CN101249567A - Preparation method of nano-scale molybdenum powder - Google Patents
Preparation method of nano-scale molybdenum powder Download PDFInfo
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- CN101249567A CN101249567A CNA2008101038833A CN200810103883A CN101249567A CN 101249567 A CN101249567 A CN 101249567A CN A2008101038833 A CNA2008101038833 A CN A2008101038833A CN 200810103883 A CN200810103883 A CN 200810103883A CN 101249567 A CN101249567 A CN 101249567A
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- molybdenum powder
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Abstract
The invention relates to a preparation method of nano-scale molybdenum powder, which belongs to the field of refractory molybdenum powder preparation technology, in particular to the preparation method of nano-scale molybdenum powder suitable for production of nano-scale molybdenum powder. The method comprises the following steps of: selecting commercial ammonium molybdate as the raw material; preparing ammonium molybdate solution of certain concentration; adding strong acid; stirring to obtain white gel; baking the gel at 100 to 300 DEG C for 1 to 3 h in an oven to obtain a precursor; and reducing in a tubular furnace in the presence of hydrogen as reducing gas at 600 to 800 DEG C for 0.5 to 2 h to obtain the nano-scale molybdenum powder.
Description
Technical field
The invention belongs to the preparing technical field of refractory metal molybdenum powder, particularly a kind of preparation method of nano-scale molybdenum powder is adapted to the production of nanometer molybdenum powder.
Background technology
Molybdenum and alloy thereof have very high elevated temperature strength and high temperature hardness, and therefore good heat conduction, electric conductivity and good features such as corrosion resistance are widely used in fields such as chemical, metallurgy and Aero-Space.In recent years, along with the develop rapidly of new and high technology, high-tech has exceeded traditional performance indications in many aspects to molybdenum and alloy material performance requirement thereof, and therefore, modern molybdenum product technology of preparing had both faced the challenge and also welcome opportunity.Wherein, the preparation of molybdenum powder is the primary link of development molybdenum industry technology.At present, the preparation of molybdenum powder is comparative maturity, but still needs further development, perfect, is still waiting to solve in particular for the technology of preparing of the molybdenum powder that satisfies some specific uses.
The traditional preparation process of molybdenum powder is to be different from the preparation of specializing in ultrafine molybdenum powder, nanometer molybdenum powder.Common traditional preparation process method has: reducing process, hydroxyl thermal decomposition method, molybdenum chloride steaming process and molybdenum chloride pyrolysismethod.The method of traditional preparation process molybdenum powder is because preparation technology's cycle is long, temperature is high, and molybdenum powder is easily grown up in this process, can not get ultrafine molybdenum powder usually.The method for preparing ultrafine molybdenum powder mainly contains: the steaming process of molybdenum chloride, evaporation attitude molybdenum trioxide reducing process, plasma reduction method and activation reduction method.At present, the nanometer preparation method of molybdenum of report mainly contains: microwave plasma method, pulse electro discharge prepare nanometer molybdenum powder etc.Usually these method energy consumptions that prepare the nanometer molybdenum powder are big, and the cost height is unsuitable for a large amount of production nano-scale molybdenum powders.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano-scale molybdenum powder, promptly adopt gel method to prepare presoma, after the low temperature hydrogen reduction is to obtain nano-scale molybdenum powder.
Preparation technology of the present invention is:
Adopting the commodity ammonium molybdate is raw material, is made into certain density ammonium molybdate solution, injects strong acid, stirs, and obtains white gels; Described white gels is placed baking oven, dried by the fire 1～3 hour under 100 ℃～300 ℃ temperature, make presoma, then described presoma is added thermal reduction in tube furnace, the recovery time is 0.5～2 hour, and reduction temperature is 600 ℃～800 ℃.
Another scheme of the present invention is: at above-mentioned ammonium molybdate solution, before injecting strong acid, add a little organic acid and ammonium salt, stir and make it dissolving.
