AU2021105398A4 - Method for preparing uniform and ultrafine nano tungsten powder of complete crystallization without agglomeration - Google Patents
Method for preparing uniform and ultrafine nano tungsten powder of complete crystallization without agglomeration Download PDFInfo
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 238000002425 crystallisation Methods 0.000 title claims abstract description 31
- 230000008025 crystallization Effects 0.000 title claims abstract description 31
- 238000005054 agglomeration Methods 0.000 title claims abstract description 28
- 230000002776 aggregation Effects 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 123
- 239000000843 powder Substances 0.000 claims abstract description 61
- 230000009467 reduction Effects 0.000 claims abstract description 29
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 238000009776 industrial production Methods 0.000 claims abstract description 9
- DZKDPOPGYFUOGI-UHFFFAOYSA-N tungsten(iv) oxide Chemical compound O=[W]=O DZKDPOPGYFUOGI-UHFFFAOYSA-N 0.000 claims description 26
- 238000011068 loading method Methods 0.000 claims description 10
- 229910052721 tungsten Inorganic materials 0.000 claims description 10
- 239000010937 tungsten Substances 0.000 claims description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 description 7
- 230000008520 organization Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 210000004940 nucleus Anatomy 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
- -1 tungsten oxide - tungsten oxide- tungsten Chemical compound 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
-
- 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
-
- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/045—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/01—Reducing atmosphere
- B22F2201/013—Hydrogen
-
- 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
- B22F2203/00—Controlling
- B22F2203/11—Controlling temperature, temperature profile
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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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
-
- 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
- B22F2304/00—Physical aspects of the powder
- B22F2304/05—Submicron size particles
- B22F2304/054—Particle size between 1 and 100 nm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for preparing uniform and ultrafine nano tungsten
powder of complete crystallization without agglomeration, comprising the following steps of:
step (1): crushing tungsten oxide powder used for industrial production by an air flow to
obtain tungsten oxide powder with a Fisher particle size of 0.5 m to 1.0 [m, wherein the
particle size of the powder is uniform, and a maximum particle size of the powder observed
under an electron microscope is 1.5 m to 3.0 [m; and step (2): carrying out hydrogen
reduction on the tungsten oxide powder obtained in step (1) through an automatic
boat-pushing four-tube furnace to obtain tungsten powder with a BET particle size of 0. 05 m
to 0.10 m. According to the invention, the uniform and ultrafine nano tungsten powder of
complete crystallization without agglomeration can be obtained by obtaining fine and uniform
tungsten powder, which is beneficial for preparing ultrafine cemented carbide products
meeting industrial requirements of a new era, and has the advantages of short process, simple
operation, low cost, non-agglomeration, uniformity and complete crystallization.
Description
The present invention belongs to the field of material preparation technologies, and
mainly relates to a method for preparing uniform and ultrafine nano tungsten powder of
complete crystallization without agglomeration.
At present, due to an excellent mechanical performance, ultrafine cemented carbide is
widely used in metal processing, electronic industry, medicine and other fields, for example,
the ultrafine cemented carbide is used as a micro drill of a printed circuit board, a milling
cutter, a cutting tool for integral hole machining, a precision tool, and a cutting tool for a
difficult-to-machine material.
Taking the application of industrial alloy in electronic industry in the new era as an
example, with the development of miniaturization, integration and precision of a circuit board,
high requirements are put forward for an organization structure of a cemented carbide material.
Therefore, the ultrafine cemented carbide is faced with the following contradictions: on one
hand, requirements of a using unit on the mechanical performance of the cemented carbide are
constantly increased, and WC grains of the cemented carbide are required to be further thinned
with a uniform organization structure; and on the other hand, due to the further thinning of the
WC grains, coarse grains are easy to be generated during sintering, which may make the
organization structure of the cemented carbide nonuniform, and the aggregation of coarse
grains and coarse particles may lead to the reduction of a strength, a wear resistance and other
related performances of the cemented carbide, which will become a source of fracture under
an action of an external force. Therefore, in order to improve a uniformity of the organization
structure of the cemented carbide, a uniformity, a stability and an activity of WC powder as a
main raw material are particularly important.
