CN105880613A - Preparation method of special molybdenum powder for producing molybdenum welding rod - Google Patents
Preparation method of special molybdenum powder for producing molybdenum welding rod Download PDFInfo
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- CN105880613A CN105880613A CN201610281360.2A CN201610281360A CN105880613A CN 105880613 A CN105880613 A CN 105880613A CN 201610281360 A CN201610281360 A CN 201610281360A CN 105880613 A CN105880613 A CN 105880613A
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- molybdenum
- powder
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- welding rod
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
Abstract
The invention discloses a preparation method of special molybdenum powder for producing a molybdenum welding rod. The preparation method comprises the following steps of uniformly mixing industrial molybdenum dioxide and molybdenum trioxide by adopting solid-phase doping to obtain MoO2-MoO3 mixed powder; then reducing the MoO2-MoO3 mixed powder at high temperature to generate molybdenum powder; and vibrating and scattering the molybdenum powder, subsequently performing 200-mesh sieving on the scattered powder and then performing 80-mesh sieving on 200-mesh screen overflow, thus obtaining a final product. According to the molybdenum powder prepared by the preparation method disclosed by the invention, particles with smaller particle sizes and larger parts are removed, produced molybdenum powder particles are relatively uniform and stable and good in consistency and flowability; and technical requirements on powder for the welding rod are met; and in addition, a finished product rate is higher and can reach 70 percent.
Description
Technical field
The invention belongs to molybdenum powder preparing technical field, be specifically related to a kind of special molybdenum for making molybdenum welding rod
Powder, preparation method thereof.
Background technology
Molybdenum is a kind of refractory metal, has higher elevated temperature strength, good electrical and thermal conductivity, thermal expansion
Coefficient is similar to glass, be widely used in manufacturing coiled filament heart yearn, go between, link up with, line cutting wire,
Being used as to do grid and anode-supported material in electron tube, in ultra-large type integrated circuit, molybdenum is used as metal oxygen
Compound grid electrode of semiconductor and various types of electrodes, target etc., but molybdenum and molybdenum alloy fusing point height, workpiece welding difficulty
Greatly.
The raw material that at present conventional Mo powder production enterprise uses is ammonium molybdate or high-purity molybdenum trioxide carries out two
Section or three sections of hydrogen reducings, use the screen cloth of certain mesh number to carry out screening reduction molybdenum powder and finally produced
Product, the molybdenum powder that this conventional method is produced shows excellent when making the product such as molybdenum product, molybdenum filament
Good quality, but when making molybdenum welding rod owing to its granule is partially thin or granulation uniformity is poor, cause producing
The welding rod performance that during welding rod, mobile performance is the best, made is difficult to uniformly, easily go out during actual welding
The phenomenons such as existing uneven, the bubble of welding bead, do not reach welding quality.
Summary of the invention
It is an object of the invention to provide a kind of special molybdenum powder preparation method for making molybdenum welding rod, solve
The welding rod that molybdenum powder that existing method obtains makes, occurs that during actual welding welding bead is uneven, bubble
Etc. problem.
The technical solution adopted in the present invention is, a kind of special molybdenum powder preparation side for making molybdenum welding rod
Method, uses commercial silica molybdenum and high-purity molybdenum trioxide solid-solid doping mix homogeneously, obtains
MoO2-MoO3Mixed-powder；Then MoO2-MoO3Mixed-powder generates molybdenum powder through high temperature reduction,
First carry out 200 mesh sieves after molybdenum powder vibration being broken up to divide, then 200 mesh oversizes carried out 80 mesh sieves and divide,
I.e. obtain making the special molybdenum powder of molybdenum welding rod.
The feature of the present invention also resides in,
High-purity molybdenum trioxide is 1:1.5～1.86 with the mass ratio of molybdenum dioxide.
Solid-solid doping mix homogeneously be by molybdenum dioxide and molybdenum trioxide in Double cone mixer batch mixing 4～
5h。
High temperature reduction is by MoO2-MoO3Mixed-powder fills according to the boat loading depth of 3.0～4.5cm
Boat, uses dew point inversely to flow through MoO for-45 DEG C～-20 DEG C of hydrogen2-MoO3Mixed-powder, high temperature is also
The former stage takes staged heating mode, according to first district insulation 2～2.5h, reduction temperature be 800 DEG C～
950℃；Second district's insulation 2h, reduction temperature is 920 DEG C～960 DEG C；3rd district insulation 2～2.5h,
Reduction temperature is 950 DEG C～995 DEG C；4th district insulation 2.5～3h, reduction temperature is 980 DEG C～1080 DEG C.
