CN101224500A - Super particle size molybdenum powder preparing method - Google Patents
Super particle size molybdenum powder preparing method Download PDFInfo
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- CN101224500A CN101224500A CNA2007101796456A CN200710179645A CN101224500A CN 101224500 A CN101224500 A CN 101224500A CN A2007101796456 A CNA2007101796456 A CN A2007101796456A CN 200710179645 A CN200710179645 A CN 200710179645A CN 101224500 A CN101224500 A CN 101224500A
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Abstract
The invention provides a preparation method of a molybdenum powder with ultra-large granularity, which relates to the preparation method used for an alloy powder with special physical performance and high melting point. The invention is characterized in that the preparation process comprises the following steps that: (1) a molybdenum powder is selected, with the Fisher particle size of 2.5-3.5 Mum, the loose density of 0.9 g/cm<3>-1.1 g/cm<3> and the oxygen content less than 0.08wt%; (2) the selected molybdenum powder is pressed into a blank under the pressure of 15MPa-30MPa; (3) the pressed blank is sintered for 1-5 hours under the temperature of 800-1200 DEG C; (4) the sintered blank is broken, ball milled and screened so as to prepare the molybdenum powder which consists of the grain groups with the average granularity of 100-200 Mum. By adopting the method of the invention, the molybdenum powder which consists of the grain groups with the average granularity of 100-200 Mum can be prepared and more than 80% of the yield can be realized.
Description
Technical field
A kind of preparation method of molybdenum of super particle size relates to a kind of preparation method who is used to have the high-melting-point alloy powder of specific physical performance.
Background technology
Have super particle size (particle mean size reaches more than the 10 μ m), (apparent density reaches 2.5g/cm to high specific gravity
3More than), the molybdenum powder of high fluidity specific physical performances such as (the Hall flow velocity reach more than the 30min/50g), have the conventional granulates molybdenum powder incomparable serviceability, show application prospects in fields such as space flight, electronics, automobiles.
Since nineteen forties as one independently since subject and the professional technique, through the development of over half a century, the powder preparation technology has obtained considerable progress.At present, the powder preparation technology can be divided into vapor phase method (comprising evaporation-condensation method and gas-phase reaction method), liquid phase method (comprising the precipitation method, sol-gel process and hydro-thermal method) and solid phase method tens of kinds of preparation technologies of three major types (Ring T A.Fundamentals of Ceramic Processing and Synthesis.London:Academic Press, 1996 such as (comprising Mechanical Method and chemical method); Lu Shouci. the powder technology handbook. Beijing: Chemical Industry Press, 2004).Because the fusing point of molybdenum and boiling point are respectively up to 2895K and 5077K, among these preparation methods, must be gas phase and liquid phase by at least one material mutually in the preparation process of vapor phase method and liquid phase method, therefore except that plasma method, this two big class technology can't be applicable to the preparation of molybdenum powder; And plasma method is because of its expensive manufacturing cost, can't realize molybdenum powder preparation in enormous quantities (Li Jianping. the international corrosion control conference collection of thesis of China powder granulation technology status and prospects .2002 China, 2002.623-626).In solid phase method, the chemical method of " molybdenum trioxide is produced in the ammonium molybdate roasting, and molybdenum trioxide segmentation thermal decomposition is a molybdenum powder " is adopted in the molybdenum powder preparation mostly.This method is fit to preparation medium size (particle mean size is 1 μ m～5 μ m) very much, (apparent density is 1g/cm to little proportion
3About), (the Hall flow velocity reaches 40～50min/50g) to lazy flow, the relatively poor conventional molybdenum powder of particle roundness.Because whole chemical treating process is controlled relatively poor, chemical method prepares comparatively difficulty (Boccaccini A R of the strict molybdenum powder of physical property, Veronsei P, Siligardi C, et al.Porous molybdenum particle reinforced glass matrix composites fabricated bymicrowave processing.Key Engineering Materials, 2002,206-213:317-320).
At present, the molybdenum powder product of this specific physical performance is monopolized by company of Japanese Nippon Steel (Nippon Steel), eastern Cao company (Tosoh), offshore companies of several family such as (Hitachi Metals) of Hitachi Metals company.Not not appearing in the newspapers as yet of the detail of its technology of preparing.
Summary of the invention
Purpose of the present invention is exactly the deficiency at above-mentioned prior art, and it is the method for the super particle size molybdenum powder formed of the cluster of grains of 100 μ m～200 μ m that a kind of can preparing by particle mean size is provided.
The objective of the invention is to be achieved through the following technical solutions.