In a method for preparing ultrafine nano tungsten carbide powder commonly used in the market at present, a strong morphology inheritance from tungsten oxide - tungsten oxide- tungsten powder -- tungsten carbide leads to a large number of aggregates and a nonuniformity of a particle size. Although the aggregates are largely eliminated by processing, crystal nucleuses causing abnormal grain growth during sintering cannot be reduced.
Meanwhile, an activity of the tungsten carbide powder is increased by preprocessing, which
leads to abnormal grain growth during sintering.
However, other methods for preparing have the disadvantages of a high cost, a
complicated process and a difficulty in scale development.
The problem to be solved by the present invention is to provide a method for preparing
uniform and ultrafine nano tungsten powder of complete crystallization without agglomeration,
which has short process, simple operation, low cost.
In order to solve the above technical problem, the technical solution used in the present
invention is a method for preparing uniform and ultrafine nano tungsten powder of complete
crystallization without agglomeration, comprising the following steps of:
step (1): crushing tungsten oxide powder with a Fisher particle size of 5 m to 40 m
used for industrial production by an air flow with a pressure of 0.7 MPa to 0.8 MPa, and
adjusting appropriate technology parameters to obtain tungsten oxide powder with a Fisher
particle size of 0.5 m to 1.0 [m, wherein the particle size of the powder is uniform, and a
maximum particle size of the powder observed under an electron microscope is 1.5 m to 3.0
[tm; and
step (2): carrying out hydrogen reduction on the tungsten oxide powder obtained in step
(1) through an automatic boat-pushing four-tube furnace to obtain tungsten powder with a
BET particle size (a specific surface analysis particle size) of 0.05 m to 0.10 [m, wherein
technological parameters of the hydrogen reduction are as follows: temperatures of five bands
are 620±20°C, 680±20°C, 740±20°C, 800±20°C and 860±20°C, a hydrogen flow rate is 34
m 3/h to 40 m 3 /h, a boat pushing time is 15 minutes/boat to 20 minutes/boat, and a boat loading
capacity is 0.6 kg/boat to 0.9 kg/boat.
In step (1), uniform fine tungsten oxide powder with a Fisher particle size of 0.5 m to
1.0 m is obtained by crushing through an air flow, a rotating speed of a stepped gear of an air flow crusher and a distance between blades of the stepped gear need to be adjusted; when the rotating speed of the stepped gear is increased and the distance between the blades is reduced, the powder is finer, and the particle size of the powder is more uniform, but a crushing efficiency of the air flow crusher is reduced. The tungsten oxide is yellow tungsten W0 3 , yellow tungsten powder with a Fisher particle size of 15 m to 40 m for industrial production is crushed by air flow with a pressure of 0.7 MPa to 0.8 MPa, a crushing speed is 30 kg/h to 60 kg/h, and appropriate technology parameters are adjusted to obtain yellow tungsten powder with a Fisher particle size of 0.5 m to 1.0 m, the particle size of the powder is uniform, and a maximum particle size of the powder observed under an electron microscope is 1.5 m to 2.0 [m; hydrogen reduction is carried out on the yellow tungsten powder obtained in the above step through an automatic boat-pushing four-tube furnace to obtain tungsten powder with a BET particle size of 0.05 [m to 0.10 m; and a boat loading capacity is 0.6 kg/boat to 0.8 kg/boat. The tungsten oxide is blue tungsten W0 2 .90 , blue tungsten powder with a Fisher particle size of 15 m to 30 m used for industrial production is crushed by an air flow with a pressure of 0.7 MPa to 0.8 MPa, a crushing speed is 20 kg/h to 30 kg/h, and appropriate technology parameters are adjusted to obtain blue tungsten powder with a Fisher particle size of 0.5 m to 1.0 jm, the particle size of the powder is uniform, and a maximum particle size of the powder observed under an electron microscope is 1.5 m to 2.5 m; hydrogen reduction is carried out on the blue tungsten powder obtained in the above step through an automatic boat-pushing four-tube furnace to obtain tungsten powder with a BET particle size of 0.05 m to 0.10 m; and a boat loading capacity is 0.6 kg/boat to 0.8 kg/boat. The tungsten oxide is violet tungstenW02. 72 , violet tungsten powder with a Fisher particle size of 10 m to 20 m used for industrial production is crushed by an air flow with a pressure of 0.7 MPa to 0.8 MPa, a crushing speed is 15 kg/h to 25 kg/h, and appropriate technology parameters are adjusted to obtain violet tungsten powder with a Fisher particle size of 0.5 pm to 1.0 m, the particle size of the powder is uniform, and a maximum particle size of the powder observed under an electron microscope is 1.5 m to 3.0 m; hydrogen reduction is carried out on the violet tungsten powder obtained in the above step through an automatic boat-pushing four-tube furnace to obtain tungsten powder with a BET particle size of 0.04 m to 0.09 jm; and a boat loading capacity is 0.7 kg/boat to 0.9 kg/boat.
