CN105645416B - A kind of inexpensive molybdenum disilicide and preparation method thereof - Google Patents
A kind of inexpensive molybdenum disilicide and preparation method thereof Download PDFInfo
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- CN105645416B CN105645416B CN201610007014.5A CN201610007014A CN105645416B CN 105645416 B CN105645416 B CN 105645416B CN 201610007014 A CN201610007014 A CN 201610007014A CN 105645416 B CN105645416 B CN 105645416B
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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
- C01B33/00—Silicon; Compounds thereof
- C01B33/06—Metal silicides
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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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- 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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Abstract
The invention discloses a kind of inexpensive molybdenum disilicide and preparation method thereof, belong to technical field of material.The method that prior art prepares molybdenum disilicide is as raw material, because the price of Mo powder is higher, so the cost of prior art production molybdenum disilicide is higher with Mo powder and Si powder.The present invention is using the relatively low MoS of price2Powder and Si powder are used as raw material.First by MoS2Powder and Si powder are mixed by certain mol proportion dispensing, and uniform mixing, briquetting, roasting obtains molybdenum disilicide.The present invention directly uses MoS2Powder and Si powder prepare molybdenum disilicide, and cost is low, simple to operate, react easily controllable, solve prior art and prepare the problem of molybdenum disilicide cost is high.
Description
Technical field
The invention belongs to technical field of material, a kind of inexpensive molybdenum disilicide and preparation method thereof is disclosed, especially
It relate to one kind MoS2The method that powder and Si powder prepare molybdenum disilicide as raw material.
Background technology
Molybdenum disilicide has high-melting-point, low-density, good thermal conductivity and good electric conductivity and excellent high temperature anti-
Oxidisability, high elastic modulus, low thermal coefficient of expansion, higher intensity, thermal shock resistance resistant to chemical etching and good.Extensively should
It is also extremely potential high-temperature structural material and resistance to for high temperature exothermic body element material and high-temperature oxidation resistant coating material
Grind material.
With developing rapidly for PM technique and material technology.MoSi2Preparation technology, which is also achieved, great to be entered
Exhibition, on the basis of the techniques such as knot are urged in the compacting of conventional arc melting, casting and powder, late 1980s self propagating high temperature is closed
Into (SHS), mechanical alloying (MA), the technology such as hot pressing (HP) achieves quick development, and they overcome traditional handicraft MoSi2
Fusing point is high, difficult synthesis, and material shortcoming oxidizable in building-up process.Occur in that spark plasma sintering is new again a few years ago
Technique, and SHS and MA also occur in that new expansion.However, these methods all use molybdenum powder and silica flour as raw material, due to molybdenum
The price of powder is higher, so causing cost of material higher.
China is the abundant country of molybdenum ore resource, by the end of the year 2008, according to《National Resource management circular》China is
Verify at Molybdenum Mining Area 411, molybdenum ore finds out that resource reserve up to 1232.23 ten thousand t, occupies the first in the world.And Molybdenum Ore in China is with original
Based on raw vulcanization molybdenum ore.If can substitute molybdenum powder as raw material with the relatively low molybdenum sulfide of price prepares molybdenum disilicide, this will be very big
Reduction prepare the cost of material of molybdenum disilicide, so as to reduce the production cost of molybdenum disilicide.Also, directly utilize the sulphur of China
Change Mo resource, eliminate molybdenum sulfide to the long flow preparation section of molybdenum, it is possible to reduce resource consumption and environmental pollution.
The content of the invention
MoS is used it is an object of the invention to provide one kind2Powder and Si powder prepare molybdenum disilicide as the low cost of raw material
Method, it is to be solved to be molybdenum powder as raw material and prepare the problem of molybdenum disilicide cost is too high.
To reach above-mentioned purpose, the technical scheme that the present invention is provided is：
A kind of method that low cost prepares molybdenum disilicide, this preparation method is with MoS2Powder and Si powder are as raw material, and mixing is equal
It is even that molybdenum disilicide product is obtained after kiln roasting, cooling.
The preferred scheme of the method is, the MoS2Powder and Si powder mol ratio are 1:3.5~4.5.
The preferred scheme of the method is to be pressed into after block, be calcined after the raw material is well mixed.
