CN105478753B - Tungsten carbide and tungsten composite powder and preparation method thereof - Google Patents
Tungsten carbide and tungsten composite powder and preparation method thereof Download PDFInfo
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- CN105478753B CN105478753B CN201510937763.3A CN201510937763A CN105478753B CN 105478753 B CN105478753 B CN 105478753B CN 201510937763 A CN201510937763 A CN 201510937763A CN 105478753 B CN105478753 B CN 105478753B
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- tungsten
- carbide
- tungsten carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
- Coating By Spraying Or Casting (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses tungsten carbide and tungsten composite powder and a preparation method thereof, and the tungsten carbide powder is firstly placed in an inert gas environment; then introducing oxygen with the molar ratio of 1-5%, heating to 300-800 ℃, and preserving heat for 5-30 minutes to decarburize the surface of the tungsten carbide to form a mixture of tungsten and tungsten oxide; then introducing hydrogen as a reducing agent, wherein the introduction amount is 0.5-4 m3Heating to 600-800 ℃, preserving heat for 1-2 hours, then heating to 1100-1500 ℃, preserving heat for 10-30 minutes, and obtaining the tungsten carbide composite powder with tungsten on the surface.
Description
Technical field
The present invention relates to heat spray coating layer material technical field, more particularly to the composite powder of a kind of tungsten carbide and tungsten and its
Preparation method.
Background technology
At present, tungsten carbide or ditungsten carbide are conventional metal ceramic wear-resisting materials, in field of thermal spray, with tungsten carbide or
Ditungsten carbide is widely used under various wear-resisting working conditions for the metal-cermic spraying material of hard, wear-resistant phase.
But in thermal spraying or spray process, because spraying temperature is higher, tungsten carbide easily decomposes generation ditungsten carbide, and then
η phases (Co is generated due to the presence of surrounding metal Binder Phase3W3C、Co6W6C etc.), the hardness that η phases not only reduce coating is also tight
The toughness of coating is reduced again, and the generation of η phases is due to that the diffusion of carbon in a metal causes, and how to suppress carbon in spraying or surfacing
In diffusion turn into improve coating toughness key.
The content of the invention
, can be using this method it is an object of the invention to provide composite powder of a kind of tungsten carbide and tungsten and preparation method thereof
Tungsten carbide surface forms the metal tungsten layer of one layer of continuous-stable, and the generation of η phases is prevented in spraying or spray process, is effectively improved
The toughness of coating.
A kind of composite powder of tungsten carbide and tungsten, for the composite powder using tungsten carbide as core, tungsten is distributed in the carbonization
The surface of tungsten forms complete clad；
And the thickness of tungsten layer is the 1~5% of the tungsten carbide core granule diameter.
The diameter range of the tungsten carbide core granule is：1~200 micron；
And the thickness range of tungsten layer is 0.05~5 micron.
Present invention also offers the preparation method of a kind of tungsten carbide and the composite powder of tungsten, methods described includes：
By tungsten-carbide powder as under inert gas environment；
Then pass to mol ratio and be 1~5% oxygen, and be heated to 300~800 DEG C, be incubated 5~30 minutes so that carbon
Change the mixture that tungsten skin decarburization forms tungsten and tungsten oxide；
Hydrogen is passed through again as reducing agent, and intake is 0.5~4m3/ h, and 600~800 DEG C are heated to, insulation 1~2 is small
When；
Then 1100~1500 DEG C are again heated to, is incubated 10~30 minutes, obtains the wolfram carbine composite powder that surface is tungsten.
The inert gas is：The gas and combination of gases not chemically reacted with tungsten carbide；
Specifically include：Nitrogen or argon gas.
The tungsten carbide is replaced with into ditungsten carbide.
