CN108455614A - A kind of method that low temperature, short route prepare nano WC powder - Google Patents
A kind of method that low temperature, short route prepare nano WC powder Download PDFInfo
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- CN108455614A CN108455614A CN201810126042.8A CN201810126042A CN108455614A CN 108455614 A CN108455614 A CN 108455614A CN 201810126042 A CN201810126042 A CN 201810126042A CN 108455614 A CN108455614 A CN 108455614A
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- C01P2002/00—Crystal-structural characteristics
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Abstract
The invention discloses a kind of methods that low temperature, short route prepare nano WC powder, it is using water-soluble ammonium metatungstate and glucose as raw material, ammonium dichromate and ammonium metavanadate are added as inhibitor, raw material and inhibitor are added in pure water, heating stirring is uniform, then spray-dried, calcining and reduction and carbonization process, obtain target product nano WC powder.Nano WC powder performance prepared by the present invention is stable, object is mutually single, ingredient is uniform, narrow particle size distribution, crystal grain are tiny, powdered ingredients are easy to control, and has industrialization, mass production ability.
Description
Technical field
The invention belongs to the preparation methods that a kind of nanometer/ultra-fine cemented carbide produces raw materials used powder, and in particular to one
The method that kind prepares nanometer tungsten carbide (WC) powder using water soluble method, low temperature, short route.The nanometer WC powder prepared using this method
End can be applied to dot-matrix printer drill bit, integrated circuit board microbit, NC machining drill bit and milling cutter, medical tooth
Brill, difficult-to-machine material cutter etc..
Background technology
As modern rapidoprint is constantly to high-end aluminium alloy, titanium alloy, magnesium alloy, high property copper alloy, stainless steel, non-
The appearance and application of brilliant Materials and various difficult-to-machine materials, and add along with Advanced Manufacturing System, high-speed cutting, ultraprecise
Work, green manufacturing development, promote cutter material to develop towards high-performance direction.
Hard alloy is commonly called as " industrial tooth ", since it is swollen with high intensity, high rigidity, high-wearing feature, low heat
Swollen coefficient, high elasticity modulus and good chemical stability so that it is in modern tool material, wear-resistant material, corrosion-resistant
It is occupied an important position with heat-resisting material etc., is widely used in wire-drawing die, machinery in all fields of national economy
Processing, material cutting, mining drill bit, wear resistant corrosion resistant part and structure member etc..
Sintered carbide tool material belongs to cermet material, is fragile material, intensity and hardness (toughness and wear-resisting
Property) between contradiction (intensity is high, and hardness is low；Intensity is low, and hard is high) it is always the principal element for perplexing its development.For a long time with
Come, people have carried out unremitting effort, such as adjust alloying component, improve alloy structure, addition trace element, using new work
The a series of measures such as skill equipment, it is intended to which harmonious contradiction between the two is allowed to organically combine, and is always the direction that people make great efforts.
The study found that under the premise of cobalt content is constant, when WC grain degree drops to 1 μm or less, hard alloy it is hard
Degree, intensity improve simultaneously, and as WC grain degree further decreases, performance is more excellent, for solution Cemented Carbide Hardness and by force
Contradiction between degree has found a new way.It can be seen that significantly improving for Cemented Carbide Properties can be by keeping chemistry
Reduce microstructure scale while ingredient and uniform microstructure to realize.