A kind of super particle size molybdenum powder preparation method is characterized in that its preparation process may further comprise the steps:
(1) selecting Fisher particle size is 2.5～3.5 μ m, and apparent density is 0.9～1.1g/cm
3, oxygen content is less than the molybdenum powder of 0.08% (weight);
(2) molybdenum powder of selecting is pressed into base under 15MPa～30MPa pressure;
(3) with the compacting blank under 800 ℃～1200 ℃ temperature, sintering 1～5 hour;
(4) with blank fragmentation, ball milling and screening behind the sintering, preparing by particle mean size is the molybdenum powder that the cluster of grains of 100～200 μ m is formed.
A kind of super particle size molybdenum powder preparation method of the present invention is characterized in that the blank sintering process of described compacting is carried out under hydrogen shield.
Raw material of the present invention is that Fisher particle size is 2.5 μ m～3.5 μ m, and apparent density is 0.9g/cm
3～1.1g/cm
3Molybdenum powder, it is more or less freely to adopt traditional chemical method to prepare, it is in order to guarantee the chemical composition of finished product molybdenum powder that the chemical composition of molybdenum powder requires, the molybdenum powder of rule is in forming process for pattern, particle better mobile can more as one man guarantee sintering strength.
In the pressing process of the present invention, the conventional molybdenum powder of certain mass is packed into behind the mould, its press power and dwell time, promptly pressed density was as the criterion to guarantee the pressed compact size.According to the molybdenum powder of different batches, press power and dwell time can fluctuate between 15MPa～30MPa, 30s～60s.The pressed compact size is definite according to hydraulic press table top size first, second can not be less than the pan feeding dimensional requirement of jaw crusher.
Low sintering sintering temperature of the present invention and sintering time fluctuate to some extent according to different batches molybdenum powder physical property.The hydrogen flowing quantity of sintering and cooling procedure is decided according to the burner hearth size of different Muffle furnaces, to guarantee that sintered blank oxidation does not take place is as the criterion.
Adopt method of the present invention directly to adopt conventional molybdenum powder to carry out subsequent treatment, lower to the requirement of raw material; Whole technical process is a physical process, is different from traditional chemical reduction method, can guarantee technical process few (nothing) pollution; Adopt the cluster of grains molybdenum powder of this method preparation, its pattern is rounding comparatively, and the sintering strength of cluster of grains inside is higher, the broken automatically phenomenon of cluster of grains in use can not occur.Can prepare by particle mean size is the molybdenum powder that the cluster of grains of 100 μ m～200 μ m is formed, and realizes the yield rate more than 80%.
Description of drawings
Fig. 1 is the microscopic appearance figure of the molybdenum powder of employing method preparation of the present invention.
Fig. 2 (a) is the macro morphology figure of the molybdenum powder of employing method preparation of the present invention.
Fig. 2 (b) is the individual particle interior tissue shape appearance figure of the molybdenum powder of employing method preparation of the present invention.
The specific embodiment
A kind of super particle size molybdenum powder preparation method may further comprise the steps:
(1) selects suitable conventional molybdenum powder.The granularity and the density of molybdenum powder is moderate, and (Fisher particle size is 2.5 μ m～3.5 μ m, and apparent density is 0.9g/cm
3～1.1g/cm
3), chemical composition even, qualified (especially oxygen content is no more than 0.08wt%), the molybdenum powder pattern is rule comparatively, no too much overlap joint.
(2) pressed compact moulding.Adopt the hydraulic press and the mould of enough tonnages, molybdenum powder is pressed into base, guarantee that pressing process reaches the press power of 15MPa～30MPa, the dwell time reaches more than the 30s, and the pressed compact size is determined according to the hydraulic press mesa dimensions.
(3) low-temperature sintering.Pressed compact is put into molybdenum matter pallet by row, and placing granularity between pressed compact and the supporting spring is the zirconia ball of 1 μ m～5 μ m, uses the molybdenum filament interval of φ 1mm between the pressed compact.The pallet that the molybdenum pressed compact is housed is put in advance the Muffle furnace that heats up, select 800 ℃～1200 ℃ temperature, to pressed compact sintering 1～5 hour.Sintering and cooling procedure guarantee that hydrogen flowing quantity is 0.3m
3/ h～0.9m
3/ h.
(4) broken and screening.At first, adopt jaw crusher to carrying out fragmentation through low sintering molybdenum plate base, the outlet granularity is 1mm～5mm, then, adopts mechanical alloying equipment, select 1: 1 ratio of grinding media to material, molybdenum particle after the fragmentation is carried out ball milling 1 hour, next, adopt 60 order boltings, adopt the 560kg pneumatic hammer that oversize is carried out fragmentation at last, continue screening.