The preferred scheme of the method is, the MoS2The purity of powder is more than 96%, and granularity is less than 0.1mm；The Si powder
Purity is more than 98%, and granularity is less than 0.1mm.
The preferred scheme of the method is that the roasting technique is to be incubated 1~5 hour at 1000~1600 DEG C.
The preferred scheme of the method is, including following preparation process：
(1) by MoS2Powder and Si powder in molar ratio 1:3.5~4.5 dispensings are mixed, and obtain well mixed powder material；
(2) powder material that will be obtained in (1), carries out briquetting with the pressure more than 1MPa at room temperature, obtains block former
Material；
(3) under the protection of inert gas, by the block stock obtained in (2) in high temperature kiln roasting, 1000~
1~5 hour is incubated at 1600 DEG C；
(4) insulation terminates, and cools down, obtains molybdenum disilicide product.
The preferred scheme of the method is that the roasting technique described in step (3) is that 4~6 are incubated at 1000~1200 DEG C
Hour.
The preferred scheme of the method is, the MoS2Powder and Si powder mol ratio are 1:3.8~4.2.
The preferred scheme of the method is, the MoS2Powder and Si powder mol ratio are 1:4.
In the method, the hybrid mode of the raw material is grinding, is stirred, one kind in ball milling；Block stock in step (3)
The stove time that enters be to be heated up with stove or to temperature enter stove；Step (4) is described to be cooled to directly take out room temperature under furnace cooling or high temperature
Middle blown inert gas cooling.
The invention further relates to molybdenum disilicide prepared by the above method, its purity is more than 96%.
The technical scheme provided using the present invention, compared with existing known technology, is had the advantages that：
(1) of the invention this uses MoS2Powder can effectively utilize the MoS of China's abundant as raw material2Resource, reduces system
The production cost of standby molybdenum disilicide；
(2) preparation technology of the invention, eliminates MoS2To Mo production process, process is shortened, resource has been saved, dropped
Low production cost；
(3) present invention passes through the control to proportion of raw material number, the selection of roasting technique and other technological parameters
Reasonable selection, the molybdenum disilicide purity of preparation is high, and impurity is few.
Brief description of the drawings
Fig. 1 is the XRD interpretation of result figures of the product component of embodiment one.
Embodiment
To further appreciate that present disclosure, with reference to accompanying drawing, the present invention is described in detail.With reference to embodiment pair
The present invention is further described.
Embodiment one：
(1) it is the MoS that 98%, granularity is less than 0.05mm by purity2Powder and purity are that 99.99%, granularity is less than 0.05mm
Si powder in molar ratio 1:4 dispensings, with taking powder sample gross mass to be 5g, add alcohol grinding, are well mixed, dry, mixing is made
Uniform powder material.
(2) powder material that will be obtained in (1), with 5MPa pressure briquetting, room temperature depresses to a diameter of 18mm cylinder
Shape block.
(3) under argon atmosphere, the block stock obtained in (2) to temperature is entered into stove, 1600 DEG C of insulations 1 of sintering temperature
Hour.
(4) insulation terminates, and takes out Argon in room temperature and cools down, obtaining molybdenum disilicide, (molecular formula is MoSi2), its purity is
98.7%, XRD diffraction pattern such as Fig. 1.
Embodiment two：
(1) it is the MoS that 96%, granularity is less than 0.1mm by purity2Powder and purity are the Si powder that 98%, granularity is less than 0.1mm
In molar ratio 1:4 dispensings, with taking powder sample gross mass to be 5g, addition alcohol grinding is well mixed, dried, is made what is be well mixed
Powder material.
(2) under argon atmosphere, the powder material obtained in (1) is heated up with stove, 1200 DEG C of insulations 4 of sintering temperature
Hour.
(3) insulation terminates, furnace cooling, and obtaining molybdenum disilicide, (molecular formula is MoSi2), its purity is 96.3%.
Embodiment three：
(1) it is that MoS2 powder and purity that 98%, granularity is less than 0.01mm are the Si that 99%, granularity is less than 0.01mm by purity
Powder in molar ratio 1:4 dispensings, with taking powder sample gross mass to be 5g, add alcohol grinding, are well mixed, dry, be made well mixed
Powder material.