The tungsten oxide is tungsten dioxide W0 2 , prepared tungsten dioxide powder with a
Fisher particle size of 5 m to 20 m is crushed by an air flow with a pressure of 0.7 MPa to
0.8 MPa, a crushing speed is 35 kg/h to 45 kg/h, and appropriate technology parameters are
adjusted to obtain tungsten dioxide powder with a Fisher particle size of 0.5 m to 1.0 [m, the
particle size of the powder is uniform, and a maximum particle size of the powder observed
under an electron microscope is 1.5 m to 2.0 [m; hydrogen reduction is carried out on the
tungsten dioxide powder obtained in the above step through an automatic boat-pushing
four-tube furnace to obtain tungsten powder with a BET particle size of 0.05 m to 0.09 [m;
and a boat loading capacity is 0.6 kg/boat to 0.9 kg/boat.
Due to a strong morphology inheritance in preparation of the ultrafine nano tungsten
carbide powder, which means that a pseudo-crystal morphology of the tungsten oxide is
inherited all the time, a large number of aggregates exist in the tungsten powder and the
tungsten carbide powder, wherein a size of large aggregates is hundreds of microns, while a
size of small aggregates is several microns. Due to different sizes of the aggregates, there is a
great difference in a discharge path of water vapor in reduction of the tungsten powder, and
evaporation deposition times of the tungsten oxide are also different, which leads to a great
difference in crystallization completeness of the tungsten powder.
Therefore, if the particle size of the tungsten oxide powder is reduced by a mechanical
method, not only the morphology inheritance is prevented, but also a reducing atmosphere of
each tungsten oxide particle is almost even, which is beneficial for obtaining uniform tungsten
powder of complete crystallization.
Due to the above technical solution, the present invention overcomes the defects of
ultrafine nano tungsten powder prepared by a traditional method, such as a coarse aggregate, a
nonuniform particle size, and easy oxidization and burning after hydrogen reduction, by
obtaining the fine and uniform tungsten powder, there is no morphology inheritance problem
in reduction of the ultrafine nano tungsten powder, and meanwhile, crystallization of the
tungsten powder is more complete, so that the uniform and ultrafine nano tungsten powder of
complete crystallization without agglomeration may be obtained. The ultraine nano tungsten
carbide powder with a high uniformity, a low activity and a good stability is obtained by
carbonization, which is beneficial for preparing ultrafine cemented carbide products meeting
industrial requirements of a new era.
The present invention has the beneficial effects that: the present invention has the
advantages of short process, simple operation, low cost, non-agglomeration, uniformity and
complete crystallization.
The present invention is further described hereinafter with reference to the embodiments.
According to the embodiments of the present invention, when the tungsten oxide powder
is crushed by an air flow crusher, air flow is cooled by a compressor, a temperature after
cooling the air flow is 1°C to 4°C, and air flow crushing is a mature technology. There are
many manufacturers of the air flow crusher in China. An automatic boat-pushing four-tube
reducing furnace is also a mature device, and there are many manufacturers in China. A length
of a furnace tube of the automatic boat-pushing four-tube reducing furnace of the present
invention is 7.5 m, a size of an inner cavity is 300 mm * 70 mm, and a size of a boat is 400
mm * 270 mm * 45 mm.
