CN102154581A - Preparation method of nano chromium carbide composite powder - Google Patents
Preparation method of nano chromium carbide composite powder Download PDFInfo
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- CN102154581A CN102154581A CN 201110070999 CN201110070999A CN102154581A CN 102154581 A CN102154581 A CN 102154581A CN 201110070999 CN201110070999 CN 201110070999 CN 201110070999 A CN201110070999 A CN 201110070999A CN 102154581 A CN102154581 A CN 102154581A
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Abstract
The invention relates to a preparation method of nano chromium carbide composite powder, which comprises the following steps: ball-milling the nickel-chromium alloy powder, placing the ball-milled nickel-chromium alloy powder in an atmosphere furnace, introducing mixed gas comprising hydrogen and carbon-containing gas, and keeping the furnace temperature of the atmosphere furnace between 650 and 950 ℃; and (3) crushing and grading the chromium carbide composite powder obtained after heat preservation. The invention takes nickel-chromium alloy as raw material, a large amount of dislocation defects are formed in metal powder through a ball milling process so as to facilitate the diffusion of carbon atoms in the dislocation of alloy metal in the subsequent process, the powder after ball milling is carbonized in a carbon-containing atmosphere, and a nano chromium carbide hard phase is generated in situ in the nickel-chromium alloy by controlling the concentration and the heating temperature of the carbon-containing atmosphere. The invention avoids the problem of the growth of nano crystal grains in the sintering process of the composite powder.
Description
Technical field
The present invention relates to a kind of preparation method of nano chromium carbide composite powder, belong to the preparing technical field of chromium carbide compounded powder.
Background technology
The chromium carbide sintering metal is a kind of broad-spectrum metal ceramic powder, and chromium carbide has a series of advantage: 1. antioxidant property is good; 2. hot hardness height; 3. wear resisting property excellence; 4. the coefficient of expansion is higher than other cermet materials and is approaching with steel; 5. the corrosion resistance height all has good corrosion resistance in various corrosive mediums; 6. density is low, is ceramic-metallic about half for wolfram varbide only.
In the thermospray industry, chromium carbide is usually used in preparing composite powder, is that the composite powder that raw material forms is usually used in 600～850 ℃ of wear Protection coatings under the high temperature friction environment with chromium carbide powder and NiCr alloy.Present Cr
3C
2The preparation method of-NiCr hot spray powder mainly contains hybrid system, broken sintering process, reunion sintering process, spray-drying process and direct atomization.
Hybrid system is with Cr
3C
2Directly mix with two kinds of powder of NiCr alloy; Broken sintering process is with mixed Cr
3C
2Sintering is at high temperature carried out in-NiCr compression moulding, and broken back forms powder; Agglomeration process is to utilize organic binder bond with Cr under mechanical agitation
3C
2Carry out agglomeration granulation with NiCr, obtain powder after the sintering processes.Directly atomization is to impact liquation liquid stream by high velocity air to obtain powder.
In the prior art, spray-drying process is with Cr
3C
2Be mixed into even feed liquid with NiCr powder and liquid organic solution, utilize spraying gun that feed liquid is disperseed to become fine mist then, and rapid evaporating solvent forms power-product in the heated drying medium, passes through suitable heat treatment process again, the Cr that can be used for spraying of acquisition
3C
2-NiCr composite powder.In addition, can also obtain the chromium carbide-nickel chromium composite powder of different components by the air-flow fragmentation that directly mixed molten liquid of nickel, chromium and chromium carbide atomized.
But above method all is difficult to obtain nano level chromium carbide particle, major cause is that powder mix, reunion sintering process, the required chromium carbide of spray-drying process are and add particle, if the chromium carbide powder that adds is a nano chromium carbide powder, then be easy to produce spontaneous reunion, be unfavorable for disperseing; Bond and hard good combination mutually in order to guarantee in sintering crushing method, reunion sintering process, the spray drying method for preparation process, powder need carry out the sintering heat treatment process, nano particle is easy to grow up in heat treatment process, the performance characteristics of forfeiture nano particle.Directly atomization is owing to mixed molten liquid temperature height, and the atomization process cooling slowly is difficult to obtain the chromium carbide of nanocrystal.
Summary of the invention
The present invention all is difficult to obtain nano level chromium carbide particulate problem for solving existing method, and a kind of preparation method of nano chromium carbide composite powder is provided.
The preparation method of nano chromium carbide composite powder of the present invention is as follows:
Nichrome powder is carried out ball milling be placed in the atmosphere furnace, feed the mixed gas that comprises hydrogen and carbonaceous gas, and the furnace temperature of described atmosphere furnace is remained between 650～950 ℃;
To carry out broken classification through the chromium carbide compounded powder that the insulation back obtains.
The present invention is raw material with the nichrome, form a large amount of dislocation defects by mechanical milling process in metal-powder inside, so that carbon atom spreads in the dislocation of alloyed metal in the subsequent process, powder behind the ball milling is carried out carbonization under carbon-containing atmosphere, concentration and Heating temperature by the control carbon-containing atmosphere, original position generates nano level chrome carbide hard phase in nichrome, its advantage is to have avoided the problem that nanocrystal is grown up in the composite powder sintering process, is fit to preparation nanometer grade composit powder end.
