CN1524651A - Preparing process for carbon-deficient type aluminium tungsten carbide solid solution powder - Google Patents
Preparing process for carbon-deficient type aluminium tungsten carbide solid solution powder Download PDFInfo
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- CN1524651A CN1524651A CNA031271618A CN03127161A CN1524651A CN 1524651 A CN1524651 A CN 1524651A CN A031271618 A CNA031271618 A CN A031271618A CN 03127161 A CN03127161 A CN 03127161A CN 1524651 A CN1524651 A CN 1524651A
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- solution powder
- tungsten carbide
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Abstract
The invention belongs to a carbon-deficient solid tungsten-aluminum carbide solution powder preparing method. Its preparing process: it uses binary alloy W0.50Al0.50 as reaction precursor, weighs the binary alloy with carbon powder with less than 300-eye particle size and greater than 95% purity according to the alloy component (W0.50Al0.50)C1-x = 0.01-0.65, where the carbon is excessive by 0-2%, makes uniform ball milling and then placing in graphite crucible, then placing in solid phase reaction furnace, raises the temperature to 1300-1600 deg.C at a speed of 45deg.C/min in vacuum or in reducing and inert atmospheres; during reaction, takes the sample out at intervals of 10-20 hours to make ball milling for 30-60 minutes, so as to accelerate solid phase reaction. The made high-hardness (W0.50Al0.50)C1-x solid solution powder has good resultant crystallization state, and little impurity pollution during synthesis. It has maximum advantages of low time consumption, no noise during production, and simple device and technique, applied to scale production.
Description
Technical field
The invention belongs to the preparation method of carbon omission type tungsten carbide-aluminum solid-solution powder.
Background technology
Tungsten carbide-aluminum is meant that part A l atom enters the case of tungsten in the WC lattice and the substitutional solid solution that forms.Chinese patent (application number 01129544.9) has been reported the preparation method of nanometer tungsten carbide aluminium, and Chinese patent (application number 03121395.2) has been reported the method for preparing tungsten carbide-aluminum by high temperature solid state reaction.
Because the interpolation of aluminium makes tungsten carbide-aluminum have lower density and production cost than wolfram varbide, and the interpolation of aluminium is expected to improve pure WC toughness defect of insufficient.But studies show that hardness ratio wolfram varbide lower slightly of tungsten carbide-aluminum and along with the increase of aluminium content forms the trend of successively decreasing.The hardness that how to improve tungsten carbide-aluminum just becomes one as the problem of scientific value and economic worth.
From the W-C binary alloy phase diagram as can be known, in wolfram varbide synthetic, if the ratio deficiency of carbon then final product be the mixture of wolfram varbide and tungsten, promptly can not generate carbon omission type carbide.Experiment is found, have carbon omission type sosoloid in the tungsten carbide-aluminum system.In the experiment with the powder of the carbon omission type tungsten carbide-aluminum of x＞0.15 after High Temperature High Pressure sinters piece into, its Vickers' hardness is mostly at 2050kg/mm
2More than, with the Vickers' hardness (1400kg/mm of the not omission type tungsten carbide-aluminum of preparation under the equal conditions
2) compare, be significantly improved, and be not less than the hardness (2000kg/mm of the tungsten carbide slug of preparation under the equal sintering condition
2).
Chinese patent (application number 01129545.7) has been reported employing mechanical alloying method and has been prepared tungsten aluminium alloy powder, because partinium has the structure of simple substance tungsten, and the technology of the synthetic WC of the high temperature solid state reaction of W and C is very ripe already, and this just obtains (W for partinium carbonization at high temperature
0.50Al
0.50) C
1-x(x=0.01-0.65) sosoloid provides possibility.
Summary of the invention
Purpose of the present invention provides a kind of preparation method of carbon omission type tungsten carbide-aluminum solid-solution powder.
