CN101126137A - Method for preparing chromium-tungsten solid solution alloy material by powder pressure sintering - Google Patents
Method for preparing chromium-tungsten solid solution alloy material by powder pressure sintering Download PDFInfo
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- CN101126137A CN101126137A CNA200710018747XA CN200710018747A CN101126137A CN 101126137 A CN101126137 A CN 101126137A CN A200710018747X A CNA200710018747X A CN A200710018747XA CN 200710018747 A CN200710018747 A CN 200710018747A CN 101126137 A CN101126137 A CN 101126137A
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Abstract
The invention discloses a powder pressure melting preparation method for chromium and tungsten solid solution alloy material. The method comprises the steps as fellow: put 50 to 93 percent of tungsten powder and 7 to 50 percent of chromium powder into a mixer; add 2 to 5 percent of the total mass of the tungsten powder and the chromium powder process control agent into the mixer and fully mix in the mixer; palletize the fully mixed powder; the palletized powder is die pressed or isostatic cool pressed; the pressed blank is hot pressing sintered or hot isostatic pressing sintered after being restored in the protection of hydrogen to gain the single phase chromium and tungsten solid solution alloy material with a microstructure. The material has the advantages of fine organization, compact structure, comparative high hardness, low interception value and high voltage proof intensity.
Description
Technical field
The invention belongs to technical field of material, relate to a kind of preparation method of solid solution alloy material, be specifically related to a kind of method for preparing chromium-tungsten solid solution alloy material with powder pressure sintering.
Background technology
Pure metal tungsten has the fusing point height, and the thermal electron emission ability is strong, and characteristics such as Young's modulus height are present widely used electrode materialss.But the emission efficiency of pure metal tungsten electrode is not high, and shut off value is too high, to there being disadvantageous effect in work-ing life of electrical equipment.Chromium-tungsten solid solution alloy material has the hardness height, proof voltage intensity height, and the advantage that shut off value is low is one of electrode materials that substitutes pure tungsten.
Because the fusing point of tungsten is 3407 ℃, the fusing point of chromium is 1857 ℃, and under existing appointed condition, it is impossible adopting conventional metallurgical method to prepare stellite.On the other hand, the method for ordinary sinter can be prepared the chromium tungstenalloy, but the porosity of material is too high, can't satisfy the service requirements of electrode materials.
Summary of the invention
The object of the present invention is to provide a kind ofly to prepare the method for chromium-tungsten solid solution alloy material with powder pressure sintering, this method can obtain single-phase chromium-tungsten solid solution tissue, and alloy material has the characteristics of high rigidity, low shut off value and high withstand voltage intensity.
The technical solution adopted in the present invention is, a kind of method of preparing chromium-tungsten solid solution alloy material by powder pressure sintering, the microstructure of this material are single-phase chromium-tungsten solid solution, and this method is carried out according to the following steps,
A. choosing particle diameter is 6～10 μ m, and purity is greater than 99.9%, and oxygen level is the tungsten powder of 500～800ppm; Choosing particle diameter is 45～100 μ m, and purity is greater than 99.9%, and oxygen level is the chromium powder of 800～1500ppm, puts into mixer in quality than the ratio of tungsten powder 50%～93%, chromium powder 7%～50%;
B. press 2～5% of tungsten powder, chromium powder total mass and add process control agents in the tungsten powder of mixer, chromium powder, mixed in mixer 3.5～5 hours, described process control agent is the easy volatile organic solvent;
C. will go up the powder granulation that the step mixes;
D. the powder after will granulating carries out mold pressing or isostatic cool pressing, and pressure is not less than 50MPa, the blank compacting of trying one's best;
E. with the blank that suppresses in 900 ℃～980 ℃ reduction under the hydrogen shield after 50～90 minutes, 1450 ℃～1600 ℃ hot pressed sinterings or HIP sintering 2～4 hours are promptly made chromium-tungsten solid solution alloy material.
Characteristics of the present invention also are,
Process control agent wherein is dehydrated alcohol or acetone.
