CN104475759A - Preparation method for high-dispersion superfine nanometer Mo-Cu compound powder - Google Patents
Preparation method for high-dispersion superfine nanometer Mo-Cu compound powder Download PDFInfo
- Publication number
- CN104475759A CN104475759A CN201510001087.9A CN201510001087A CN104475759A CN 104475759 A CN104475759 A CN 104475759A CN 201510001087 A CN201510001087 A CN 201510001087A CN 104475759 A CN104475759 A CN 104475759A
- Authority
- CN
- China
- Prior art keywords
- molybdenum
- preparation
- composite powder
- copper
- nanometer
- 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.)
- Pending
Links
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method for high-dispersion superfine nanometer Mo-Cu compound powder. Firstly, an ammonia-water solution of copper salt is added to a deionized water solution of molybdenum salt, a mixed solution is formed, the pH of the mixed solution is adjusted to be 5-7, then the water solution is heated, filtered, washed, dried and calcined, and precursor molybdenum and copper oxide power is obtained; secondly, the precursor powder is restored in hydrogen, and the high-dispersion superfine nanometer Mo-Cu compound powder is obtained. The nanometer powder prepared through the method has the advantages of being large in specific surface area, fine and uniform in particle diameter, high in purity and the like. Through the simple and effective method that the molybdenum and copper precursor powder is prepared through chemical coprecipitation, magnetic stirring and thermostatic waterbath heating, and then is calcined and restored, the method is simple and rapid, the process is easy to operate and control, the yield of the powder is large, efficiency is high, and the preparation method is suitable for industrial volume production.
Description
Technical field
The invention discloses a kind of preparation method of high-dispersion ultrafine nanometer Mo-Cu composite powder, belong to powder metallurgy preparing technical field.
Background technology
Composite material of molybdenum and copper is a kind of pseudo-alloy, combines the high-ductility of the high-melting-point of molybdenum, high strength and copper, high-conductivity, has the combination property that high temperature resistance, resistance to ablation etc. are good.Electrical contact mainly as high-voltage switch gear before molybdenum copper product is applied, and is widely used in the fields such as electrotechnical, electronic, instrument and meter, defence and military, Aero-Space in recent years.
Because Mo and Cu is immiscible, the Mo-Cu alloy sintering performance adopting common " powder mixing+shaping+liquid-phase sintering " technique or the molten method of oozing to produce is lower, all there is the shortcomings such as component segregation, relative density are not high, have a strong impact on the performance of molybdenum copper product, be difficult to the requirements at the higher level that satisfied new application proposes.Powder metallurgy sintered molybdenum-copper composite nano-powder is utilized can effectively to avoid above shortcoming to prepare composite material of molybdenum and copper.Prepare nanometer molybdenum cuprum powder at present and be mainly divided into Mechanical Method and chemical method, Mechanical Method, by ball milling molybdenum Cu oxide, reaches the object of micronized particles, and reduction obtains molybdenum-copper compound powder, but ball milling introduces the impurity such as Fe for a long time, has a strong impact on the combination property of molybdenum copper product; Chemical method avoids introducing impurity, by producing micro-nano molybdenum copper precursor, obtains molybdenum-copper compound powder by calcining reduction.But there is corresponding shortcoming, existing chemical method has metal oxide co-reducing process, chemical vaporization coacervation, mechanical thermal chemical method, electroless plating method etc., and these methods are high to equipment requirement, or technique relative complex, wherein individually multistage is also needed to reduce, or manufacturing cycle is very long.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art and a kind of preparation method of high-dispersion ultrafine nanometer Mo-Cu composite powder is provided.The nano composite powder particle mean size that the method prepares is less than 60nm, and equipment, technique are simple, with short production cycle.
Technical scheme of the present invention is:
A preparation method for high-dispersion ultrafine nanometer Mo-Cu composite powder, comprises the steps:
(1) preparation of molybdenum copper composite oxide power
According to mass ratio 28:7 ~ 16 of molybdenum and copper, the concentrated ammonia solution of mantoquita is joined in molybdenum salting liquid, obtain mixed solution, mixed solution pH to 5 ~ 7 are regulated with hydrochloric acid, then heat 5 ~ 15 minutes in the water-bath of 60 ~ 80 DEG C, again after filtration, washing, dry, the dried powder obtained is calcined, obtains molybdenum Cu oxide precursor powder; Wherein, the consumption of concentrated ammonia liquor is 1 ~ 2 times of copper ion quality, and the mass fraction of concentrated ammonia liquor is 25 ~ 28%;
(2) preparation of high-dispersion ultrafine nanometer molybdenum cuprum composite powder
Step (1) gained molybdenum Cu oxide precursor powder is placed in H2 atmosphere reduce, obtains high-dispersion ultrafine nanometer Mo-Cu composite powder.