Synthesis material of the present invention is the carbon dust and the W of the preparation of mechanical alloying synthetic method
0.50Al
0.50Alloy powder.The present invention is after reaction is carried out 5 hours, and each sample confirms all to occur reaction intermediate through the experiment of powder x ray diffraction.This intermediate product is for having six side W
2(the W of C-structure
0.50Al
0.50)
2C
1-xAlong with the passing in reaction times, W
2The peak of C-structure phase is step-down gradually, and reaction is carried out can obtaining final product (W in 50-100 hour
0.50Al
0.50) C
1-xProduct turns out to be through powder x ray diffraction has the symmetric WC structure of six sides.As shown in Figure 1, the x ray diffraction peaks of product is sharp-pointed, does not have assorted peak, and crystal form is good.
Preparation process of the present invention is with W
0.50Al
0.50Binary alloy is as the reaction precursor body, with granularity less than 300 orders, purity is pressed alloy compositions (W greater than 95% carbon dust
0.50Al
0.50) C
1-x=0.01-0.65 weighing, the excessive 0-2% of carbon is in the plumbago crucible of packing into behind the ball milling mixing, put into the solid state reaction stove again, be warming up to 1300-1600 ℃ under vacuum or reducing atmosphere, inert atmosphere, heat-up rate is 45 ℃/minute, and soaking time is 50-100 hour; In the reaction process, sample was taken out ball milling 30-60 minute, accelerate solid-phase reaction velocity with this every 10-20 hour.
Characteristics of the present invention are to prepare carbon omission type, high rigidity (W by high temperature solid state reaction
0.50Al
0.50) C
1-xSolid-solution powder, the product crystal form is good, and the building-up process contaminating impurity is few.This method biggest advantage is consuming time few, the production process noiselessness, and equipment, technology are simple, are fit to large-scale production.
Embodiment
Embodiment 1: with W
0.50Al
0.50Alloy powder, purity are greater than 97%, and with carbon dust, granularity is less than 300 orders, and purity is greater than 95%, by (W
0.50Al
0.50) C
0.99Weighing, C is inexcessive, and the raw material total amount is 15 grams, and the plumbago crucible of packing into behind the ball milling mixing is put into the solid state reaction stove again, is warming up to 1600 ℃ under vacuum condition.Every reaction was taken out after 20 hours, ball milling 30 minutes.React and to get product (W in 80 hours
0.5Al
0.5) C
0.99
Embodiment 2: with W
0.50Al
0.50Alloy powder, purity is the same, and with carbon dust, granularity, purity are the same, by (W
0.50Al
0.50) C
0.85Weighing, C is excessive 1%, and the raw material total amount is the same, and the plumbago crucible of packing into behind the ball milling mixing is put into the solid state reaction stove again, under protection of inert gas, is warming up to 1550 ℃, and every insulation was then taken out ball milling in 15 hours 40 minutes.Total soaking time reach 75 hours and get final product product (W
0.50Al
0.50) C
0.85, its sintered compact vickers hardness number is 2213kg/mm
2
Embodiment 3:W
0.50Al
0.50Alloy powder, purity is the same, and with carbon dust, granularity, purity are the same, by (W
0.50Al
0.50) C
0.65Weighing, carbon is excessive 2%, and the raw material total amount is the same.The plumbago crucible of packing into behind the ball milling mixing is put into the solid state reaction stove again, under the hydrogen reducing atmosphere protection, is warming up to 1450 ℃.Every insulation was then taken out ball milling in 13 hours 60 minutes, reacted to obtain product (W after 65 hours
0.50Al
0.50) C
0.65, its sintered compact vickers hardness number is 2301kg/mm
2
Embodiment 4:W
0.50Al
0.50Alloy powder, purity is the same, and with carbon dust, purity, granularity are the same, by (W
0.50Al
0.50) C
0.50Weighing, C is excessive 2%, and the raw material total amount is the same, and the solid state reaction condition is with (W
0.50Al
0.50) C
0.99, every insulation was then taken out ball milling in 10 hours 60 minutes, can get product (W after 50 hours
0.50Al
0.5) C
0.50, its x-ray diffractogram of powder is seen accompanying drawing 1.Product sintered compact vickers hardness number is 2508kg/mm
2
Embodiment 5: with W
0.50Al
0.50Alloy powder, purity is the same, and with carbon dust, purity, granularity are the same, by (W
0.50Al
0.50) C
0.35Weighing, C is excessive 1%, and the raw material total amount is the same; the plumbago crucible of packing into behind the wolfram varbide spherical tank ball milling mixing is put into the solid state reaction stove, again under protection of inert gas; be warming up to 1300 ℃, every insulation was then taken out ball milling in 10 hours 60 minutes, reacted can get product (W after 100 hours
0.50Al
0.50) C
0.35, powder x ray diffraction characteristic peak is sharp-pointed, does not have assorted peak, and crystal form is good.
