CN1013352B - Manufacturing technique of supper-fine molybdenum powder - Google Patents
Manufacturing technique of supper-fine molybdenum powderInfo
- Publication number
- CN1013352B CN1013352B CN 88103510 CN88103510A CN1013352B CN 1013352 B CN1013352 B CN 1013352B CN 88103510 CN88103510 CN 88103510 CN 88103510 A CN88103510 A CN 88103510A CN 1013352 B CN1013352 B CN 1013352B
- Authority
- CN
- China
- Prior art keywords
- molybdenum powder
- supper
- weight
- molybdenum
- ammonium paramolybdate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 7
- 230000002829 reductive effect Effects 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 4
- 239000011733 molybdenum Substances 0.000 abstract description 4
- 238000002485 combustion reaction Methods 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 2
- 240000005373 Panax quinquefolius Species 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The method uses ammonium paramolybdate as raw materials, a double-layer combustion boat and the low dew point of H2 to directly carry out two-stage low temperature reduction, and high performance ultrafine molybdenum powder (specific surface area achieves about 1.6m<2>/g) can be obtained. The method has the advantages of low manufacturing cost, high yield (the ratio of the weight of the ultrafine molybdenum powder and the weight of molybdenum elements is more than 95%), easy enforcement and small area occupation of workshops, and is suitable for industrial scale production.
Description
The manufacture method of ultrafine molybdenum powder belongs to the rare metal powder metallurgical technology.
Ultrafine molybdenum powder (＜0.5 μ m) manufacture method of having reported at present mainly contains three kinds, i.e. the ultra-fine MoO that hydrogen reduction molybdenum chloride steaming process, hydrogen reduction vapour deposition come out
3Powder method and plasma reduction method.Because these method cost height should not carry out industrial-scale production, so its application is restricted.In addition, also have along H
2Reduction method also can be made ultrafine molybdenum powder, but its output capacity is very low, has only about 25%, so cost is also higher, its industrial application is restricted.
The objective of the invention is for lower cost industrial-scale production ultrafine molybdenum powder, so that can produce high performance various molybdenum base and goods thereof at lower cost.Now details are as follows with present method process and performance etc.
It is that raw material is used H through two steps that the present invention adopts ammonium paramolybdate
2As reductive agent, low-temperature heat restores the molybdenum powder that mean particle size (BET nitrogen adsorption method) is less than or equal to 0.5 μ m.Wherein the ammonium paramolybdate composition is selected for use according to GB3460-82.Molybdenum content 〉=56%, Fei Shi (FiSher) mean particle size＜2.0 μ m, loose specific weight is 0.4-0.7g/cm
3
The first step reduction process: less than 2.0 μ m, loose specific weight is the 0.4-0.7 gram per centimeter with mean particle size
3Ammonium paramolybdate pack into and have in the bilevel burning boat, and the thickness of every layered material is less than 15 millimeters.With flow is 2-6m
3/ h, the H of dew point≤-30 ℃
2With burn that boat is reverse to reduce, reduction temperature 420-550 ℃ of its reduction reaction is as follows:
The volatile MoO that has just decomposited
3(420-550 ℃) has little time to volatilize, deposit, bond, grow up at low temperatures, at once by H on every side
2Stream reduces promptly:
Reduced resulting MoO through 30-120 minute
2Be the false particle of porosity and looseness, in this temperature (420-550 ℃), MoO
3Saturated vapor pressure very little, not volatile and deposition is grown up.
The second step reduction process: with the first step reductive MoO
2Pack in the above-mentioned two-layer burning boat, charging thickness is less than 15 millimeters equally.Employed H
2And flow, the flow direction and dew point be same as the first step reduction numerical value, and reduction temperature is 720-850 ℃, and recovery time 30-90 minute, its reaction was as follows:
Because MoO under this temperature (720-850 ℃)
2Saturated vapor pressure little, it is very little to volatilize, grow up, resulting product is the very frangible false particle molybdenum powder that loosens.
The present invention has overcome the shortcoming of aforesaid method, low cost of manufacture not only, and production rate height, and go up detective, floor space is little, also can utilize existing general industry molybdenum powder reduction equipment to carry out after part transforms, by this processing method, can the mass production ultrafine molybdenum powder.
The molybdenum powder productivity of Sheng Chaning (ultrafine powder weight/used molybdenum element weight) is up to more than 95% according to the method described above.Except that the operating process loss, there is not other loss.Its main physical chemical property of the molybdenum powder of Sheng Chaning is as follows according to the method described above:
Physicals:
Loose density 0.7-1.2 gram per centimeter
3
Mean particle size (BET method) 0.2-0.5 μ m
Chemical Composition (measured value):
Elementary composition % elementary composition %
Fe????0.0048????Bi????＜0.0001
Mg????0.0007????Ni????0.00025
Al????0.0012????Sn????＜0.0001
Mn????0.0006????Cu????＜0.0003
Si????0.0013????Pb????＜0.0001
V????0.0001????Ca????0.0001
Sb????0.0005????O????0.2-0.8
Ti＜0.001 molybdenum surplus
Claims (2)
1, a kind of method that is used for making (≤0.5 μ m) metal molybdenum powder is a raw material with the ammonium paramolybdate, as reductive agent, through secondary reduction, it is characterized in that the mean particle size＜2.0 μ m of ammonium paramolybdate with H2, and loose specific weight is 0.4-0.7g/cm
3H2 flow 2-6M
3/ h, dew point≤-30 ℃ reverse H2 of advancing reduce; Reduction temperature is that 420-550 ℃, time are 30-120 minute, and the secondary reduction temperature is that 720-850 ℃, time are 30-90 minute.
2, the described method of claim 1 is characterized in that using the double-deck charging thickness＜15mm that burns on boat and the every layer of burning boat.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88103510 CN1013352B (en) | 1988-06-09 | 1988-06-09 | Manufacturing technique of supper-fine molybdenum powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88103510 CN1013352B (en) | 1988-06-09 | 1988-06-09 | Manufacturing technique of supper-fine molybdenum powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1038232A CN1038232A (en) | 1989-12-27 |
| CN1013352B true CN1013352B (en) | 1991-07-31 |
Family
ID=4832634
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88103510 Expired CN1013352B (en) | 1988-06-09 | 1988-06-09 | Manufacturing technique of supper-fine molybdenum powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1013352B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3947118B2 (en) * | 2003-03-03 | 2007-07-18 | Ｊｆｅミネラル株式会社 | Surface-treated metal ultrafine powder, method for producing the same, conductive metal paste, and multilayer ceramic capacitor |
| CN100464902C (en) * | 2007-03-19 | 2009-03-04 | 江苏峰峰钨钼制品股份有限公司 | Molybdenum powder potassium impurity removal method |
| CN101200000B (en) * | 2007-12-17 | 2010-06-02 | 金堆城钼业股份有限公司 | Method for reducing molybdenum oxide by adjusting dew point of hydrogen |
| CN101966593A (en) * | 2010-11-01 | 2011-02-09 | 金堆城钼业股份有限公司 | Submicron molybdenum powder production method |
| CN114833349B (en) * | 2022-07-04 | 2023-01-31 | 成都虹波实业股份有限公司 | Method for manufacturing low-potassium large-particle-size molybdenum powder |
-
1988
- 1988-06-09 CN CN 88103510 patent/CN1013352B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN1038232A (en) | 1989-12-27 |
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Legal Events
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| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C13 | Decision | ||
| GR02 | Examined patent application | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |