CN109249015B - Preparation method of rare earth molybdenum alloy mixed powder - Google Patents
Preparation method of rare earth molybdenum alloy mixed powder Download PDFInfo
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- CN109249015B CN109249015B CN201811420779.7A CN201811420779A CN109249015B CN 109249015 B CN109249015 B CN 109249015B CN 201811420779 A CN201811420779 A CN 201811420779A CN 109249015 B CN109249015 B CN 109249015B
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- 229910001182 Mo alloy Inorganic materials 0.000 title claims abstract description 41
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 35
- 239000011812 mixed powder Substances 0.000 title claims abstract description 34
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 38
- 239000011268 mixed slurry Substances 0.000 claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 24
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 9
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 10
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 5
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 claims description 3
- 229910000457 iridium oxide Inorganic materials 0.000 claims description 3
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 claims description 3
- 229910003452 thorium oxide Inorganic materials 0.000 claims description 3
- 239000002002 slurry Substances 0.000 abstract description 9
- 239000007787 solid Substances 0.000 abstract description 7
- 238000005204 segregation Methods 0.000 abstract description 6
- 239000000428 dust Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 2
- -1 rare earth nitrate Chemical class 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- GVZGGVWONIKLCN-UHFFFAOYSA-N [Mo]=O.[Ir] Chemical compound [Mo]=O.[Ir] GVZGGVWONIKLCN-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- DMOXXSIMUDQRTG-UHFFFAOYSA-N molybdenum thorium Chemical compound [Mo][Th] DMOXXSIMUDQRTG-UHFFFAOYSA-N 0.000 description 1
- 238000009856 non-ferrous metallurgy Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- B22F1/0003—
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of rare earth molybdenum alloy mixed powder, which comprises the following steps: firstly, adding rare earth oxide powder with the average Fisher particle size of not more than 3.0 mu m into ethanol with the volume purity of more than 95 percent, and uniformly mixing to obtain mixed slurry A; secondly, uniformly mixing the mixed slurry A with molybdenum powder with the average Fisher particle size of 1.6-5.0 mu m to obtain mixed slurry B; and thirdly, carrying out vacuum drying on the mixed slurry B to obtain rare earth molybdenum alloy mixed powder. According to the invention, the rare earth oxide powder and ethanol are mixed into slurry, and then the slurry is mixed with the molybdenum powder to obtain the rare earth molybdenum alloy mixed powder through drying, so that the problems of dust pollution and component segregation in the process of preparing the rare earth molybdenum alloy mixed powder through solid-solid doping are solved, and the distribution uniformity of the rare earth oxide powder in the rare earth molybdenum alloy mixed powder is improved.
Description
Technical Field
The invention belongs to the technical field of molybdenum alloy powder preparation, and particularly relates to a preparation method of rare earth molybdenum alloy mixed powder.
Background
Molybdenum is a refractory metal with high boiling point and high melting point, and has wide application in the fields of steel industry, nonferrous metallurgy, electronics, electric light sources, chemical industry, agriculture and the like. With the continuous progress of science and technology, the application field of molybdenum is continuously expanded. Rare earth molybdenum alloy can be obtained by adding a small amount of rare earth oxides (0.2 wt% -2 wt%) such as lanthanum oxide, cerium oxide and the like into molybdenum alloy, and compared with common molybdenum alloy, the high-temperature mechanical property and the recrystallization property of the rare earth molybdenum alloy are greatly improved.
Various published data show that the main methods for preparing the rare earth molybdenum alloy doped powder are as follows: (1) solid-solid doping, namely adopting molybdenum oxide or molybdenum powder, uniformly mixing with rare earth oxide powder, sieving or reducing to obtain doped alloy powder; (2) solid-liquid doping, wherein molybdenum oxide and rare earth nitrate solution are adopted, and doped powder is obtained by reduction after drying, which is a main method for batch production at present; (3) liquid-liquid doping, namely, adding a rare earth nitrate solution into an ammonium molybdate solution by adopting a hydrometallurgy method, crystallizing by adopting acid precipitation to obtain a eutectic, and then reducing to obtain molybdenum alloy powder. Among the above methods, the conventional solid-solid doping method is widely used, but the method has disadvantages that the rare earth oxide powder is liable to form floating dust and contamination during the mixing and sieving processes, and segregation is liable to form in the mixed powder components, resulting in non-uniformity of alloy components. This is one of the main reasons that practically restrict the application of the solid-solid doping method.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of rare earth molybdenum alloy mixed powder aiming at the defects of the prior art. According to the method, the rare earth oxide powder and ethanol are mixed into slurry, and then the slurry and the molybdenum powder are mixed into slurry and dried to obtain the rare earth molybdenum alloy mixed powder, so that the problems of dust pollution and component segregation in the process of preparing the rare earth molybdenum alloy mixed powder by solid-solid doping are solved, and the distribution uniformity of the rare earth oxide powder in the rare earth molybdenum alloy mixed powder is improved.