As seen from the above technical solution provided by the invention, one layer of company can be formed in tungsten carbide surface using this method
Continue stable metal tungsten layer, the generation of η phases is prevented in spraying or spray process, effectively improves the toughness of coating.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is provided the preparation method schematic flow sheet of the composite powder of tungsten carbide and tungsten by the embodiment of the present invention.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
Preparation method described in the embodiment of the present invention passes through in one layer of tungsten layer of tungsten carbide (or ditungsten carbide) Surface Creation, shape
Into the composite powder of tungsten carbide/tungsten, and as spraying, surfacing raw material, to solve tungsten carbide (or ditungsten carbide) in thermal jet
Apply, the problem of η phases is easily generated in spray process.
For the tungsten carbide and the composite powder of tungsten that the embodiment of the present invention is provided using tungsten carbide as core, tungsten is distributed in the carbon
The surface for changing tungsten forms complete clad；
And the thickness of tungsten layer is the 1~5% of the tungsten carbide core granule diameter.
In the specific implementation, the diameter range of the tungsten carbide core granule is：1~200 micron；And the thickness range of tungsten layer is
0.05~5 micron.
The preparation method flow for providing the composite powder of tungsten carbide and tungsten by the embodiment of the present invention as shown in Figure 1 is illustrated
Figure, methods described include：
Step 11：By tungsten-carbide powder as under inert gas environment；
Here, the inert gas is：The gas and combination of gases not chemically reacted with tungsten carbide；
It can specifically include：Nitrogen or argon gas.
Step 12：Then pass to mol ratio and be 1~5% oxygen, and be heated to 300~800 DEG C, be incubated 5~30 minutes,
So that tungsten carbide surface decarburization forms the mixture of tungsten and tungsten oxide；
Step 13：Hydrogen is passed through again as reducing agent, and intake is 0.5~4m3/ h, and 600~800 DEG C are heated to, protect
Temperature 1~2 hour；
In this step, the hydrogen can also be replaced with other reducibility gas, such as decompose ammonia, carbon monoxide.
Step 14：Then 1100~1500 DEG C are again heated to, is incubated 10~30 minutes, surface is obtained and is answered for the tungsten carbide of tungsten
Close powder.
In the specific implementation, above-mentioned tungsten carbide can also replace with ditungsten carbide.
The technical process of above-mentioned preparation method is described in detail with specific example below：
Embodiment 1, first by grain graininess d50=10 microns of tungsten carbide is placed in nitrogen, oxygen mixed gas, wherein
Oxygen accounts for the 1.5% of gas gross, is heated to 350 DEG C, is incubated 10 minutes；
Then pass to hydrogen, hydrogen flowing quantity：0.5m3/ h, 630 DEG C are heated to, are incubated 1 hour；
1100 DEG C are increased to again, is incubated 10 minutes, and obtaining the Surface coating tungsten-carbide powder of tungsten layer, tungsten layer thickness is about
0.3 micron.
Embodiment 2, first by grain graininess d50=60 microns of tungsten carbide/ditungsten carbide eutectic powder is placed in nitrogen, oxygen
In oxygen mixture, wherein oxygen accounts for the 5% of gas gross, is heated to 800 DEG C, is incubated 15 minutes；
Then pass to hydrogen, hydrogen flowing quantity：2m3/ h, 780 DEG C are heated to, are incubated 1.5 hours；
1300 DEG C are increased to again, is incubated 30 minutes, and obtaining the Surface coating tungsten-carbide powder of tungsten layer, tungsten layer thickness is about
1.5 micron.
Embodiment 3, first by grain graininess d50=2 microns of tungsten-carbide powder is placed in nitrogen, oxygen mixed gas, its
Middle oxygen accounts for the 2% of gas gross, is heated to 300 DEG C, is incubated 10 minutes；
Then pass to hydrogen, hydrogen flowing quantity：4m3/ h, 720 DEG C are heated to, are incubated 1 hour；
1150 DEG C are increased to again, is incubated 30 minutes, and obtaining the Surface coating tungsten-carbide powder of tungsten layer, tungsten layer thickness is about
0.1 micron.