Further, ageing 8 ~ 10 hours before described mixed solution heating water bath.
Further, described molybdenum salt is ammonium molybdate or ammonium paramolybdate.
Further, described mantoquita is copper chloride or copper nitrate.
Further, in described mixed solution, the molar concentration of molybdenum ion is 0.1 ~ 0.8mol/L, and the molar concentration of copper ion is 0.1 ~ 0.3mol/L, and the concentration of molybdenum ion is greater than the concentration of copper ion.
Further, the calcining heat of step (1) is 350 ~ 450 DEG C, and the time is 0.5 ~ 2.5 hour.
Further, the reduction temperature of step (2) is 600 ~ 800 DEG C, and the time is 1 ~ 3 hour.
Beneficial effect of the present invention is:
The present invention adopts the method for chemical coprecipitation to prepare presoma, and mixed solution is through magnetic agitation water bath with thermostatic control heating, and the precursor powder density that the method obtains is high, Tissue distribution is even, particle is tiny, and particle mean size can be less than 60nm, contributes to the densified of follow-up sintering; Regulate mantoquita in mixed solution with the proportioning of molybdenum salt, the nanometer molybdenum cuprum composite powder of arbitrary proportion in certain limit can be obtained.Compared with the method reported, the inventive method simple and fast, technique is easy to control, and powder output is large, and efficiency is high, is applicable to industrial volume production.
Accompanying drawing explanation
Fig. 1 is the XRD diffraction pattern of the embodiment of the present invention 1 products therefrom.
Fig. 2,3,4,5 is that the Flied emission SEM of the embodiment of the present invention 1 products therefrom schemes.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further details, but the present invention is not limited to this.
Embodiment 1
(1) take 16.94g Sodium Molybdate Dihydrate, 7.70g copper chloride dihydrate, measure the concentrated ammonia liquor that 0.1L mass fraction is 25%, be mixed with the aqueous solution of sodium molybdate, the ammonia spirit of copper chloride, mixing adds the mixed solution that deionized water is configured to 0.5L.
(2) (1) is prepared the solution obtained and be divided into four parts, be placed in magnetic agitation water bath with thermostatic control container 60 DEG C of heating water baths respectively 10 minutes.
(3) solution (2) obtained is through filtration, washing, drying.
(4) sediment (3) obtained is in atmosphere through 350 DEG C of calcinings, and calcination time is 1h, obtains molybdenum Cu oxide composite powder.
Composite powder obtained to (4) is incubated 2h in 750 DEG C in H2, obtains the nanometer molybdenum cuprum composite powder of 70Mo-30Cu.As can be seen from Figure 1, embodiment 1 gained powder is made up of molybdenum and copper two kinds of materials.
The data obtained by Fig. 1, analyzed by Jade and obtain half-peak breadth, utilize Scherrer formula by half-peak breadth, calculating average grain size is 57nm.
Dhkl＝kλ/βcosθ
Wherein, Dhkl is that k is Scherrer constant, and λ is incident X-rays wavelength, and θ is Bragg diffraction angle (°), and β is the peak width at half height (rad) of diffraction maximum along the crystal grain diameter perpendicular to crystal face (hkl) direction.
As can be seen from Fig. 2,3,4,5, the second particle that embodiment 1 gained powder is assembled by very little primary particle forms, and specific area is flourishing, and particle is tiny and be evenly distributed.
Embodiment 2
(1) take 19.36g Sodium Molybdate Dihydrate, 5.17g copper chloride dihydrate, measure the concentrated ammonia liquor that 0.08L mass fraction is 28%, be mixed with the aqueous solution of sodium molybdate, the ammonia spirit of copper chloride, mixing adds the mixed solution that deionized water is configured to 0.5L.
(2) (1) is prepared the solution obtained and be divided into four parts, be placed in magnetic agitation water bath with thermostatic control container 80 DEG C of heating water baths respectively 5 minutes.
(3) solution (2) obtained is through filtration, washing, drying.
(4) sediment (3) obtained is in atmosphere through 450 DEG C of calcinings, and calcination time is 0.5h, obtains molybdenum Cu oxide composite powder.
(5) composite powder obtained to (4) is incubated 3h in 600 DEG C in H2, obtains the nanometer molybdenum cuprum composite powder of 80Mo-20Cu.
Embodiment 3
(1) take 18.88g Sodium Molybdate Dihydrate, 10.77g copper chloride dihydrate, measure the concentrated ammonia liquor that 0.1L mass fraction is 26%, be mixed with the aqueous solution of sodium molybdate, the ammonia spirit of copper chloride, mixing adds the mixed solution that deionized water is configured to 0.5L.