Another scheme of the present invention is: above-mentioned strong acid comprises hydrochloric acid, nitric acid or chloroazotic acid.
Another scheme of the present invention is: when adding the described presoma of thermal reduction, use hydrogen as protective gas.
The benefit of this method is that equipment is simple, and is easy to operate, can significantly reduce production costs, and helps producing in a large number nano-scale molybdenum powder.
The invention has the advantages that:
(1) equipment is simple, small investment;
(2) raw material easily obtain, and the presoma course of reaction is simple and easy to control;
(3) reaction intermediate is gas, volatile or labile material, can do recycling, avoids forming environmental pollution.
Description of drawings
Accompanying drawing 1 is the field emission electromicroscopic photograph of the nano-scale molybdenum powder of embodiment 2.
Accompanying drawing 2 is the field emission electromicroscopic photograph of the nano-scale molybdenum powder of embodiment 3.
Accompanying drawing 3 is the field emission electromicroscopic photograph of the nano-scale molybdenum powder of embodiment 4.
The specific embodiment
Embodiment 1:
Take by weighing the commodity ammonium molybdate, add deionized water, compound concentration is the 0.80mol/L ammonium molybdate solution.Measure the 20ml ammonium molybdate solution and put into beaker, slowly add 5ml red fuming nitric acid (RFNA) on one side, stir on one side, in whipping process, generate white gels; Get gel and place baking oven, 100 ℃ of oven temperatures dried by the fire 3 hours; Reduce in tube furnace then, hydrogen is as reducing gas, at 600 ℃ of reductase 12s hour, takes out then, obtains nano level molybdenum powder.
Embodiment 2:
Take by weighing the commodity ammonium molybdate, add deionized water, compound concentration is the 0.80mol/L ammonium molybdate solution.Measure the 20ml ammonium molybdate solution and put into beaker, slowly add 5ml red fuming nitric acid (RFNA) on one side, stir on one side, in whipping process, generate white gels; Get gel and place baking oven, 100 ℃ of oven temperatures dried by the fire 2 hours; Reduce in tube furnace then, hydrogen, takes out 650 ℃ of reduction 1.5 hours then as reducing gas, obtains nano level molybdenum powder, as Fig. 1.
Embodiment 3:
Take by weighing the commodity ammonium molybdate, add deionized water, compound concentration is the 1.60mol/L ammonium molybdate solution.Measure the 20ml ammonium molybdate solution and put into beaker, add 4 gram oxalic acid, stir and make it dissolving, slowly add the 10ml chloroazotic acid then on one side, stir on one side, white gels in whipping process, generated; Get gel and place baking oven, 200 ℃ of oven temperatures dried by the fire 1 hour; Reduce in tube furnace then, hydrogen, takes out 700 ℃ of reduction 1.5 hours then as reducing gas, obtains nano level molybdenum powder, as Fig. 2.
Embodiment 4:
Take by weighing the commodity ammonium molybdate, add deionized water, compound concentration is the 2.40mol/L ammonium molybdate solution.Measure the 20ml ammonium molybdate solution, add in the beaker, add 4 gram oxalic acid and 2 gram ammonium nitrate, stir and make it dissolving, slowly add the 10ml red fuming nitric acid (RFNA) then on one side, stir on one side, white gels in whipping process, generated; Get gel and place baking oven, 250 ℃ of oven temperatures dried by the fire 1 hour; Reduce in tube furnace then, hydrogen, takes out 750 ℃ of reduction 1 hour then as reducing gas, obtains nano level molybdenum powder, as Fig. 3.