(2) powder material that will be obtained in (1), at room temperature with 10MPa pressure briquetting, is pressed into a diameter of 18mm cylinder
Shape block.
(3) under argon atmosphere, the block stock obtained in (2) to temperature is entered into stove, 1000 DEG C of insulations 5 of sintering temperature
Hour.
(4) insulation terminates, and takes out Argon in room temperature and cools down, obtains molybdenum disilicide (molecular formula is MoSi2), its purity is
98.2%.
Claims (8)
1. a kind of method that low cost prepares molybdenum disilicide, it is characterised in that this preparation method is with MoS2Powder and Si powder are used as original
Material, is well mixed after kiln roasting, cooling and obtains molybdenum disilicide product；Wherein described MoS2Powder and Si powder mol ratio are 1:
3.5~4.5；The roasting technique is to be incubated 1~5 hour at 1000~1600 DEG C.
2. the method that a kind of low cost according to claim 1 prepares molybdenum disilicide, it is characterised in that the raw material mixing
It is pressed into after block, is calcined after uniform.
3. the method that a kind of low cost according to claim 1 prepares molybdenum disilicide, it is characterised in that the MoS2Powder
Purity is more than 96%, and granularity is less than 0.1mm；The purity of the Si powder is more than 98%, and granularity is less than 0.1mm.
4. the method that a kind of low cost according to claim 1 prepares molybdenum disilicide, it is characterised in that including following system
Standby step：
(1) by MoS2Powder and Si powder in molar ratio 1:3.5~4.5 dispensings are mixed, and obtain well mixed powder material；
(2) powder material that will be obtained in (1), carries out briquetting with the pressure more than 1MPa at room temperature, obtains block stock；
(3) under the protection of inert gas, by the block stock obtained in (2) in high temperature kiln roasting, at 1000~1600 DEG C
Lower insulation 1~5 hour；
(4) insulation terminates, and cools down, obtains molybdenum disilicide product.
5. the method that a kind of low cost according to claim 4 prepares molybdenum disilicide, it is characterised in that institute in step (3)
The roasting technique stated is to be incubated 4~5 hours at 1000~1200 DEG C.
6. the method that a kind of low cost according to claim 1 or 4 prepares molybdenum disilicide, it is characterised in that the MoS2Powder
It is 1 with Si powder mol ratio:3.8~4.2.
7. the method that a kind of low cost according to claim 1 or 4 prepares molybdenum disilicide, it is characterised in that the MoS2Powder
It is 1 with Si powder mol ratio:4.
8. molybdenum disilicide prepared by the methods described of claim 1 or 4, it is characterised in that its purity is more than 96%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610007014.5A CN105645416B (en) | 2016-01-05 | 2016-01-05 | A kind of inexpensive molybdenum disilicide and preparation method thereof |
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| CN201610007014.5A CN105645416B (en) | 2016-01-05 | 2016-01-05 | A kind of inexpensive molybdenum disilicide and preparation method thereof |
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| CN105645416A CN105645416A (en) | 2016-06-08 |
| CN105645416B true CN105645416B (en) | 2017-10-31 |
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| CN107043111B (en) * | 2017-01-09 | 2019-11-08 | 北京科技大学 | A method of silica gel is prepared using silicon monosulfide hydrolysis |
| CN111847458B (en) * | 2020-07-31 | 2022-05-20 | 辽宁中色新材科技有限公司 | Preparation method of high-purity and low-cost molybdenum disilicide |
| CN113086985B (en) * | 2021-03-25 | 2022-04-15 | 北京科技大学 | Low-cost preparation method of molybdenum silicide without emission of sulfur-containing gas |
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| FR2114251A5 (en) * | 1970-11-20 | 1972-06-30 | Pechiney | Metal silicide prepn - from halosilane and metal sulphides at below 900c |
| CN100465090C (en) * | 2007-01-04 | 2009-03-04 | 北京科技大学 | Method of preparing molybdenum silicide powder |
| JP5313858B2 (en) * | 2009-12-21 | 2013-10-09 | 株式会社豊田中央研究所 | MnSix powder and manufacturing method thereof, and CaSiy powder for manufacturing MnSix powder and manufacturing method thereof |
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