Embodiment 1:
Purchased yellow tungsten powder (with a Fisher particle size of 34 m) was crushed by
air flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted,
a particle size of obtained yellow tungsten powder was 0.68 [m, and a maximum particle size
observed under an electron microscope was 1.9 [m. Reduction was carried out through an
automatic boat-pushing four-tube furnace, and a BET particle size of obtained tungsten
powder was 0.06 [m. Non-agglomeration, complete crystallization of the tungsten powder,
and a maximum particle size of 0.18 m were observed under an electron microscope.
Embodiment 2:
Purchased yellow tungsten powder (with a Fisher particle size of 30 m) was crushed by
air flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted,
a particle size of obtained yellow tungsten powder was 0.64jm, and a maximum particle size
observed under an electron microscope was 2.0 jm. Reduction was carried out through an
automatic boat-pushing four-tube furnace, and a BET particle size of obtained tungsten
powder was 0.07jm. Non-agglomeration, complete crystallization of the tungsten powder,
and a maximum particle size of 0.20 m were observed under an electron microscope.
Embodiment 3: Purchased yellow tungsten powder (with a Fisher particle size of 24 m) was crushed by air flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted, a particle size of obtained yellow tungsten powder was 0.65 [m, and a maximum particle size observed under an electron microscope was 1.5 [m. Reduction was carried out through an automatic boat-pushing four-tube furnace, and a BET particle size of obtained tungsten powder was 0.09 [m. Non-agglomeration, complete crystallization of the tungsten powder, and a maximum particle size of 0.17 m were observed under an electron microscope. Embodiment 4: Purchased blue tungsten powder (with a Fisher particle size of 26 m) was crushed by air flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted, a particle size of obtained blue tungsten powder was 0.65 [m, and a maximum particle size observed under an electron microscope was 2.4 jm. Reduction was carried out through an automatic boat-pushing four-tube furnace, a BET particle size of obtained tungsten powder was 0.06 jm, and non-agglomeration, complete crystallization of the tungsten powder, and a maximum particle size of 0.20 m were observed under an electron microscope. Embodiment 5: Purchased blue tungsten powder (with a Fisher particle size of 20 m) was crushed by air flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted, a particle size of obtained blue tungsten powder was 0.94 jm, and a maximum particle size observed under an electron microscope was 2.5 jm. Reduction was carried out through an automatic boat-pushing four-tube furnace, a BET particle size of obtained tungsten powder was 0.07 jm, and non-agglomeration, complete crystallization of the tungsten powder, and a maximum particle size of 0.18 m were observed under an electron microscope. Embodiment 6: Purchased blue tungsten powder (with a Fisher particle size of 18 m) was crushed by air flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted, a particle size of obtained blue tungsten powder was 0.81 jm, and a maximum particle size observed under an electron microscope was 2.1 jm. Reduction was carried out through an automatic boat-pushing four-tube furnace, a BET particle size of obtained tungsten powder was 0.08 jm, and non-agglomeration, complete crystallization of the tungsten powder, and a maximum particle size of 0.19 m were observed under an electron microscope.
Embodiment 7:
Prepared violet tungsten powder (with a Fisher particle size of 18 m) was crushed by air
flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted, a
particle size of obtained violet tungsten powder was 0.65 [m, and a maximum particle size
observed under an electron microscope was 2.6 [m. Reduction was carried out through an
automatic boat-pushing four-tube furnace, a BET particle size of obtained tungsten powder
was 0.05 [m, and non-agglomeration, complete crystallization of the tungsten powder, and a
maximum particle size of 0.21 m were observed under an electron microscope.