It is to use nano WC powder to want preparing nano structure hard alloy, precondition.Conventionally produced WC powder
It is since prepared by ammonium paratungstate (APT), object phase transition is：APT → tungsten oxide → tungsten (W) powder → WC powder, i.e.,：With APT
Tungsten oxide is produced using rotary kiln for raw material, then tungsten oxide is reduced by W powder using reduction furnace, W powder passes through mixed with carbon black, ball milling
Material, >=1300 DEG C of reduction and carbonization stoves prepare ultra-fine/nano WC powder.Conventionally produced nano WC powder it is the most key be
The production of tungsten oxide powder, there are four types of the tungsten oxides of APT calcination-reductions production, and form is (yellow tungsten WO3, blue tungsten WO2.9, purple tungsten
WO2.72, brown tungsten WO2), at present nano WC powder, powder grain degree≤200nm can be produced only with purple tungsten.Because of APT calcinings-
Also original production WO2.72Harsh to equipment, environmental requirement, control is improper, is easy to generate WO3、WO2.9、WO2.72、WO2Compound, and
WO2.72It is thinner to be reduced into W Powder Particle Sizes, easily oxidation and spontaneous combustion, reduction controls improper W powder and is easy to grow up.Meanwhile W in carbonisation
Powder and lighter carbon black are easy to mix uneven, and reduction and carbonization be easy to cause component segregation.
Invention content
For the shortcoming present in existing nano WC powder production technology, the present invention is intended to provide a kind of low temperature, short
The method that flow prepares nano WC powder, problem to solve is that：Avoid APT calcination-reductions formed a variety of tungsten oxides,
WO2.72It is reduced into W powder easily oxidation and spontaneous combustion, reduction and controls that improper W powder crystals grain is easy to grow up, W powder is mixed with carbon black and be easy to cause
Component segregation.
The present invention is to realize goal of the invention, is adopted the following technical scheme that：
The invention discloses a kind of method that low temperature, short route prepare nano WC powder, feature is：It is with water solubility
Ammonium metatungstate and glucose are raw material, add ammonium dichromate and ammonium metavanadate as inhibitor, raw material and inhibitor are added pure
In water, heating stirring is uniform, and then spray-dried, calcining and reduction and carbonization process obtain target product nano WC powder.Tool
Body includes the following steps：
1) dispensing
According to mass percentage be water-soluble ammonium metatungstate 60~70%, glucose 29~38%, ammonium metavanadate 0.1~
1.0%, the ratio of ammonium dichromate 0.1~1.0% carries out dispensing；
Each material is added in the pure water for accounting for 0.4~1.5 times of material gross mass, 50~100 DEG C stir evenly, and obtain pH
=1~5 mixed slurry；
2) it is spray-dried
By mixed slurry obtained by step 1) by atomizer drying, obtain spherical presoma composite powder, it is described from
Core type spray drying condition be：Inlet air temperature is 180~260 DEG C, and leaving air temp is 80~150 DEG C, atomizer rotating speed 10000
~15000r/min, 2~4kg/min of feed rate；
3) it calcines
By spherical presoma composite powder obtained by step 2) under the conditions of 450~650 DEG C, be passed through nitrogen calcining 30~
90min, then keep spherical shell broken through dry ball milling, obtain carbon-coated nano WO3Powder；
4) reduction and carbonization
By carbon-coated nano WO obtained by step 3)3Powder is passed through in 850~1250 DEG C of conditions by H2With CH4By volume
(90~99)：(1~10) the gaseous mixture constituted, 30~120min of reduction and carbonization obtain target product nano WC powder.
Compared with the prior art, beneficial effects of the present invention are embodied in：
1, ammonium metatungstate and glucose sugar are mixed with slurry by the present invention with solwution method, and tungsten, carbon atom is made to reach molecular water
Flat uniform mixing, and hig h-speed centrifugal spray drying is used to provide premise, and gained precursor spherical powder to prepare nanometer powder
The large specific surface area at end reduces W atoms, C atoms form the reduction and carbonization temperature of WC powder.Ammonium metatungstate and glucose sugar are sprayed
Precursor composite powder prepared by mist drying, can mutually single, the pure WO of formation through calcining3, avoid APT calcination-reductions
It is easy to be formed a variety of tungsten oxides in the process and the problems such as tungsten oxide is reduced into tungsten powder spontaneous combustion, crystal grain is grown up, not easy to control.Meanwhile
The WO formed after calcining3In-situ reactive synthesis nanometer WC composite powders occur at low temperature with activated carbon, avoid traditional handicraft W
Powder mixed with carbon black it is uneven caused by component segregation and dirtyization.
