CN1228250C - Method for preparing tungsten disilicide powder - Google Patents
Method for preparing tungsten disilicide powder Download PDFInfo
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- CN1228250C CN1228250C CN 200410039513 CN200410039513A CN1228250C CN 1228250 C CN1228250 C CN 1228250C CN 200410039513 CN200410039513 CN 200410039513 CN 200410039513 A CN200410039513 A CN 200410039513A CN 1228250 C CN1228250 C CN 1228250C
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Abstract
The present invention provides a method for preparing tungsten disilicide powder, which comprises the following steps: tungsten powder and silicon powder are proportioned according to the molar ratio of 1:2, titanium powder and graphite powder are proportioned according to the molar ratio of 1:1, and then the proportioned materials are mixed respectively and uniformly; the W-Si mixed powder is arranged in the center of a crucible, the Ti-C mixed powder is arranged between the W-Si mixed powder and the crucible, finally, one layer of the Ti-C mixed powder is arranged on the top of all of the mixed powder, and the weight ratio of the Ti-C mixed powder to the W-Si mixed powder in the crucible is (0.8 to 1.2): 1; the crucible in which the mixed powder is arranged is put in a sealed reactor which is pumped into vacuum and then filled with argon, and then the reactor is energized by using a tungsten wire to initiate the reaction of the mixed powder; after the reactor is cooled, material after the reaction is taken out, titanium carbide and tungsten disilicide are separated and broken respectively to obtain titanium carbide powder and the tungsten silicide powder. The present invention has the advantages of simple technique, energy saving and time saving, and simultaneously, the powder of TiC can be synthesized.
Description
Technical Field
The invention relates to a method for preparing tungsten disilicide powder. More specifically, the method is a method for synthesizing tungsten disilicide powder by using tungsten powder and silicon powder as raw materials and utilizing the exothermic reaction between tungsten and silicon.
Background
Combustion synthesis, otherwise known as self-propagating high temperature synthesis, is a technique for synthesizing materials using exothermic reactions. For an exothermic reaction, the empirical thermodynamic criterion of whether it will self-sustain until all materials have reacted is the adiabatic combustion temperature T of the reactionad≥1800K。
Reaction to synthesize tungsten disilicide from elemental tungsten and silicon: calculated adiabatic combustion temperature Tad1511K. This does not satisfy the thermodynamic criterion of self-maintenance of the reaction described above. Therefore, it is impossible to synthesize WSi by direct ignition with a mixed powder of tungsten and silicon2In (1).
Munir et al, U.S. Pat. No.5380409 and their article, "Field Effects in Self-promoting Solid State Synthesis Reactions" (Solid State ions, 1997, 101-2. But this requires an additional set of means for applying the electric field and consumes electrical energy.
Disclosure of Invention
The invention aims to provide: a method for preparing tungsten disilicide powder is provided, wherein the synthesis reaction of tungsten and silicon is heated and ignited by the reaction heat of a highly exothermic system.
WSi of the invention2The preparation method comprises the following steps:
(1) mixing tungsten powder and silicon powder according to a molar ratio of 1: 2, mixing titanium powder and graphite powder according to a molar ratio of 1: 1, and then respectively mixing uniformly;
(2) the method comprises the following steps of (1) filling W-Si mixed powder in the center of a crucible, uniformly filling Ti-C mixed powder between the W-Si mixed powder and the crucible, and finally filling a layer of Ti-C mixed powder on the top of all the mixed powder, wherein the weight ratio of the Ti-C mixed powder to the W-Si mixed powder in the crucible is (0.8-1.2) to 1;
(3) filling the crucible filled with the mixed powder into a closed reactor, vacuumizing, filling argon, and electrifying by usinga tungsten wire to initiate the reaction between the mixed materials;
(4) and taking out the reacted material after cooling, separating titanium carbide and tungsten disilicide, and crushing the titanium carbide and the tungsten disilicide respectively to obtain titanium carbide and tungsten disilicide powder.