The invention has the beneficial effects as follows,
(1) this method does not has new requirement to equipment, it is not necessary to increases conventional production lines or changes and appoints
What part, is only achieved that the production of this special molybdenum powder by technique adjustment, is suitable for industrialized production.
(2) this method is simple, it is not necessary to the personnel producing this specification molybdenum powder carry out too many knowledge
Updating, train, the personnel possessing traditional Mo powder production technology can rest in this production method soon.
(3) molybdenum powder that this method produces eliminates that granularity is the thinnest and part bigger than normal, the molybdenum powder granule of production
Relatively uniform, concordance and mobility are moderately good, meet the technology requirement of welding rod powder.
(4) the welding rod special molybdenum powder yield rate that this method produces is higher, can reach 70%.
Accompanying drawing explanation
Fig. 1 is the electron-microscope scanning figure of the molybdenum powder that the inventive method obtains.
Detailed description of the invention
The present invention is described in detail with detailed description of the invention below in conjunction with the accompanying drawings.
The present invention is for making the special molybdenum powder preparation method of molybdenum welding rod, it is provided that a kind of technique is simple, finished product
Rate is high, be suitable for the production technology of the special molybdenum powder of molybdenum welding rod of industrialized production, and the method is to use three oxidations
Molybdenum and commercial silica molybdenum mixture be raw material through a high temperature reduction, then through twice screening produce-80
Mesh～+200 mesh, granule uniformly, the making special molybdenum powder of molybdenum welding rod of good flowing properties.
Concrete preparation process is as follows:
Step 1, is that 1:1.5～1.86 is at bipyramid by high-purity molybdenum trioxide and commercial silica molybdenum in mass ratio
In batch mixer, batch mixing 4～5h, obtain MoO2-MoO3Mixed-powder；Wherein commercial silica molybdenum Fei Shi
Granularity is 3.5～10.2 μm, apparent density 0.95～1.50g/cm3；
Step 2, the MoO that step 1 is obtained2-MoO3Mixed-powder according to 3.0～4.5cm dress boat
Thickness carries out filling boat, uses dew point inversely to flow through MoO for-45 DEG C～-20 DEG C of hydrogen2-MoO3Mixed powder
End, the high temperature reduction stage takes staged heating mode, according to the firstth district insulation 2～2.5h, reduction temperature
Degree is 800 DEG C～950 DEG C；Second district's insulation 2h, reduction temperature is 920 DEG C～960 DEG C；3rd district is protected
Temperature 2～2.5h, reduction temperature is 950 DEG C～995 DEG C；4th district insulation 2.5～3h, reduction temperature is
980 DEG C～1080 DEG C, obtain molybdenum powder；
Step 3, molybdenum powder step 2 obtained vibration first carries out 200 mesh sieves after breaing up and divides, then to 200
Mesh oversize carries out 80 mesh sieves and divides, and i.e. obtains making the special molybdenum powder of molybdenum welding rod.
Fig. 1 is the electron-microscope scanning figure of the special molybdenum powder of molybdenum welding rod that preparation method of the present invention obtains, from Fig. 1
It can be seen that the granule of molybdenum powder prepared by the inventive method is essentially independent individual particle distribution, granulated
Looks distribution is the most uniform；In powder flowbility is tested, find that this molybdenum powder has preferable mobility.
High-purity molybdenum trioxide and commercial silica molybdenum are 1:1.5～1.86 by the inventive method in mass ratio
Mixing obtains final products, because molybdenum trioxide has relatively low through high temperature reduction furnace high temperature reduction, screening again
Melt temperature, when 795 DEG C, equally distributed molybdenum trioxide can melt and enter molybdenum dioxide about
Row parcel, the molybdenum trioxide of this package status is the most uniformly reunited with molybdenum dioxide mixture
The molybdenum powder of state distribution, but because between molybdenum trioxide and molybdenum dioxide mixture, there is again the dioxy of infusibility
Change molybdenum segmentation crystal boundary, so the reunion state molybdenum powder that reduction generates, present with multiple independent molybdenum dioxide as core
Reunion state molybdenum powder, between each reunion state molybdenum powder interface, reunion strength is more weak, and this molybdenum powder is through certain
Vibration, bounce, can divide between interface, depolymerization, form larger particles independence molybdenum powder, then to this molybdenum powder
Sieving, sieve order is first to cross 200 eye mesh screens again, and 200 mesh oversizes are crossed 80 eye mesh screens again,
The molybdenum powder granule obtained is relatively uniform, complete, good fluidity, and the welding molybdenum powder according to said method produced
Quality is high, steady quality, and yield rate can reach about 70%.