2, preparation process flow of the present invention is short, simple for process, process is few, low to equipment and environmental requirement, is more advantageous to and receives
The quality control of rice tungsten-carbide powder.
3, nano WC powder performance prepared by the present invention is stable, object is mutually single, ingredient is uniform, narrow particle size distribution, crystal grain are thin
Small, powdered ingredients are easy to control, and have industrialization, mass production ability.
Description of the drawings
Fig. 1 is the preparation flow schematic diagram of nano WC powder of the present invention；
Fig. 2 is the SEM photograph for the presoma composite powder that the embodiment of the present invention 2 obtains；
Fig. 3 is the carbon-coated nano WO that the embodiment of the present invention 2 obtains3The SEM photograph of powder；
Fig. 4 is the carbon-coated nano WO that the embodiment of the present invention 2 obtains3The XRD photos of powder
Fig. 5 is the SEM photograph for the nano WC powder that the embodiment of the present invention 2 obtains；
Fig. 6 is the XRD photos for the nano WC powder that the embodiment of the present invention 2 obtains；
Fig. 7 is the SEM elemental map photos for the nano WC powder that implementation column 2 of the present invention obtains, wherein：(a) WC powder；
(b) W elements；(c) C element.
Specific implementation mode
It elaborates below in conjunction with the accompanying drawings to the embodiment of the present invention, following embodiments are being with technical solution of the present invention
Under the premise of implemented, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to
Following embodiments.
Embodiment 1
The present embodiment prepares nano WC powder as follows：
1) dispensing
100Kg water solubilitys ammonium metatungstate, 54Kg glucose, 0.6Kg ammonium metavanadates and 0.9Kg ammonium dichromates are dissolved in quality
Be 1.0 times of solid gross mass pure water in, 80 DEG C stir evenly, and obtain the mixed slurry of pH=4；
2) it is spray-dried
By mixed slurry obtained by step 1) by atomizer drying, obtain spherical presoma composite powder, it is described from
Core type spray drying condition be：Inlet air temperature is 260 DEG C, and leaving air temp is 140 DEG C, atomizer rotating speed 15000r/min, into
Expect rate 3.4kg/min；
3) it calcines
By spherical presoma composite powder obtained by step 2) under the conditions of 600 DEG C, it is passed through nitrogen calcining 60min, then through dry
Method ball milling keeps spherical shell broken, obtains carbon-coated nano WO3Powder；
4) reduction and carbonization
By carbon-coated nano WO obtained by step 3)3Powder is under the conditions of 1200 DEG C, in H2:CH4(volume ratio)=98.5:1.5
Atmosphere under carry out reduction and carbonization 60min, obtain nano WC powder.
The present embodiment has detected the physical property and chemical composition of gained nano WC powder, and the results are shown in Table 1.
Embodiment 2
The present embodiment prepares nano WC powder as follows：
1) dispensing
100Kg water solubilitys ammonium metatungstate, 49Kg glucose, 0.4Kg ammonium metavanadates and 0.8Kg ammonium dichromates are dissolved in quality
Be 0.6 times of solid gross mass pure water in, 60 DEG C stir evenly, and obtain the mixed slurry of pH=3.2；
2) it is spray-dried
Mixed slurry obtained by step 1) is dried by atomizer, obtains presoma composite powder, it is described centrifugal
The condition of spray drying is：Inlet air temperature is 260 DEG C, and leaving air temp is 120 DEG C, atomizer rotating speed 12000r/min, charging speed
Rate 3.0kg/min；
Electron microscope analysis is scanned to presoma composite powder obtained by the present embodiment, the results are shown in Figure 2, it can be seen that institute
It is chondritic to obtain presoma composite powder, and sphericity is high, broken few, and mobility is preferable.
3) it calcines
By spherical presoma composite powder obtained by step 2) under the conditions of 550 DEG C, it is passed through nitrogen calcining 60min, then through dry
Method ball milling keeps spherical shell broken, obtains carbon-coated nano WO3Powder；
To carbon-coated nano WO obtained by the present embodiment3Powder is scanned electron microscope analysis, and the results are shown in Figure 3, can see
Go out gained carbon-coated nano tungsten oxide powder to be easily broken and be crushed uniformly through ball milling, can increase sintered surface through ball mill crushing, drop
Low porosity).