Embodiment 8:
Prepared violet tungsten powder (with a Fisher particle size of 17 m) was crushed by air
flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted, a
particle size of obtained violet tungsten powder was 0.94 [m, and a maximum particle size
observed under an electron microscope was 2.6 jm. Reduction was carried out through an
automatic boat-pushing four-tube furnace, a BET particle size of obtained tungsten powder
was 0.06 jm, and non-agglomeration, complete crystallization of the tungsten powder, and a
maximum particle size of 0.18 m were observed under an electron microscope.
Embodiment 9:
Prepared violet tungsten powder (with a Fisher particle size of 15 m) was crushed by air
flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted, a
particle size of obtained violet tungsten powder was 0.81 jm, and a maximum particle size
observed under an electron microscope was 2.0 jm. Reduction was carried out through an
automatic boat-pushing four-tube furnace, a BET particle size of obtained tungsten powder
was 0.04 jm, and non-agglomeration, complete crystallization of the tungsten powder, and a
maximum particle size of 0.16 m were observed under an electron microscope.
Embodiment 10:
Prepared tungsten dioxide powder (with a Fisher particle size of 13 m) was crushed by
air flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted,
a particle size of obtained tungsten dioxide powder was 0.61 jm, and a maximum particle size
observed under an electron microscope was 1.8 jm. Reduction was carried out through an
automatic boat-pushing four-tube furnace, a BET particle size of obtained tungsten powder was 0.05 [m, and non-agglomeration, complete crystallization of the tungsten powder, and a maximum particle size of 0.16 m were observed under an electron microscope. Embodiment 11: Prepared tungsten dioxide powder (with a Fisher particle size of 10 m) was crushed by air flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted, a particle size of obtained tungsten dioxide powder was 0.71 [m, and a maximum particle size observed under an electron microscope was 1.4 [m. Reduction was carried out through an automatic boat-pushing four-tube furnace, a BET particle size of obtained tungsten powder was 0.06 [m, and non-agglomeration, complete crystallization of the tungsten powder, and a maximum particle size of 0.18 m were observed under an electron microscope. Embodiment 12: Prepared tungsten dioxide powder (with a Fisher particle size of 8 m) was crushed by air flow with an air flow pressure of 0.8 MPa, a rotating speed of a stepped gear was adjusted, a particle size of obtained tungsten dioxide powder was 0.75 jm, and a maximum particle size observed under an electron microscope was 2.0 jm. Reduction was carried out through an automatic boat-pushing four-tube furnace, a BET particle size of obtained tungsten powder was 0.07 jm, and non-agglomeration, complete crystallization of the tungsten powder, and a maximum particle size of 0.15 m were observed under an electron microscope. The foregoing describes the embodiments of the present invention in detail, but the contents are only the preferred embodiments of the present invention, which cannot be regarded as limiting the implementation scope of the present invention. All equal changes and improvements made according to the scope of the present invention shall still fall within the coverage scope of the patent of the present invention.
Claims (6)
1. A method for preparing uniform and ultrafine nano tungsten powder of complete crystallization without agglomeration, comprising the following steps of: step (1): crushing tungsten oxide powder with a Fisher particle size of 5 m to 40 m used for industrial production by an air flow with a pressure of 0.7 MPa to 0.8 MPa to obtain tungsten oxide powder with a Fisher particle size of 0.5 m to 1.0 m, wherein the particle size of the powder is uniform, and a maximum particle size of the powder observed under an electron microscope is 1.5 m to 3.0 [m; and step (2): carrying out hydrogen reduction on the tungsten oxide powder obtained in step (1) through an automatic boat-pushing four-tube furnace to obtain tungsten powder with a BET particle size of 0.05 m to 0.10 m, wherein technological parameters of the hydrogen reduction are as follows: temperatures of five bands are 620±20°C, 680±20°C, 740±20°C, 800±20°C and 860±20°C, a hydrogen flow rate is 34 m 3/h to 40 m3 /h, a boat pushing time is minutes/boat to 20 minutes/boat, and a boat loading capacity is 0.6 kg/boat to 0.9 kg/boat.