In order to solve the technical problems, the invention adopts the technical scheme that: the preparation method of the rare earth molybdenum alloy mixed powder is characterized by comprising the following steps of:
step one, adding rare earth oxide powder with average Fisher size not more than 3.0 mu m into ethanol with volume purity more than 95 percent, and uniformly mixing to obtain mixed slurry A; the mass of the rare earth oxide powder added into each 1000mL of ethanol is not more than 143 g;
step two, uniformly mixing the mixed slurry A obtained in the step one with molybdenum powder with the average Fisher particle size of 1.6-5.0 μm to obtain mixed slurry B;
step three, carrying out vacuum drying on the mixed slurry B obtained in the step two to obtain rare earth molybdenum alloy mixed powder; the pressure of the vacuum drying is 200 Pa-1000 Pa, and the temperature is 40-65 ℃; the mass content of the rare earth oxide in the rare earth molybdenum alloy mixed powder is 0.5-2%.
The rare earth oxide powder and the molybdenum powder are mixed uniformly to prepare the slurry, the slurry and the molybdenum powder are mixed uniformly, and then the rare earth molybdenum alloy mixed powder is obtained through vacuum drying, so that the problems of dust pollution and component segregation in the process of preparing the rare earth molybdenum alloy mixed powder by solid-solid doping are solved, the distribution uniformity of the rare earth oxide powder in the rare earth molybdenum alloy mixed powder is improved, the average Fisher particle size of the commonly used molybdenum powder is enlarged from 3.0-5.0 mu m to 1.6-5.0 mu m, the use variety of the molybdenum powder raw material is enlarged, and the application range of the preparation method is enlarged.
The preparation method of the rare earth molybdenum alloy mixed powder is characterized in that in the first step, the rare earth oxide powder is lanthanum oxide powder, cerium oxide powder, iridium oxide powder or thorium oxide powder. The common rare earth oxide powder can be used as a raw material for preparing the rare earth molybdenum alloy, so that the practicability of the preparation method is improved, and the popularization and the use of the method are facilitated.
The preparation method of the rare earth molybdenum alloy mixed powder is characterized in that the ratio of the volume of the mixed slurry A to the mass of the molybdenum powder in the step two is 1: (5-7), the volume unit is mL, and the mass unit is g. By further limiting the volume of the mixed slurry A and the mass of the molybdenum powder, the rare earth oxide powder and the molybdenum powder in the mixed slurry B achieve a better ratio, the mixing uniformity of the rare earth oxide powder and the molybdenum powder in the mixed slurry B is improved, and the component segregation in the finally prepared rare earth molybdenum alloy mixed powder is further reduced.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the rare earth oxide powder and ethanol are mixed into slurry, and then the slurry is mixed with the molybdenum powder to obtain the rare earth molybdenum alloy mixed powder through drying, so that the problems of dust pollution and component segregation in the process of preparing the rare earth molybdenum alloy mixed powder through solid-solid doping are solved, and the distribution uniformity of the rare earth oxide powder in the rare earth molybdenum alloy mixed powder is improved.
2. The preparation method is simple, has low requirements on raw materials, is easy to obtain, has easy control of production process, is simple, convenient, safe and reliable to operate, and is suitable for large-scale production.
3. The rare earth oxide powder in the rare earth molybdenum alloy mixed powder has rich source types, and the preparation method has wider application range.
The technical solution of the present invention is further described in detail by examples below.
Detailed Description
Example 1
The preparation method of this example includes the following steps:
step one, 140g of lanthanum oxide powder with the average Fisher size of 3.0 mu m is added into 978mL of ethanol with the volume purity of 96% and is uniformly mixed to obtain mixed slurry A;
step two, uniformly mixing the mixed slurry A obtained in the step one with 6860g of molybdenum powder with the average Fisher size of 5.0 mu m to obtain mixed slurry B;
and step three, carrying out vacuum drying on the mixed slurry B obtained in the step two under the conditions that the pressure is 200Pa and the temperature is 40 ℃ to obtain lanthanum oxide and molybdenum alloy mixed powder.
Example 2
The preparation method of this example includes the following steps:
step one, adding 60g of cerium oxide powder with the average Fisher size of 2.0 mu m into 992mL of ethanol with the volume purity of 98 percent, and uniformly mixing to obtain mixed slurry A;
step two, uniformly mixing the mixed slurry A obtained in the step one with 5940g of molybdenum powder with the average Fisher particle size of 1.6 mu m to obtain mixed slurry B;
and step three, carrying out vacuum drying on the mixed slurry B obtained in the step two under the conditions that the pressure is 600Pa and the temperature is 50 ℃ to obtain cerium oxide and molybdenum alloy mixed powder.
