetic cavity cylindric using molybdenum powder and melamine as raw material；Cylindric raw material is packed into heating container, is put into synthetic cavity, in the case where pressure is 4.0 ~ 5.0 GPa, temperature is 1500 ~ 1900 DEG C heat-insulation pressure keeping 10 minutes；Release is finally cooled down, molybdenum nitride bulk material is made.Present invention process process is simple, shortens manufacturing cycle and sintering time；Do not generate air pollution and the wasting of resources；By optimum synthesis temperature, pressure and soaking time, the molybdenum nitride of two kinds of single-phases can be synthesized.
Description
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. a kind of high temperature and high pressure preparation process of molybdenum nitride is using molybdenum powder, melamine as raw material, through raw material briquetting, assembling, height
Molybdenum nitride bulk material is made in warm high-pressure synthesis, the technical process for cooling down release；The raw material briquetting, refers to and utilizes hydraulic press
Raw material is made into the cylindric of sandwich structure (two panels melamine wraps up a piece of molybdenum) by synthetic cavity size；Described
Assembling is that blocky cylindric raw material 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
Block is assembled after heating naturally cools to room temperature, then release.
2. the high temperature and high pressure preparation process of molybdenum nitride according to claim 1, characterized in that the raw material briquetting, it will
Molybdenum powder and melamine respectively with cold press be pressed into diameter be 4 mm with a thickness of the disk and diameter of 1 mm be 4 mm with a thickness of
The disk of 0.75 mm；Two panels is wrapped in a piece of disk being pressed into molybdenum powder with the piece that melamine is pressed into and forms sandwich knot
The sample of structure is packed into synthetic cavity；The described high temperature and pressure synthesis, be pressure be 4.0 ~ 5.0 GPa, temperature be 1500 ~
Heat-insulation pressure keeping 10 minutes at 1900 DEG C.
3. a kind of high temperature and high pressure preparation process of molybdenum nitride, the molybdenum nitride is the cubic phase molybdenum nitride of sodium chloride structure；With
Molybdenum powder and melamine are raw material, are synthesized through raw material briquetting, assembling, high temperature and pressure, obtained cube of the technical process of cooling release
The nitridation molybdenum material of phase；The raw material briquetting is referred to and raw material is made into Sanming City by synthetic cavity size using hydraulic press
Control the cylindric of structure (two panels melamine wraps up a piece of molybdenum)；The assembling is that blocky cylindric raw material is packed into heating
Container is put into synthetic cavity；The high temperature and pressure synthesis, is kept the temperature in the case where pressure is 5.0 GPa, temperature is 1500 DEG C
Pressure maintaining 10 minutes；The cooling release, assembling block naturally cools to room temperature after being off electrified regulation, then release.
4. a kind of high temperature and high pressure preparation process of molybdenum nitride, the molybdenum nitride is the hexagonal phase molybdenum nitride of carbonization tungsten structure；With
Molybdenum powder and melamine are raw material, are synthesized through raw material briquetting, assembling, high temperature and pressure, obtained cube of the technical process of cooling release
The nitridation molybdenum material of phase；The raw material briquetting, it is 4 mm thick that molybdenum powder and melamine, which are pressed into diameter with cold press respectively,
Degree is the disk of 0.7 mm and diameter is disk of 4 mm with a thickness of 0.75 mm；Two panels is wrapped up with the piece that melamine is pressed into
The a piece of disk that is pressed into molybdenum powder form the sample of sandwich structure and be packed into synthetic cavity；The assembling is by block
The cylindric raw material of shape is packed into heating container, is put into synthetic cavity；The described high temperature and pressure synthesis, be pressure be 5.0 GPa,
Temperature is heat-insulation pressure keeping 10 minutes at 1800 DEG C；The cooling release, assembling block naturally cools to after being off electrified regulation
Room temperature, then release.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113942982A (en) * | 2021-12-01 | 2022-01-18 | 四川大学 | MoP/Mo2N composite material and preparation method and application thereof |
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