The reaction of titanium and graphite combustion to form titanium carbide is a highly exothermic reaction which reacts The adiabatic combustion temperature of (2) is up to 3210K. The invention utilizes the reaction heat of the reaction to heat and ignite the synthesized WSi2The reaction of (1): 。
the invention has the advantages that: simple process, energy saving and time saving. And TiC powder can be synthesized at the same time.
Drawings
FIG. 1 is a schematic view showing a manner of filling a mixed powder of titanium and graphite and a mixed powder of tungsten and silicon of the present invention in a crucible. In the figure, a tungsten wire 1, Ti-C mixed powder 2, W-Si mixed powder 3 and a crucible 4 are used for ignition reaction.
FIG. 2 is a diagram of a WSi synthesized in accordance with the present invention2X-ray diffraction pattern of (a). It can be seen that WSi can be obtained according to the present invention2。
Detailed Description
Example 1: firstly, titanium powder and graphite powder as well as tungsten powder and silicon powder are respectively proportioned and uniformly mixed according to the mol ratio of 1: 1 and 1: 2, and then the mixture is loaded into a crucible. The weight ratio of the Ti-C mixed powder and the W-Si mixed powder in the crucible is 0.8: 1, the W-Si mixed powder is filled in the center of the crucible, the Ti-C mixed powder is uniformly filled between the W-Si mixed powder and the crucible, and finally a layer of Ti-C mixed powder is filled on the top of all the mixed powder. And igniting the Ti-C mixed powder on the top layer in the crucible after electrifying the tungsten wire.
Example 2: firstly, titanium powder and graphite powder as well as tungsten powder and silicon powder are respectively proportioned and uniformly mixed according to the mol ratio of 1: 1 and 1: 2, and then the mixture is loaded into a crucible. The weight ratio of the Ti-C mixed powder and the W-Si mixed powder in the crucible is 1.2: 1, the W-Si mixed powder is filled in the center of the crucible, the Ti-C mixed powder is uniformly filled between the W-Si mixed powder and the crucible, and finally a layer of Ti-C mixed powder is filled on the top of all the mixed powder.
As the Ti-C reaction progresses downward, its reaction heat heats and ignites the W-Si mixed powder. Thus, all the mixed powders were fully reacted. To obtain WSi2And meanwhile, TiC powder can be obtained.
Claims (1)
1. A method of preparing tungsten disilicide powder, comprising: the preparation method comprises the following specific steps:
a. mixing tungsten powder and silicon powder according to a molar ratio of 1: 2, mixing titanium powder and graphite powder according to a molar ratio of 1: 1, and then respectively mixing uniformly;
b. the method comprises the following steps of (1) filling W-Si mixed powder in the center of a crucible, uniformly filling Ti-C mixed powder between the W-Si mixed powder and the crucible, and finally filling a layer of Ti-C mixed powder on the top of all the mixed powder, wherein the weight ratio of the Ti-C mixed powder to the W-Si mixed powder in the crucible is (0.8-1.2) to 1;
c. filling the crucible filled with the mixed powder into a closed reactor, vacuumizing, filling argon, and electrifying by using a tungsten wire to initiate the reaction between the mixed materials;
d. and taking out the reacted material after cooling, separating tungsten disilicide from titanium carbide, and crushing the tungsten disilicide and the titanium carbide respectively to obtain tungsten disilicide powder and titanium carbide powder.
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CN 200410039513 CN1228250C (en) | 2004-02-05 | 2004-02-05 | Method for preparing tungsten disilicide powder |
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CN 200410039513 CN1228250C (en) | 2004-02-05 | 2004-02-05 | Method for preparing tungsten disilicide powder |
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CN1557724A CN1557724A (en) | 2004-12-29 |
CN1228250C true CN1228250C (en) | 2005-11-23 |
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CN 200410039513 Expired - Fee Related CN1228250C (en) | 2004-02-05 | 2004-02-05 | Method for preparing tungsten disilicide powder |
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Families Citing this family (2)
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CN104785789A (en) * | 2015-04-16 | 2015-07-22 | 柳州豪祥特科技有限公司 | Silicon-mixed tungsten powder preparation process |
CN115497739B (en) * | 2022-10-25 | 2023-07-04 | 广州市美登电子有限公司 | Alloy magnetic powder core material, preparation method and application thereof |
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