2. The method for preparing uniform and ultrafine nano tungsten powder of complete crystallization without agglomeration according to claim 1, wherein the tungsten oxide is yellow tungsten W03 , yellow tungsten powder with a Fisher particle size of 15 m to 40 m for industrial production is crushed by air flow with a pressure of 0.7 MPa to 0.8 MPa to obtain yellow tungsten powder with a Fisher particle size of 0.5 m to 1.0 m, the particle size of the powder is uniform, and a maximum particle size of the powder observed under an electron microscope is 1.5 m to 2.0jm; hydrogen reduction is carried out on the yellow tungsten powder obtained in the above step through an automatic boat-pushing four-tube furnace to obtain tungsten powder with a BET particle size of 0.05 m to 0.10 m; and a boat loading capacity is 0.6 kg/boat to 0.8 kg/boat.
3. The method for preparing uniform and ultrafine nano tungsten powder of complete crystallization without agglomeration according to claim 1, wherein the tungsten oxide is blue tungsten W02.90 , blue tungsten powder with a Fisher particle size of 15 m to 30 m used for industrial production is crushed by an air flow with a pressure of 0.7 MPa to 0.8 MPa to obtain blue tungsten powder with a Fisher particle size of 0.5 m to 1.0jm, the particle size of the powder is uniform, and a maximum particle size of the powder observed under an electron microscope is 1.5 m to 2.5jm; hydrogen reduction is carried out on the blue tungsten powder obtained in the above step through an automatic boat-pushing four-tube furnace to obtain tungsten powder with a BET particle size of 0.05 m to 0.10 [m; and a boat loading capacity is 0.6 kg/boat to 0.8 kg/boat.
4. The method for preparing uniform and ultrafine nano tungsten powder of complete crystallization without agglomeration according to claim 1, wherein the tungsten oxide is violet tungstenW0 2.72, violet tungsten powder with a Fisher particle size of 10 m to 20 m used for industrial production is crushed by an air flow with a pressure of 0.7 MPa to 0.8 MPa to obtain violet tungsten powder with a Fisher particle size of 0.5 m to 1.0 [m, the particle size of the powder is uniform, and a maximum particle size of the powder observed under an electron microscope is 1.5 m to 3.0 jm; hydrogen reduction is carried out on the violet tungsten powder obtained in the above step through an automatic boat-pushing four-tube furnace to obtain tungsten powder with a BET particle size of 0.04 m to 0.09 jm; and a boat loading capacity is 0.7 kg/boat to 0.9 kg/boat.
5. The method for preparing uniform and ultrafine nano tungsten powder of complete crystallization without agglomeration according to claim 1, wherein the tungsten oxide is tungsten dioxideW0 2,prepared tungsten dioxide powder with a Fisher particle size of 5 m to m is crushed by an air flow with a pressure of 0.7 MPa to 0.8 MPa to obtain tungsten dioxide powder with a Fisher particle size of 0.5 m to 1.0jm, the particle size of the powder is uniform, and a maximum particle size of the powder observed under an electron microscope is 1.5 m to 2.0 m; hydrogen reduction is carried out on the tungsten dioxide powder obtained in the above step through an automatic boat-pushing four-tube furnace to obtain tungsten powder with a BET particle size of 0.05 m to 0.09 m; and a boat loading capacity is 0.6 kg/boat to 0.9 kg/boat.
6. The method for preparing uniform and ultrafine nano tungsten powder of complete crystallization without agglomeration according to any one of claims 1 to 5, wherein uniform fine powder with a Fisher particle size of 0.5 m to 1.0 m is obtained by crushing through an air flow, a rotating speed of a stepped gear of an air flow crusher and a distance between blades of the stepped gear need to be adjusted; when the rotating speed of the stepped gear is increased and the distance between the blades is reduced, the powder is finer, and the particle size of the powder is more uniform, but a crushing efficiency of the air flow crusher is reduced.
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| CN113929099A (en) * | 2021-10-27 | 2022-01-14 | 赣州海盛钨钼集团有限公司 | Preparation method of superfine tungsten carbide powder |
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| CN113929099A (en) * | 2021-10-27 | 2022-01-14 | 赣州海盛钨钼集团有限公司 | Preparation method of superfine tungsten carbide powder |
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