To carbon-coated nano WO obtained by the present embodiment3Powder carries out X-ray diffraction analysis, and the results are shown in Figure 4, can be with
Find out that gained carbon-coated nano tungsten oxide powder is WO3, object is mutually pure, single, and does not occur other tungsten oxide phases in powder
WO2.9、WO2.72、WO2。
4) reduction and carbonization
By step 3) gained carbon-coated nano tungsten oxide powder under the conditions of 1150 DEG C, in H2:CH4(volume ratio)=97.5:
Reduction and carbonization 100min is carried out under 2.5 atmosphere, obtains nano WC powder.
Electron microscope analysis is scanned to nano WC powder obtained by the present embodiment, the results are shown in Figure 5, it can be seen that gained is received
Rice WC powder grain size is uniform, and crystal grain is small, mean grain size 60nm..
X-ray diffraction analysis is carried out to nano WC powder obtained by the present embodiment, the results are shown in Figure 6, it can be seen that gained
Nano WC powder carbonization is complete, object is mutually pure, is simple substance WC phases, does not occur scarce carbon phase (W2C、W3C、W)。
Field emission scanning electron microscope is carried out to nano WC powder obtained by the present embodiment and amplifies 10000 times of lower elemental maps point
Analysis, the results are shown in Figure 7, it can be seen that gained nano WC powder W, C element are evenly distributed.
The present embodiment tests the physical property and chemical composition of gained nano WC powder, and the results are shown in Table 1.
Embodiment 3
The present embodiment prepares nano WC powder as follows：
1) dispensing
100Kg water solubilitys ammonium metatungstate, 46Kg glucose, 0.3Kg ammonium metavanadates and 0.9Kg ammonium dichromates are dissolved in quality
Be 0.8 times of solid gross mass pure water in ,=70 DEG C stir evenly, and obtain the mixed slurry of pH=3.4；
2) it is spray-dried
By mixed slurry obtained by step 1) by atomizer drying, obtain spherical presoma composite powder, it is described from
Core type spray drying condition be：Inlet air temperature is 260 DEG C, and leaving air temp is 115 DEG C, atomizer rotating speed 10000r/min, into
Expect rate 2.8kg/min；
3) it calcines
By spherical presoma composite powder obtained by step 2) under the conditions of 500 DEG C, it is passed through nitrogen calcining 80min, then through dry
Method ball milling keeps spherical shell broken, obtains carbon-coated nano WO3Powder；
4) reduction and carbonization
By carbon-coated nano WO obtained by step 3)3Powder is under the conditions of 1100 DEG C, in H2:CH4(volume ratio)=94.5:5.5
Atmosphere under carry out reduction and carbonization 120min, obtain nano WC powder.
The present embodiment has detected the physical property and chemical composition of gained nano WC powder, and the results are shown in Table 1.
The physical property and chemical composition for the nano WC powder that 1 various embodiments of the present invention of table obtain
As can be seen from Table 1, the present invention is prepared nano WC powder specific surface area is larger, apparent density is relatively low, grain
Degree distribution is wider, and the later stage is crushed partition size range by narrow distribution through air-flow；And the nanometer WC that the present invention is prepared
Oxygen content is relatively low in powder, and free carbon content is relatively low.
It these are only exemplary embodiment of the present invention, be not intended to limit the invention, all spirit in the present invention
With within principle made by all any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention.
Claims (2)
1. a kind of method that low temperature, short route prepare nano WC powder, it is characterised in that：It is with water-soluble ammonium metatungstate and grape
Sugar is raw material, adds ammonium dichromate and ammonium metavanadate as inhibitor, raw material and inhibitor is added in pure water, heating stirring is equal
Even, then spray-dried, calcining and reduction and carbonization process obtain target product nano WC powder.