Embodiment 1
At first, selecting Fisher particle size is 2.76 μ m, and apparent density is 0.98g/cm
3Molybdenum powder, its oxygen content is 0.067wt%, microscopic appearance as shown in Figure 1.Then, on YA32-315A type four-column hydraulic press, adopt the press power of 20MPa and the dwell time of 30s to be pressed into base, pressed compact is of a size of 16mm * 60mm * 160mm.Pressed compact is put into molybdenum matter pallet by row, and placing granularity between pressed compact and the supporting spring is the zirconia ball of 1 μ m～5 μ m, uses the molybdenum filament interval of φ 1mm between the pressed compact.Pallet is put into Muffle furnace, select the technology of 900 ℃/2.5h to carry out low-temperature sintering.Cooled off 1 hour the cooling zone that pushes Muffle furnace behind the heat preservation sintering, and the hydrogen flowing quantity of Muffle furnace is 0.7m
3/ h～0.8m
3/ h.Subsequently the molybdenum plate base behind the sintering being fed one by one the product YGM7826 of Shanghai machine Manufacturing Co., Ltd of generation nation type flour mill smashs to pieces; to 1: 1 ratio of grinding media to material of outlet particle; ball milling is 1 hour in three batch mixers, and mechanical milling process vacuumizes protection to ball grinder, and (vacuum reaches 10
-2MPa).Ball milling and cooling back adopt 60 order vibratory sieves to sieve; the screenings collecting packing; oversize puts into that (anvil block is equipped with protective sleeve on the anvil block of 560kg pneumatic hammer; in case molybdenum powder pollutes); reforge hits 3～4 times, the molybdenum powder 60 mesh sieve branches after the collection hammering, screenings collecting packing; oversize is suppressed the slab of other purposes as the molybdenum waste material.
Adopt the molybdenum powder grain graininess of this method preparation can reach 100 μ m～200 μ m, its pattern is rounding (Fig. 2) comparatively, can satisfy follow-up instructions for uses such as thermal spraying.
Embodiment 2
Other conditions are with example 1, and selecting Fisher particle size is 2.5 μ m～3.5 μ m, and apparent density is 0.9g/cm
3～1.1g/cm
3, oxygen content is less than the molybdenum powder of 0.08% (weight); Be pressed into base at 15MPa; Under 800 ℃ temperature, sintering hour; With blank fragmentation, ball milling and the screening behind the sintering, preparing by particle mean size is the molybdenum powder that the cluster of grains of 100 μ m～200 μ m is formed.Its pattern is rounding comparatively, can satisfy follow-up instructions for uses such as thermal spraying.
Embodiment 3
Other conditions are with example 1, and selecting Fisher particle size is 2.5 μ m～3.5 μ m, and apparent density is 0.9g/cm
3～1.1g/cm
3, oxygen content is less than the molybdenum powder of 0.08% (weight); Under 30MPa pressure, be pressed into base; With the compacting blank under 1200 ℃ temperature, sintering 1 hour; With blank fragmentation, ball milling and the screening behind the sintering, preparing by particle mean size is the molybdenum powder that the cluster of grains of 100 μ m～200 μ m is formed.Its pattern is rounding comparatively, can satisfy follow-up instructions for uses such as thermal spraying.
Claims (2)
1. super particle size molybdenum powder preparation method is characterized in that its preparation process may further comprise the steps:
(1) selecting Fisher particle size is 2.5 μ m～3.5 μ m, and apparent density is 0.9g/cm
3～1.1g/cm
3, oxygen content is less than the molybdenum powder of 0.08% (weight);
(2) molybdenum powder of selecting is pressed into base under 15MPa～30MPa pressure;
(3) with the compacting blank under 800 ℃～1200 ℃ temperature, sintering 1～5 hour;
(4) with blank fragmentation, ball milling and screening behind the sintering, preparing by particle mean size is the molybdenum powder that the cluster of grains of 100 μ m～200 μ m is formed.