(2) (1) is prepared the solution obtained and be divided into four parts, be placed in magnetic agitation water bath with thermostatic control container 70 DEG C of heating water baths respectively 15 minutes.
(3) solution (2) obtained is through filtration, washing, drying.
(4) sediment (3) obtained is in atmosphere through 400 DEG C of calcinings, and calcination time is 2.5h, obtains molybdenum Cu oxide composite powder.
(5) composite powder obtained to (4) is incubated 2h in 800 DEG C in H2, obtains the nanometer molybdenum cuprum composite powder of 65Mo-35Cu.
Claims (8)
1. a preparation method for high-dispersion ultrafine nanometer Mo-Cu composite powder, is characterized in that comprising the steps:
(1) preparation of molybdenum copper composite oxide power
According to mass ratio 28:7 ~ 16 of molybdenum and copper, the concentrated ammonia solution of mantoquita is joined in molybdenum salting liquid, obtain mixed solution, mixed solution pH to 5 ~ 7 are regulated with hydrochloric acid, then heat 5 ~ 15 minutes in the water-bath of 60 ~ 80 DEG C, again after filtration, washing, dry, the dried powder obtained is calcined, obtains molybdenum Cu oxide precursor powder;
(2) preparation of high-dispersion ultrafine nanometer molybdenum cuprum composite powder
Step (1) gained molybdenum Cu oxide precursor powder is placed in H
2reduce in atmosphere, obtain high-dispersion ultrafine nanometer Mo-Cu composite powder.
2. the preparation method of high-dispersion ultrafine nanometer Mo-Cu composite powder according to claim 1, is characterized in that: ageing 8 ~ 10 hours before described mixed solution heating water bath.
3. the preparation method of high-dispersion ultrafine nanometer Mo-Cu composite powder according to claim 1 and 2, is characterized in that: the consumption of described concentrated ammonia liquor is 1 ~ 2 times of copper ion quality, and the mass fraction of described concentrated ammonia liquor is 25 ~ 28%.
4. the preparation method of high-dispersion ultrafine nanometer Mo-Cu composite powder according to claim 1 and 2, is characterized in that: described molybdenum salt is ammonium molybdate or ammonium paramolybdate.
5. the preparation method of high-dispersion ultrafine nanometer Mo-Cu composite powder according to claim 1 and 2, is characterized in that: described mantoquita is copper chloride or copper nitrate.
6. the preparation method of high-dispersion ultrafine nanometer Mo-Cu composite powder according to claim 1 and 2, it is characterized in that: in described mixed solution, the molar concentration of molybdenum ion is 0.1 ~ 0.8mol/L, the molar concentration of copper ion is 0.1 ~ 0.3mol/L, and the concentration of molybdenum ion is greater than the concentration of copper ion.
7. the preparation method of high-dispersion ultrafine nanometer Mo-Cu composite powder according to claim 1 and 2, is characterized in that: the calcining heat of described step (1) is 350 ~ 450 DEG C, and the time is 0.5 ~ 2.5 hour.
8. the preparation method of high-dispersion ultrafine nanometer Mo-Cu composite powder according to claim 1 and 2, is characterized in that: the reduction temperature of described step (2) is 600 ~ 800 DEG C, and the time is 1 ~ 3 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510001087.9A CN104475759A (en) | 2015-01-04 | 2015-01-04 | Preparation method for high-dispersion superfine nanometer Mo-Cu compound powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510001087.9A CN104475759A (en) | 2015-01-04 | 2015-01-04 | Preparation method for high-dispersion superfine nanometer Mo-Cu compound powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104475759A true CN104475759A (en) | 2015-04-01 |
Family
ID=52750435
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510001087.9A Pending CN104475759A (en) | 2015-01-04 | 2015-01-04 | Preparation method for high-dispersion superfine nanometer Mo-Cu compound powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104475759A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722769A (en) * | 2015-04-16 | 2015-06-24 | 柳州豪祥特科技有限公司 | Copper molybdenum powder preparation process |
| CN104722768A (en) * | 2015-04-16 | 2015-06-24 | 柳州豪祥特科技有限公司 | Iron molybdenum powder preparation method |
| CN110695367A (en) * | 2019-10-29 | 2020-01-17 | 金堆城钼业股份有限公司 | Preparation method of molybdenum-tungsten alloy powder |
| CN115612883A (en) * | 2022-10-31 | 2023-01-17 | 西安交通大学 | Method for preparing porous molybdenum-copper alloy framework by in-situ decomposition of ammonium molybdate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134243A (en) * | 2007-09-26 | 2008-03-05 | 中南大学 | Ultra-fine or nanometer molybdenum cuprum composite powder and method of producing the alloy thereof |