Among the step e wherein, the heat-up rate that is warming up to 900 ℃～980 ℃ is smaller or equal to 10 ℃/minute, and the heat-up rate that is warming up to 1450 ℃～1600 ℃ is smaller or equal to 25 ℃/minute.
Among the step e, the pressure of hot pressing or HIP sintering is at least 30Mpa.
Among the step e, the atmosphere of hot pressing or hot isostatic pressing is that hydrogen or vacuum tightness are at least 10
-3The vacuum atmosphere of MPa.
The inventive method is simple to operate, can prepare the material that microstructure is single-phase chromium-tungsten solid solution, and this material structure is tiny, and compact structure has high hardness, low shut off value and very high proof voltage intensity.
Embodiment
The present invention is described in detail below in conjunction with specific examples.
The present invention utilizes tungsten, chromium can form the characteristics of sosoloid, by becoming the control of component selections and manufacturing process, obtains chromium-tungsten solid solution single phase structure, the performance that the chromium-tungsten solid solution alloy material that the inventive method obtains can reach such as following table 1.
The salient features of table 1 chromium tungsten alloy material
| Density % | Hardness HB | Density g/cm 3 | Air content ppm | Shut off value A | Proof voltage intensity V/m | |
| O 2 | N 2 | |||||
| ＞96 | ＞400 | 12.5～18 | 80～300 | ＜20 | ＜2.30 | ～10 8 |
Specific examples is as follows:
Embodiment 1
1. choosing the tungsten powder median size is 5 μ m, and purity is greater than 99.9%, and oxygen level is 500ppm; Chromium powder size distribution 55 μ m, purity is greater than 99.9%, and oxygen level is 800ppm;
2. above-mentioned tungsten powder 93%, chromium powder 7% are prepared in proportion, in mixer, pressed 2% of tungsten powder, chromium powder total mass and add dehydrated alcohol, mixed system 3.5 hours;
3. the powder that mixes is granulated;
4. the powder after will granulating carries out mold pressing, and pressure is 60MPa;
With the blank that suppresses being warming up to 900 ℃ of reduction under the hydrogen shield after 90 minutes, continued to be warming up to 1450 ℃ of hot pressed sinterings 4 hours, pressure is 35MPa; The above-mentioned heat-up rate that is warming up to 900 ℃ is 10 ℃/minute, and 900 ℃～1450 ℃ heat-up rate is 15 ℃/minute.
The performance of the chromium-tungsten solid solution alloy material that obtains such as following table 2.
The salient features of table 2 chromium 7%-tungsten 93% chromium tungsten alloy material
| Density % | Hardness HB | Density g/cm 3 | Air content ppm | Shut off value A | Proof voltage intensity * 10 8V/m | |
| O 2 | N 2 | |||||
| 98.6 | 408 | 17.8 | 263 | 11 | 2.25 | 0.98 |
Embodiment 2
1. choosing the tungsten powder median size is 7 μ m, and purity is greater than 99.9%, and oxygen level is 800ppm; Chromium powder size distribution 55 μ m, purity is greater than 99.9%, and oxygen level is 1500ppm;
2. above-mentioned tungsten powder 50%, chromium powder 50% are prepared in proportion, in mixer, pressed 5% of tungsten powder, chromium powder total mass and add acetone, mixed system 5 hours;
3. the powder that mixes is granulated;
4. the powder after will granulating carries out isostatic cool pressing, and pressure is 80MPa;
With the blank that suppresses being warming up to 980 ℃ of reduction under the hydrogen shield after 60 minutes, vacuumize, vacuum tightness is greater than 10
-3MPa continued to be warming up to 1550 ℃ of HIP sintering 2.5 hours, and pressure is 30MPa; The above-mentioned heat-up rate that is warming up to 900 ℃ is 8 ℃/minute, and 900 ℃～1450 ℃ heat-up rate is 25 ℃/minute.
The performance of the chromium-tungsten solid solution alloy material that obtains such as following table 3.