Why the present invention selects-80 mesh～the molybdenum powder of+200 mesh, because of whole to molybdenum powder of the special molybdenum powder of welding rod
Body particle requirement is the strictest, it is desirable to uniform, good fluidity.The present invention, in the high temperature reduction stage, uses
Molybdenum trioxide melts the form of parcel molybdenum dioxide, makes molybdenum powder granule have certain reunion, increases molybdenum
Powder particles size, the particle size of this molybdenum powder is substantially all more than 200 eye mesh screen mesh diameters, and 80
Below eye mesh screen aperture, 200 mesh first eliminate the part that granularity is the thinnest, and 80 mesh sieves divide that to eliminate granularity inclined
Big part, product takes on 200 mesh sieves, and under 80 mesh sieves, this stage molybdenum powder granularity is substantially uniform, consistent
Property relatively strong and good fluidity.
When the molybdenum powder using preparation method of the present invention to prepare makes welding rod, welding rod is homogeneous, when welding
The phenomenons such as the welding rod welding bead when welding avoiding tradition molybdenum powder making is uneven, bubble.
Embodiment 1
Step 1, mixes at bipyramid for 1:1.86 in mass ratio by high-purity molybdenum trioxide and commercial silica molybdenum
In material machine, batch mixing 4h, obtains MoO2-MoO3Mixed-powder；Wherein commercial silica molybdenum average Fei Shi grain
Degree is 6.8 μm, apparent density 1.0g/cm3；
Step 2, the MoO that step 1 is obtained2-MoO3Mixed-powder is according to the boat loading depth of 3.5cm
Carry out filling boat, use dew point inversely to flow through MoO for-45 DEG C of hydrogen2-MoO3Mixed-powder, high temperature reduction
Stage takes staged heating mode, and according to first district's insulation 2h, reduction temperature is 900 DEG C；Secondth district
Insulation 2h, reduction temperature is 920 DEG C；3rd district's insulation 2.5h, reduction temperature is 950 DEG C；4th district
Insulation 2.5h, reduction temperature is 1000 DEG C, obtains molybdenum powder；
Step 3, molybdenum powder step 2 obtained vibration first carries out 200 mesh sieves after breaing up and divides, then to 200
Mesh oversize carries out 80 mesh sieves and divides, and i.e. obtains making the special molybdenum powder of molybdenum welding rod.
Embodiment 2
Step 1, is that 1:1.5 is at bipyramid batch mixing by high-purity molybdenum trioxide and commercial silica molybdenum in mass ratio
Batch mixing 5h in machine, obtains MoO2-MoO3Mixed-powder；The wherein average Fisher particle size of commercial silica molybdenum
It is 3.5 μm, apparent density 1.20g/cm3；
Step 2, the MoO that step 1 is obtained2-MoO3Mixed-powder is according to the boat loading depth of 4.5cm
Carry out filling boat, use dew point inversely to flow through MoO for-30 DEG C of hydrogen2-MoO3Mixed-powder, high temperature reduction
Stage takes staged heating mode, and according to first district's insulation 2.5h, reduction temperature is 800 DEG C；Second
District's insulation 2h, reduction temperature is 940 DEG C；3rd district's insulation 2h, reduction temperature is 980 DEG C；4th district
Insulation 3h, reduction temperature is 1080 DEG C, obtains molybdenum powder；
Step 3, molybdenum powder step 2 obtained vibration first carries out 200 mesh sieves after breaing up and divides, then to 200
Mesh oversize carries out 80 mesh sieves and divides, and i.e. obtains making the special molybdenum powder of molybdenum welding rod.