Embodiment
The invention provides following four preferred embodiments:
Embodiment 1:
Select nichrome powder, the granularity of described nichrome powder is below 75 μ m, then nichrome powder is carried out ball milling, the ball milling time as in the atmosphere furnace, fed the mixture of hydrogen and carbonaceous gas with the powder behind the ball milling more than 30 minutes in the stove, furnace temperature remains between 650～950 ℃, the insulation back obtains chromium carbide compounded powder, and the powder that obtains is carried out broken classification, obtains the finished product powder.The weight ratio of chromium is 70～80% in the described nichrome powder.The granularity of described nichrome powder is 20～45 μ m.The amount stream of described carbonaceous gas and hydrogen is than being 1: 1.2～5.Described carbonaceous gas is acetylene, methane, propane, carbon monoxide or oil gas.Described soaking time is 1～3 hour.
Embodiment 2:
Choose powder diameter below 45 μ m, the NiCr powdered alloy 1kg that contains chromium 70%, ball milling was placed in the graphite week ware in 30 minutes, placed atmosphere furnace (stove directly is 150mm) to be heated to 950 ℃, fed the gas mixture (throughput ratio of acetylene and hydrogen is 1: 4.5) of acetylene and hydrogen then, hydrogen flowing quantity is 150ml/min, be incubated after 1 hour, cooling is carried out fragmentation with powder, obtain the chromium carbide compounded powder of nickel chromium triangle of the about 70wt% of chrome carbide, the chromium carbide grain-size is in 30～80 nanometers.
Embodiment 3:
Choose powder diameter below 45 μ m, the NiCr powdered alloy 1kg that contains chromium 80%, ball milling was placed in the graphite week ware in 60 minutes, placed atmosphere furnace (stove directly is 150mm) to be heated to 650 ℃, fed the gas mixture (throughput ratio of acetylene and hydrogen is 1: 1.2) of acetylene and hydrogen then, hydrogen flowing quantity is 200ml/min, be incubated after 3 hours, cooling is carried out fragmentation with powder, obtain the chromium carbide compounded powder of nickel chromium triangle of the about 75wt% of chrome carbide, the chromium carbide grain-size is in 30～80 nanometers.
Embodiment 4:
Choose powder diameter below 45 μ m, the NiCr powdered alloy 1kg that contains chromium 80%, be placed in the graphite week ware in 120 minutes behind the ball milling, place atmosphere furnace (stove directly is 150mm) to be heated to 800 ℃, feed the gas mixture (throughput ratio of acetylene and hydrogen is 1: 2.5) of acetylene and hydrogen then, hydrogen flowing quantity is 180ml/min, be incubated after 3 hours, cooling is carried out fragmentation with powder, obtain the chromium carbide compounded powder of nickel chromium triangle of the about 75wt% of chrome carbide, the chromium carbide grain-size is in 30～80 nanometers.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (7)
1. the preparation method of a nano chromium carbide composite powder is characterized in that, comprising:
Nichrome powder is carried out ball milling be placed in the atmosphere furnace, feed the mixed gas that comprises hydrogen and carbonaceous gas, and the furnace temperature of described atmosphere furnace is remained between 650～950 ℃;
To carry out broken classification through the chromium carbide compounded powder that the insulation back obtains.
2. preparation method according to claim 1 is characterized in that, in described nichrome powder, the weight ratio that described chromium accounts for is 70～80%.
3. preparation method according to claim 1 is characterized in that, the granularity of described nichrome powder is 20～45 μ m.
4. preparation method according to claim 1 is characterized in that, the ball milling time of described nichrome powder is more than 30 minutes.
5. preparation method according to claim 1 is characterized in that, in the mixed gas of described hydrogen and carbonaceous gas, the amount of described carbonaceous gas and described hydrogen stream is than being 1: 1.2～5.
6. preparation method according to claim 1 is characterized in that, described carbonaceous gas is acetylene, methane, propane, carbon monoxide or oil gas.
7. preparation method according to claim 1 is characterized in that, the time of described insulation is 1～3 hour.
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| CN102154581B CN102154581B (en) | 2012-10-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102876951A (en) * | 2012-10-09 | 2013-01-16 | 西安交通大学 | Method for preparing pure metal ceramic Cr7C3 block |
| CN105562698A (en) * | 2014-10-17 | 2016-05-11 | 东睦新材料集团股份有限公司 | Hole sealing method for powder metallurgy chromium alloy fuel battery connecting part |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724349A (en) * | 2004-07-20 | 2006-01-25 | 中南大学 | Process for preparing nano chromium carbide powder |
| CN101003086A (en) * | 2006-11-27 | 2007-07-25 | 北京矿冶研究总院 | Cr (chromium)3C2-NiCr composite powder preparation technology |
-
2011
- 2011-03-23 CN CN201110070999A patent/CN102154581B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724349A (en) * | 2004-07-20 | 2006-01-25 | 中南大学 | Process for preparing nano chromium carbide powder |
| CN101003086A (en) * | 2006-11-27 | 2007-07-25 | 北京矿冶研究总院 | Cr (chromium)3C2-NiCr composite powder preparation technology |
Non-Patent Citations (2)
| Title |
|---|
| 《材料导报》 20100930 张雪峰等 碳热还原法制取碳化铬、金属铬的热力学分析 第108-111页 1-7 第24卷, 第9期 2 * |
| 《硬质合金》 20041231 颜练武等 超细V8C7和Cr3C2粉末的制备方法 第244-248页 1-7 第21卷, 第4期 2 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102876951A (en) * | 2012-10-09 | 2013-01-16 | 西安交通大学 | Method for preparing pure metal ceramic Cr7C3 block |
| CN102876951B (en) * | 2012-10-09 | 2014-04-23 | 西安交通大学 | Method for preparing pure metal ceramic Cr7C3 block |
| CN105562698A (en) * | 2014-10-17 | 2016-05-11 | 东睦新材料集团股份有限公司 | Hole sealing method for powder metallurgy chromium alloy fuel battery connecting part |
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| CN102154581B (en) | 2012-10-10 |
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