Example 3
The preparation method of this example includes the following steps:
step one, adding 50g of thorium oxide powder with the average Fisher particle size of 0.2 mu m into 1995mL of ethanol with the volume purity of 99 percent, and uniformly mixing to obtain mixed slurry A;
step two, uniformly mixing the mixed slurry A obtained in the step one with 9950g of molybdenum powder with the average Fisher particle size of 3.0 mu m to obtain mixed slurry B;
and step three, carrying out vacuum drying on the mixed slurry B obtained in the step two under the conditions that the pressure is 1000Pa and the temperature is 65 ℃ to obtain thorium-molybdenum alloy mixed powder.
Example 4
The preparation method of this example includes the following steps:
step one, 91.37g of iridium oxide powder with the average Fisher size of 0.5 mu m is added into 982mL of ethanol with the volume purity of 99 percent and is uniformly mixed to obtain mixed slurry A;
step two, uniformly mixing the mixed slurry A obtained in the step one with 6000g of molybdenum powder with the average Fisher particle size of 4.0 mu m to obtain mixed slurry B;
and step three, carrying out vacuum drying on the mixed slurry B obtained in the step two under the conditions that the pressure is 800Pa and the temperature is 55 ℃ to obtain iridium oxide molybdenum alloy mixed powder.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (2)
1. The preparation method of the rare earth molybdenum alloy mixed powder is characterized by comprising the following steps of:
step one, adding rare earth oxide powder with average Fisher size not more than 3.0 mu m into ethanol with volume purity more than 95 percent, and uniformly mixing to obtain mixed slurry A; the mass of the rare earth oxide powder added into each 1000mL of ethanol is not more than 143 g; the rare earth oxide powder is lanthanum oxide powder, cerium oxide powder, iridium oxide powder or thorium oxide powder;
step two, uniformly mixing the mixed slurry A obtained in the step one with molybdenum powder with the average Fisher particle size of 1.6-5.0 μm to obtain mixed slurry B;
step three, carrying out vacuum drying on the mixed slurry B obtained in the step two to obtain rare earth molybdenum alloy mixed powder; the pressure of the vacuum drying is 200 Pa-1000 Pa, and the temperature is 40-65 ℃; the mass content of the rare earth oxide in the rare earth molybdenum alloy mixed powder is 0.5-2%.
2. The method for preparing a rare earth molybdenum alloy mixed powder as claimed in claim 1, wherein the ratio of the volume of the mixed slurry A to the mass of the molybdenum powder in the second step is 1: (5-7), the volume unit is mL, and the mass unit is g.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234430A (en) * | 2008-02-22 | 2008-08-06 | 中南大学 | Method for preparing ultrafine molybdenum powder and ultrafine molybdenum powder doped with rare earth |
| CN102534334A (en) * | 2012-02-21 | 2012-07-04 | 西安建筑科技大学 | High-strength and high-toughness molybdenum alloy and preparation method thereof |
| CN102839309A (en) * | 2012-08-16 | 2012-12-26 | 西安建筑科技大学 | Mixing method for preparing high-strength high-tenacity molybdenum alloy |
| CN103276266A (en) * | 2013-06-08 | 2013-09-04 | 金堆城钼业股份有限公司 | Method for preparing TZM alloy material through spray drying |
| CN103706802A (en) * | 2013-12-18 | 2014-04-09 | 金堆城钼业股份有限公司 | Method for preparing lanthanum-doped alloy molybdenum powder |
| CN108149112A (en) * | 2017-12-04 | 2018-06-12 | 株洲夏普高新材料有限公司 | Cermet containing rare earth element y and preparation method thereof |
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2018
- 2018-11-27 CN CN201811420779.7A patent/CN109249015B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234430A (en) * | 2008-02-22 | 2008-08-06 | 中南大学 | Method for preparing ultrafine molybdenum powder and ultrafine molybdenum powder doped with rare earth |
| CN102534334A (en) * | 2012-02-21 | 2012-07-04 | 西安建筑科技大学 | High-strength and high-toughness molybdenum alloy and preparation method thereof |
| CN102839309A (en) * | 2012-08-16 | 2012-12-26 | 西安建筑科技大学 | Mixing method for preparing high-strength high-tenacity molybdenum alloy |
| CN103276266A (en) * | 2013-06-08 | 2013-09-04 | 金堆城钼业股份有限公司 | Method for preparing TZM alloy material through spray drying |
| CN103706802A (en) * | 2013-12-18 | 2014-04-09 | 金堆城钼业股份有限公司 | Method for preparing lanthanum-doped alloy molybdenum powder |
| CN108149112A (en) * | 2017-12-04 | 2018-06-12 | 株洲夏普高新材料有限公司 | Cermet containing rare earth element y and preparation method thereof |
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