Embodiment 5:
Take by weighing the commodity ammonium molybdate, add deionized water, compound concentration is the 2.40mol/L ammonium molybdate solution.Measure the 20ml ammonium molybdate solution, add in the beaker, add 4 gram oxalic acid and 2 gram ammonium nitrate, stir and make it dissolving, slowly add the 10ml red fuming nitric acid (RFNA) then on one side, stir on one side, white gels in whipping process, generated; Get gel and place baking oven, 300 ℃ of oven temperatures dried by the fire 1 hour; Reduce in tube furnace then, hydrogen, takes out 800 ℃ of reduction 0.5 hour then as reducing gas, obtains nano level molybdenum powder.
Claims (4)
1, a kind of preparation method of nano-scale molybdenum powder is characterized in that: adopting the commodity ammonium molybdate is raw material, is made into certain density ammonium molybdate solution, injects strong acid, stirs, and obtains white gels; Described white gels is placed baking oven, dried by the fire 1～3 hour under 100 ℃～300 ℃ temperature, make presoma, described presoma being added the thermal reduction recovery time then in tube furnace is 0.5～2 hour, and reduction temperature is 600 ℃～800 ℃.
2, the preparation method of a kind of nano-scale molybdenum powder as claimed in claim 1 is characterized in that: described ammonium molybdate solution, before injecting strong acid, add organic acid and ammonium salt, and stir and make it dissolving.
3, the preparation method of a kind of nano-scale molybdenum powder as claimed in claim 1 or 2 is characterized in that: described strong acid comprises hydrochloric acid, nitric acid or chloroazotic acid.
4, the preparation method of a kind of nano-scale molybdenum powder as claimed in claim 1 or 2 is characterized in that: when adding the described presoma of thermal reduction, with hydrogen as protective gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008101038833A CN101249567A (en) | 2008-04-11 | 2008-04-11 | Preparation method of nano-scale molybdenum powder |
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| CNA2008101038833A CN101249567A (en) | 2008-04-11 | 2008-04-11 | Preparation method of nano-scale molybdenum powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353264B (en) * | 2008-09-26 | 2010-04-21 | 北京科技大学 | Method for improving ceramic metallized layer microstructure |
| CN103252506A (en) * | 2013-05-14 | 2013-08-21 | 厦门理工学院 | Preparation method of nanometer molybdenum powder containing homodisperse carbon nano tubes |
| CN106623962A (en) * | 2016-12-31 | 2017-05-10 | 湖南省华京粉体材料有限公司 | Method for preparing nanometer tungsten powder by organizing sodium tungstate |
| CN106735282A (en) * | 2016-12-31 | 2017-05-31 | 湖南省华京粉体材料有限公司 | A kind of sodium molybdate organises the method for preparing nano Mo powder |
-
2008
- 2008-04-11 CN CNA2008101038833A patent/CN101249567A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353264B (en) * | 2008-09-26 | 2010-04-21 | 北京科技大学 | Method for improving ceramic metallized layer microstructure |
| CN103252506A (en) * | 2013-05-14 | 2013-08-21 | 厦门理工学院 | Preparation method of nanometer molybdenum powder containing homodisperse carbon nano tubes |
| CN103252506B (en) * | 2013-05-14 | 2015-05-13 | 厦门理工学院 | Preparation method of nanometer molybdenum powder containing homodisperse carbon nano tubes |
| CN106623962A (en) * | 2016-12-31 | 2017-05-10 | 湖南省华京粉体材料有限公司 | Method for preparing nanometer tungsten powder by organizing sodium tungstate |
| CN106735282A (en) * | 2016-12-31 | 2017-05-31 | 湖南省华京粉体材料有限公司 | A kind of sodium molybdate organises the method for preparing nano Mo powder |
| CN106623962B (en) * | 2016-12-31 | 2018-07-31 | 湖南省华京粉体材料有限公司 | A kind of sodium tungstate organises the method for preparing nano-tungsten powder |
| CN106735282B (en) * | 2016-12-31 | 2018-07-31 | 湖南省华京粉体材料有限公司 | A kind of sodium molybdate organises the method for preparing nano Mo powder |
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Open date: 20080827 |