The salient features of table 3 chromium 50%-tungsten 50% chromium tungsten alloy material
| Density % | Hardness HB | Density g/cm 3 | Air content ppm | Shut off value A | Proof voltage intensity * 10 8V/m | |
| O 2 | N 2 | |||||
| 96.5 | 465 | 12.5 | 55 | 16 | 1.8 | 1.01 |
Embodiment 3
1. choosing the tungsten powder median size is 9 μ m, and purity is greater than 99.9%, and oxygen level is 600ppm; Chromium powder size distribution 90 μ m, purity is greater than 99.9%, and oxygen level is 800ppm;
2. above-mentioned tungsten powder 33%, chromium powder 67% are prepared in proportion, in mixer, pressed 4% of tungsten powder, chromium powder total mass and add dehydrated alcohol, mixed system 4 hours;
3. the powder that mixes is granulated;
4. the powder after will granulating carries out mold pressing, and pressure is 60MPa;
With the blank that suppresses being warming up to 950 ℃ of reduction under the hydrogen shield after 80 minutes, continued to be warming up to 1600 ℃ of HIP sintering 3 hours, pressure is 38MPa; The above-mentioned heat-up rate that is warming up to 900 ℃ is 7 ℃/minute, and 900 ℃～1450 ℃ heat-up rate is 20 ℃/minute.
The performance of the chromium-tungsten solid solution alloy material that obtains such as following table 4.
The salient features of table 4 chromium 33%-tungsten 67% chromium tungsten alloy material
| Density % | Hardness HB | Density g/cm 3 | Air content ppm | Shut off value A | Proof voltage intensity * 10 8V/m | |
| O 2 | N 2 | |||||
| 97.2 | 433 | 14.6 | 289 | 6 | 2.03 | 1.02 |
Embodiment 4
1. choosing the tungsten powder median size is 6 μ m, and purity is greater than 99.9%, and oxygen level is 700ppm; Chromium powder size distribution 55 μ m, purity is greater than 99.9%, and oxygen level is 800ppm;
2. above-mentioned tungsten powder 75%, chromium powder 25% are prepared in proportion, in mixer, pressed 3% of tungsten powder, chromium powder total mass and add acetone, mixed system 4.5 hours;
3. the powder that mixes is granulated;
4. the powder after will granulating carries out isostatic cool pressing, and pressure is 75MPa;
With the blank that suppresses being warming up to 980 ℃ of reduction under the hydrogen shield after 70 minutes, vacuumize, vacuum tightness is greater than 10
-3MPa continued to be warming up to 1500 ℃ of HIP sintering 3 hours, and pressure is 45MPa; The above-mentioned heat-up rate that is warming up to 900 ℃ is 6 ℃/minute, and 900 ℃～1450 ℃ heat-up rate is 20 ℃/minute.
The performance of the chromium-tungsten solid solution alloy material that obtains such as following table 5.
The salient features of table 5 chromium 25%-tungsten 75% chromium tungsten alloy material
| Density % | Hardness HB | Density g/cm 3 | Air content ppm | Shut off value A | Proof voltage intensity * 10 8V/m | |
| O 2 | N 2 | |||||
| 97.6 | 429 | 15.8 | 186 | 14 | 2.1 | 1.01 |
Claims (5)
1. the method for a preparing chromium-tungsten solid solution alloy material by powder pressure sintering is characterized in that, the microstructure of this material is single-phase chromium-tungsten solid solution, and this method is carried out according to the following steps,
A. choosing particle diameter is 6～10 μ m, and purity is greater than 99.9%, and oxygen level is the tungsten powder of 500～800ppm; Choosing particle diameter is 45～100 μ m, and purity is greater than 99.9%, and oxygen level is the chromium powder of 800～1500ppm, puts into mixer in quality than the ratio of tungsten powder 50%～93%, chromium powder 7%～50%;
B. press 2～5% of tungsten powder, chromium powder total mass and add process control agents in the tungsten powder of mixer, chromium powder, mixed in mixer 3.5～5 hours, described process control agent is the easy volatile organic solvent;
C. will go up the powder granulation that the step mixes;
D. the powder after will granulating carries out mold pressing or isostatic cool pressing, and pressure is not less than 50MPa, the blank compacting of trying one's best;
E. with the blank that suppresses in 900 ℃～980 ℃ reduction under the hydrogen shield after 50～90 minutes, 1450 ℃～1600 ℃ hot pressed sinterings or HIP sintering 2～4 hours are promptly made chromium-tungsten solid solution alloy material.
2. in accordance with the method for claim 1, it is characterized in that described process control agent is dehydrated alcohol or acetone.
3. in accordance with the method for claim 1, it is characterized in that among the described step e, the heat-up rate that is warming up to 900 ℃～980 ℃ is smaller or equal to 10 ℃/minute, the heat-up rate that is warming up to 1450 ℃～1600 ℃ is smaller or equal to 25 ℃/minute.
4. in accordance with the method for claim 1, it is characterized in that among the described step e, the pressure of hot pressing or HIP sintering is at least 30Mpa.
5. in accordance with the method for claim 1, it is characterized in that among the described step e, the atmosphere of hot pressing or hot isostatic pressing is that hydrogen or vacuum tightness are at least 10
-3The vacuum atmosphere of MPa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101170A (en) * | 2010-12-28 | 2011-06-22 | 株洲硬质合金集团有限公司 | Method for producing tungsten bar for calendering |
| CN102416475A (en) * | 2011-11-24 | 2012-04-18 | 西安瑞福莱钨钼有限公司 | Method for preparing nuclear functional material tungsten-tantalum alloy plate |
| CN102513789A (en) * | 2011-12-21 | 2012-06-27 | 宁波江丰电子材料有限公司 | Manufacturing method of tungsten target material |
| CN105345007A (en) * | 2014-08-15 | 2016-02-24 | 安泰科技股份有限公司 | Preparation method for highly dense chromium-tungsten alloy target |
| CN105364074A (en) * | 2014-08-15 | 2016-03-02 | 安泰科技股份有限公司 | Preparation method for high-compactness chromium-tungsten alloy target material |
| CN107299269A (en) * | 2017-06-12 | 2017-10-27 | 合肥工业大学 | A kind of W Cr Al composites of resistance to high temperature oxidation and preparation method thereof |
| CN113445042A (en) * | 2020-03-27 | 2021-09-28 | 中国工程物理研究院材料研究所 | Low-activation steel substrate-based tungsten-chromium alloy coating and preparation method thereof |
-
2007
- 2007-09-26 CN CNB200710018747XA patent/CN100503853C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101170A (en) * | 2010-12-28 | 2011-06-22 | 株洲硬质合金集团有限公司 | Method for producing tungsten bar for calendering |
| CN102416475A (en) * | 2011-11-24 | 2012-04-18 | 西安瑞福莱钨钼有限公司 | Method for preparing nuclear functional material tungsten-tantalum alloy plate |
| CN102513789A (en) * | 2011-12-21 | 2012-06-27 | 宁波江丰电子材料有限公司 | Manufacturing method of tungsten target material |
| CN102513789B (en) * | 2011-12-21 | 2014-04-09 | 宁波江丰电子材料有限公司 | Manufacturing method of tungsten target material |
| CN105345007A (en) * | 2014-08-15 | 2016-02-24 | 安泰科技股份有限公司 | Preparation method for highly dense chromium-tungsten alloy target |
| CN105364074A (en) * | 2014-08-15 | 2016-03-02 | 安泰科技股份有限公司 | Preparation method for high-compactness chromium-tungsten alloy target material |
| CN107299269A (en) * | 2017-06-12 | 2017-10-27 | 合肥工业大学 | A kind of W Cr Al composites of resistance to high temperature oxidation and preparation method thereof |
| CN107299269B (en) * | 2017-06-12 | 2019-01-11 | 合肥工业大学 | A kind of W-Cr-Al composite material and preparation method of resistance to high temperature oxidation |
| CN113445042A (en) * | 2020-03-27 | 2021-09-28 | 中国工程物理研究院材料研究所 | Low-activation steel substrate-based tungsten-chromium alloy coating and preparation method thereof |
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| CN100503853C (en) | 2009-06-24 |
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