Embodiment 3
Step 1, mixes at bipyramid for 1:1.67 in mass ratio by high-purity molybdenum trioxide and commercial silica molybdenum
In material machine, batch mixing 4.5h, obtains MoO2-MoO3Mixed-powder；The wherein average Fei Shi of commercial silica molybdenum
Granularity is 10.2 μm, apparent density 1.50g/cm3；
Step 2, the MoO that step 1 is obtained2-MoO3Mixed-powder is according to the boat loading depth of 3.0cm
Carry out filling boat, use dew point inversely to flow through MoO for-20 DEG C of hydrogen2-MoO3Mixed-powder, high temperature reduction
Stage takes staged heating mode, and according to first district's insulation 2.2h, reduction temperature is 950 DEG C；Second
District's insulation 2h, reduction temperature is 960 DEG C；3rd district's insulation 2.3h, reduction temperature is 995 DEG C；4th
District's insulation 2.8h, reduction temperature is 1020 DEG C, obtains molybdenum powder；
Step 3, molybdenum powder step 2 obtained vibration first carries out 200 mesh sieves after breaing up and divides, then to 200
Mesh oversize carries out 80 mesh sieves and divides, and i.e. obtains making the special molybdenum powder of molybdenum welding rod.
Embodiment 4
Step 1, mixes at bipyramid for 1:1.75 in mass ratio by high-purity molybdenum trioxide and commercial silica molybdenum
In material machine, batch mixing 4.5h, obtains MoO2-MoO3Mixed-powder；The wherein average Fei Shi of commercial silica molybdenum
Granularity is 8.2 μm, apparent density 0.95g/cm3；
Step 2, the MoO that step 1 is obtained2-MoO3Mixed-powder is according to the boat loading depth of 4.0cm
Carry out filling boat, use dew point inversely to flow through MoO for-40 DEG C of hydrogen2-MoO3Mixed-powder, high temperature reduction
Stage takes staged heating mode, and according to first district's insulation 2.3h, reduction temperature is 920 DEG C；Second
District's insulation 2h, reduction temperature is 950 DEG C；3rd district's insulation 2.2h, reduction temperature is 960 DEG C；4th
District's insulation 2.5h, reduction temperature is 980 DEG C, obtains molybdenum powder；
Step 3, molybdenum powder step 2 obtained vibration first carries out 200 mesh sieves after breaing up and divides, then to 200
Mesh oversize carries out 80 mesh sieves and divides, and i.e. obtains making the special molybdenum powder of molybdenum welding rod.
Claims (4)
1. the special molybdenum powder preparation method being used for making molybdenum welding rod, it is characterised in that by industry dioxy
Change molybdenum and molybdenum trioxide uses solid-solid doping mix homogeneously, obtain MoO2-MoO3Mixed-powder；Then
MoO2-MoO3Mixed-powder generates molybdenum powder through high temperature reduction, first carries out 200 after molybdenum powder vibration being broken up
Mesh sieve divides, and then 200 mesh oversizes is carried out 80 mesh sieves and divides, and i.e. obtains making the special molybdenum of molybdenum welding rod
Powder.
Special molybdenum powder preparation method for making molybdenum welding rod the most according to claim 1, its feature
Being, described molybdenum trioxide is 1:1.5～1.86 with the mass ratio of molybdenum dioxide.
Special molybdenum powder preparation method for making molybdenum welding rod the most according to claim 1 and 2, its
Being characterised by, solid-solid doping mix homogeneously is molybdenum dioxide and molybdenum trioxide to be mixed in Double cone mixer
Material 4～5h.
Special molybdenum powder preparation method for making molybdenum welding rod the most according to claim 1, its feature
Being, high temperature reduction is by MoO2-MoO3Mixed-powder is carried out according to the boat loading depth of 3.0～4.5cm
Dress boat, uses dew point inversely to flow through MoO for-45 DEG C～-20 DEG C of hydrogen2-MoO3Mixed-powder, high temperature
Reduction phase takes staged heating mode, and according to the firstth district insulation 2～2.5h, reduction temperature is
800 DEG C～950 DEG C；Second district's insulation 2h, reduction temperature is 920 DEG C～960 DEG C；3rd district insulation 2～
2.5h, reduction temperature is 950 DEG C～995 DEG C；4th district insulation 2.5～3h, reduction temperature be 980 DEG C～
1080℃。
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| JP2009527640A (en) * | 2006-02-17 | 2009-07-30 | クライマックス エンジニアード マテリアルズ リミテッド ライアビリティ カンパニー | High density molybdenum metal powder and method for producing the same |
| CN101224500A (en) * | 2007-12-17 | 2008-07-23 | 金堆城钼业股份有限公司 | Super particle size molybdenum powder preparing method |
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