| CN101168197A (en) * | 2006-10-25 | 2008-04-30 | 中南大学 | Method for preparing ultra-fine/nano tungsten-copper-nickel composite powder |
| KR20120072236A (en) * | 2010-12-23 | 2012-07-03 | 재단법인 포항산업과학연구원 | Cu-sn-mo based alloy having superior strength, and manufacturing method thereof |
| CN102909389A (en) * | 2012-11-13 | 2013-02-06 | 中南大学 | Method for reducing and preparing nano molybdenum-copper composite powder with low temperature |
-
2015
- 2015-01-04 CN CN201510001087.9A patent/CN104475759A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168197A (en) * | 2006-10-25 | 2008-04-30 | 中南大学 | Method for preparing ultra-fine/nano tungsten-copper-nickel composite powder |
| CN101134243A (en) * | 2007-09-26 | 2008-03-05 | 中南大学 | Ultra-fine or nanometer molybdenum cuprum composite powder and method of producing the alloy thereof |
| KR20120072236A (en) * | 2010-12-23 | 2012-07-03 | 재단법인 포항산업과학연구원 | Cu-sn-mo based alloy having superior strength, and manufacturing method thereof |
| CN102909389A (en) * | 2012-11-13 | 2013-02-06 | 中南大学 | Method for reducing and preparing nano molybdenum-copper composite powder with low temperature |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722769A (en) * | 2015-04-16 | 2015-06-24 | 柳州豪祥特科技有限公司 | Copper molybdenum powder preparation process |
| CN104722768A (en) * | 2015-04-16 | 2015-06-24 | 柳州豪祥特科技有限公司 | Iron molybdenum powder preparation method |
| CN110695367A (en) * | 2019-10-29 | 2020-01-17 | 金堆城钼业股份有限公司 | Preparation method of molybdenum-tungsten alloy powder |
| CN115612883A (en) * | 2022-10-31 | 2023-01-17 | 西安交通大学 | Method for preparing porous molybdenum-copper alloy framework by in-situ decomposition of ammonium molybdate |
| CN115612883B (en) * | 2022-10-31 | 2023-08-04 | 西安交通大学 | Method for preparing porous molybdenum-copper alloy framework by in-situ decomposition of ammonium molybdate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106077695B (en) | A kind of preparation method of high-copper tungsten copper nano composite powder | |
| CN103537686B (en) | A kind of preparation method with the WCu composite powder of tungsten coated copper phenomenon | |
| CN104475759A (en) | Preparation method for high-dispersion superfine nanometer Mo-Cu compound powder | |
| CN102350508B (en) | Method for preparing doped-tungsten-based composite powder | |
| CN106994517B (en) | A kind of preparation method of high-thermal-conductivity low-expansibility W-Cu encapsulating material | |
| CN106564927A (en) | Preparation method of superfine yttrium oxide doped tungsten composite precursor powder | |
| CN108580917B (en) | Method for preparing tungsten dispersion strengthening copper superfine powder by low-temperature combustion synthesis | |
| CN102941350B (en) | Preparation method of nano copper powder | |
| Wang et al. | Preparation of w–cu nano-composite powders with high copper content using a chemical co-deposition technique | |
| CN101433968B (en) | Method for preparing micro spherical tungsten powder | |
| CN108543952A (en) | A kind of method of precursor process synthesis WC base nano composite powders | |
| CN102942471B (en) | Prepare the method for oxalate | |
| CN107900373B (en) | Superfine W-Cu composite powder and preparation method thereof | |
| CN104528803B (en) | A kind of preparation method of the flake porous nano materials of ZnO | |
| CN110184488A (en) | A kind of method that short route prepares metal dispersion-strengthened Cu | |
| CN107470646B (en) | Preparation method of superfine tungsten powder composite powder | |
| TW201542038A (en) | Method and apparatus for producing core-shell type metal nanoparticles | |
| CN103951416B (en) | A kind of composite Nano ZnO voltage-sensitive ceramic raw powder's production technology | |
| CN102909389B (en) | Method for reducing and preparing nano molybdenum-copper composite powder with low temperature | |
| CN103600087B (en) | A kind of aerosol spray-reducing process prepares the method at ultrafine tungsten argentum composite powder end | |
| CN101214994B (en) | Process for preparing nano powder of copper indium oxide | |
| CN104445350A (en) | Superfine Y2O3 powder prepared by adopting ultrasonically-assisted precipitation method | |
| CN104495905A (en) | Ultrasonic-assisted precipitation preparation method for Y2O3 ultrafine powder | |
| CN104843792B (en) | A kind of method of preparing the purple tungsten powder of nanometer needle-like | |
| Wang et al. | Crystallization behavior of 3D-structured OMS-2 under hydrothermal conditions |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150401 |
|
| RJ01 | Rejection of invention patent application after publication |