Embodiment 6: with (W
0.50Al
0.50) alloy powder, purity is the same, and with carbon dust, purity, granularity are the same, by (W
0.50Al
0.50) C
0.50Weighing, C is excessive 1%, and the raw material total amount is the same, and ball milling mixes and puts into the solid state reaction stove again after 18 hours, at vacuum gas and down, is warming up to 1450 ℃, is incubated 20 hours and can gets product (W
0.50Al
0.50) C
0.50, powder x ray diffraction characteristic peak is sharp-pointed, does not have assorted peak, and crystal form is good.Its sintered compact vickers hardness number is 2554kg/mm
2
Claims (1)
1. the preparation method of carbon omission type tungsten carbide-aluminum solid-solution powder is characterized in that W
0.50Al
0.50Binary alloy is as the reaction precursor body, with granularity less than 300 orders, purity is pressed alloy compositions (W greater than 95% carbon dust
0.50Al
0.50) C
1-xThe x=0.01-0.65 weighing, the excessive 0-2% of carbon is in the plumbago crucible of packing into behind the ball milling mixing, put into the solid state reaction stove again, be warming up to 1300-1600 ℃ under vacuum or reducing atmosphere, inert atmosphere, heat-up rate is 45 ℃/minute, and soaking time is 50-100 hour; In the reaction process, sample was taken out ball milling 30-60 minute, make high rigidity (W at last every 10-20 hour
0.50Al
0.50) C
1-xSolid-solution powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03127161 CN1208161C (en) | 2003-09-17 | 2003-09-17 | Preparing process for carbon-deficient type aluminium tungsten carbide solid solution powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03127161 CN1208161C (en) | 2003-09-17 | 2003-09-17 | Preparing process for carbon-deficient type aluminium tungsten carbide solid solution powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1524651A true CN1524651A (en) | 2004-09-01 |
| CN1208161C CN1208161C (en) | 2005-06-29 |
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ID=34285989
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03127161 Expired - Fee Related CN1208161C (en) | 2003-09-17 | 2003-09-17 | Preparing process for carbon-deficient type aluminium tungsten carbide solid solution powder |
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|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299860C (en) * | 2004-10-26 | 2007-02-14 | 中国科学院长春应用化学研究所 | Preparing process for carbon-position vacancy type tungsten carbide aluminium sintering body |
| CN102660707A (en) * | 2012-06-08 | 2012-09-12 | 株洲硬质合金集团有限公司 | Production method for WC-Al4W pre-alloy powder |
-
2003
- 2003-09-17 CN CN 03127161 patent/CN1208161C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299860C (en) * | 2004-10-26 | 2007-02-14 | 中国科学院长春应用化学研究所 | Preparing process for carbon-position vacancy type tungsten carbide aluminium sintering body |
| CN102660707A (en) * | 2012-06-08 | 2012-09-12 | 株洲硬质合金集团有限公司 | Production method for WC-Al4W pre-alloy powder |
| CN102660707B (en) * | 2012-06-08 | 2013-07-31 | 株洲硬质合金集团有限公司 | Production method for WC-Al4W pre-alloy powder |
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| Publication number | Publication date |
|---|---|
| CN1208161C (en) | 2005-06-29 |
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Granted publication date: 20050629 Termination date: 20190917 |