2. a kind of super particle size molybdenum powder preparation method according to claim 1 is characterized in that the blank burning process of described compacting is carried out under hydrogen shield.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102294490A (en) * | 2011-08-03 | 2011-12-28 | 成都虹波实业股份有限公司 | Crude molybdenum powder preparing method |
| CN103691934A (en) * | 2013-12-18 | 2014-04-02 | 浙江帕特尼触头有限公司 | Powder granulating method |
| CN104226979A (en) * | 2008-10-17 | 2014-12-24 | H.C.施塔克公司 | Molybdenum metal powder |
| CN105880613A (en) * | 2016-04-29 | 2016-08-24 | 金堆城钼业股份有限公司 | Preparation method of special molybdenum powder for producing molybdenum welding rod |
| CN108927514A (en) * | 2018-08-17 | 2018-12-04 | 曾爱华 | A kind of production method of powder metallurgy spherolite |
| CN110453166A (en) * | 2019-09-17 | 2019-11-15 | 厦门钨业股份有限公司 | A kind of preparation method proposing High-Purity Molybdenum bulk plasticity |
| CN110576180A (en) * | 2019-09-25 | 2019-12-17 | 福建阿石创新材料股份有限公司 | preparation method of molybdenum powder with low oxygen content |
| CN112091228A (en) * | 2020-09-23 | 2020-12-18 | 矿冶科技集团有限公司 | Preparation method of large-particle spherical tungsten powder |
| CN112207282A (en) * | 2020-09-17 | 2021-01-12 | 洛阳科威钨钼有限公司 | Preparation method of spraying molybdenum powder |
| CN112355312A (en) * | 2020-10-23 | 2021-02-12 | 中南大学 | Activation sintering preparation method of ultrafine-grained pure molybdenum metal material |
| CN113385679A (en) * | 2021-06-17 | 2021-09-14 | 安徽寒锐新材料有限公司 | Method for preparing cobalt powder with high apparent density |
| CN114247894A (en) * | 2020-09-25 | 2022-03-29 | 安泰天龙钨钼科技有限公司 | Method for preparing large-particle-size spherical tungsten powder by radio frequency plasma method |
| CN114850473A (en) * | 2022-04-13 | 2022-08-05 | 金堆城钼业股份有限公司 | Molybdenum and molybdenum alloy material sintering method and application thereof |
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2007
- 2007-12-17 CN CNA2007101796456A patent/CN101224500A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104226979A (en) * | 2008-10-17 | 2014-12-24 | H.C.施塔克公司 | Molybdenum metal powder |
| CN102294490A (en) * | 2011-08-03 | 2011-12-28 | 成都虹波实业股份有限公司 | Crude molybdenum powder preparing method |
| CN102294490B (en) * | 2011-08-03 | 2016-06-29 | 成都虹波实业股份有限公司 | A kind of method producing thick molybdenum powder |
| CN103691934A (en) * | 2013-12-18 | 2014-04-02 | 浙江帕特尼触头有限公司 | Powder granulating method |
| CN105880613A (en) * | 2016-04-29 | 2016-08-24 | 金堆城钼业股份有限公司 | Preparation method of special molybdenum powder for producing molybdenum welding rod |
| CN105880613B (en) * | 2016-04-29 | 2017-12-26 | 金堆城钼业股份有限公司 | A kind of special molybdenum powder preparation method for being used to make molybdenum welding rod |
| CN108927514A (en) * | 2018-08-17 | 2018-12-04 | 曾爱华 | A kind of production method of powder metallurgy spherolite |
| CN110453166A (en) * | 2019-09-17 | 2019-11-15 | 厦门钨业股份有限公司 | A kind of preparation method proposing High-Purity Molybdenum bulk plasticity |
| CN110576180A (en) * | 2019-09-25 | 2019-12-17 | 福建阿石创新材料股份有限公司 | preparation method of molybdenum powder with low oxygen content |
| CN110576180B (en) * | 2019-09-25 | 2022-01-11 | 福建阿石创新材料股份有限公司 | Preparation method of molybdenum powder with low oxygen content |
| CN112207282A (en) * | 2020-09-17 | 2021-01-12 | 洛阳科威钨钼有限公司 | Preparation method of spraying molybdenum powder |
| CN112091228A (en) * | 2020-09-23 | 2020-12-18 | 矿冶科技集团有限公司 | Preparation method of large-particle spherical tungsten powder |
| CN114247894A (en) * | 2020-09-25 | 2022-03-29 | 安泰天龙钨钼科技有限公司 | Method for preparing large-particle-size spherical tungsten powder by radio frequency plasma method |
| CN112355312A (en) * | 2020-10-23 | 2021-02-12 | 中南大学 | Activation sintering preparation method of ultrafine-grained pure molybdenum metal material |
| CN113385679A (en) * | 2021-06-17 | 2021-09-14 | 安徽寒锐新材料有限公司 | Method for preparing cobalt powder with high apparent density |
| CN114850473A (en) * | 2022-04-13 | 2022-08-05 | 金堆城钼业股份有限公司 | Molybdenum and molybdenum alloy material sintering method and application thereof |
| CN114850473B (en) * | 2022-04-13 | 2024-02-02 | 金堆城钼业股份有限公司 | Sintering method and application of molybdenum and molybdenum alloy material |
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Open date: 20080723 |