In summary, the method provided using the embodiment of the present invention can be in tungsten carbide surface one layer of continuous-stable of formation
Metal tungsten layer, the generation of η phases is prevented in spraying or spray process, effectively improve the toughness of coating.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can readily occur in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (4)
1. the preparation method of the composite powder of a kind of tungsten carbide and tungsten, it is characterised in that methods described includes：
Tungsten-carbide powder is placed under inert gas environment；
Then pass to molar content and be 1~5% oxygen, and be heated to 300~800 DEG C, be incubated 5~30 minutes so that carbonization
Tungsten skin decarburization forms the mixture of tungsten and tungsten oxide；
Hydrogen is passed through again as reducing agent, and intake is 0.5~4m3/ h, and 600~800 DEG C are heated to, it is incubated 1~2 hour；
Then 1100~1500 DEG C are again heated to, is incubated 10~30 minutes, obtains the wolfram carbine composite powder that surface is tungsten；
Wherein, for the composite powder using tungsten carbide as core, the surface that tungsten is distributed in the tungsten carbide forms complete clad；
And the thickness of tungsten layer is the 1~5% of the tungsten carbide core granule diameter；
The diameter range of the tungsten carbide core granule is 1~200 micron；
And the thickness range of tungsten layer is 0.05~5 micron.
2. the preparation method of the composite powder of tungsten carbide and tungsten according to claim 1, it is characterised in that
The inert gas is the gas and combination of gases not chemically reacted with tungsten carbide.
3. the preparation method of the composite powder of tungsten carbide and tungsten according to claim 2, it is characterised in that
The inert gas specifically includes：Nitrogen or argon gas.
4. the preparation method of the composite powder of tungsten carbide and tungsten according to claim 1, it is characterised in that
The tungsten carbide is replaced with into ditungsten carbide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510937763.3A CN105478753B (en) | 2015-12-15 | 2015-12-15 | Tungsten carbide and tungsten composite powder and preparation method thereof |
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| CN201510937763.3A CN105478753B (en) | 2015-12-15 | 2015-12-15 | Tungsten carbide and tungsten composite powder and preparation method thereof |
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| CN105478753A CN105478753A (en) | 2016-04-13 |
| CN105478753B true CN105478753B (en) | 2018-02-06 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106747449B (en) * | 2016-12-26 | 2020-06-09 | 哈尔滨职业技术学院 | Novel tungsten carbide composite material and preparation method thereof |
| CN107716917B (en) * | 2017-09-20 | 2019-07-23 | 西安理工大学 | A kind of method that gas carburization method reaction in-situ prepares W/WC composite powder |
| CN109321803B (en) * | 2018-11-30 | 2021-03-23 | 苏州艾默特材料技术有限公司 | Heating element with porous ceramic coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62192501A (en) * | 1986-02-18 | 1987-08-24 | Mitsubishi Metal Corp | Co-w coated wc powder |
| US5912399A (en) * | 1995-11-15 | 1999-06-15 | Materials Modification Inc. | Chemical synthesis of refractory metal based composite powders |
| CN1608983A (en) * | 2004-09-16 | 2005-04-27 | 北京科技大学 | Prepn process of nano level tungsten powder and WC powder |
-
2015
- 2015-12-15 CN CN201510937763.3A patent/CN105478753B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62192501A (en) * | 1986-02-18 | 1987-08-24 | Mitsubishi Metal Corp | Co-w coated wc powder |
| US5912399A (en) * | 1995-11-15 | 1999-06-15 | Materials Modification Inc. | Chemical synthesis of refractory metal based composite powders |
| CN1608983A (en) * | 2004-09-16 | 2005-04-27 | 北京科技大学 | Prepn process of nano level tungsten powder and WC powder |
Non-Patent Citations (1)
| Title |
|---|
| 碳化钨涂覆金刚石的新方法;李玲玲;《中国钨业》;19970410(第04期);第27页 * |
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