2. the method that low temperature according to claim 1, short route prepare nano WC powder, which is characterized in that including as follows
Step：
1) dispensing
According to mass percentage be water-soluble ammonium metatungstate 60~70%, glucose 29~38%, ammonium metavanadate 0.1~
1.0%, ammonium dichromate 0.1~1.0% carries out dispensing；
Each material is added in the pure water for accounting for 0.4~1.5 times of material gross mass, 50~100 DEG C stir evenly, and obtain pH=1
~5 mixed slurry；
2) it is spray-dried
Mixed slurry obtained by step 1) is dried by atomizer, obtains spherical presoma composite powder, it is described centrifugal
The condition of spray drying is：Inlet air temperature is 180~260 DEG C, and leaving air temp is 80~150 DEG C, atomizer rotating speed 10000~
15000r/min, 2~4kg/min of feed rate；
3) it calcines
By spherical presoma composite powder obtained by step 2) under the conditions of 450~650 DEG C, it is passed through nitrogen and calcines 30~90min, then
Keep spherical shell broken through dry ball milling, obtains carbon-coated nano WO3Powder；
4) reduction and carbonization
By carbon-coated nano WO obtained by step 3)3Powder is passed through in 850~1250 DEG C of conditions by H2With CH4By volume (90~
99)：(1~10) the gaseous mixture constituted, 30~120min of reduction and carbonization obtain target product nano WC powder.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108675299A (en) * | 2018-08-30 | 2018-10-19 | 浙江德威硬质合金制造有限公司 | Low temperature synthesizes the preparation method of WC |
| CN109055796A (en) * | 2018-08-30 | 2018-12-21 | 浙江德威硬质合金制造有限公司 | Low temperature synthesis WC is the method that raw material produce hard alloy |
| CN109128141A (en) * | 2018-09-30 | 2019-01-04 | 合肥工业大学 | A kind of preparation method of nanometer WC-Co composite powder |
| CN110029261A (en) * | 2019-05-10 | 2019-07-19 | 重庆文理学院 | A kind of preparation method of Micro-Nano Hardmetal cutter material |
| CN110817879A (en) * | 2019-12-04 | 2020-02-21 | 北京科技大学 | Method for synthesizing nano WC powder by using carbon thermal reduction combustion precursor |
| CN112408485A (en) * | 2020-11-26 | 2021-02-26 | 江西理工大学 | Method for preparing tungsten oxide with array micro/nano structure |
| CN113184853A (en) * | 2021-05-26 | 2021-07-30 | 崇义章源钨业股份有限公司 | Superfine tungsten carbide powder and preparation method and application thereof |
| CN117845088A (en) * | 2024-03-06 | 2024-04-09 | 崇义章源钨业股份有限公司 | Binding phase-free hard alloy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108675299A (en) * | 2018-08-30 | 2018-10-19 | 浙江德威硬质合金制造有限公司 | Low temperature synthesizes the preparation method of WC |
| CN109055796A (en) * | 2018-08-30 | 2018-12-21 | 浙江德威硬质合金制造有限公司 | Low temperature synthesis WC is the method that raw material produce hard alloy |
| CN109128141A (en) * | 2018-09-30 | 2019-01-04 | 合肥工业大学 | A kind of preparation method of nanometer WC-Co composite powder |
| CN110029261A (en) * | 2019-05-10 | 2019-07-19 | 重庆文理学院 | A kind of preparation method of Micro-Nano Hardmetal cutter material |
| CN110029261B (en) * | 2019-05-10 | 2020-07-14 | 重庆文理学院 | Preparation method of micro-nano hard alloy cutter material |
| CN110817879A (en) * | 2019-12-04 | 2020-02-21 | 北京科技大学 | Method for synthesizing nano WC powder by using carbon thermal reduction combustion precursor |
| CN110817879B (en) * | 2019-12-04 | 2021-06-18 | 北京科技大学 | Method for synthesizing nano WC powder by using carbon thermal reduction combustion precursor |
| CN112408485A (en) * | 2020-11-26 | 2021-02-26 | 江西理工大学 | Method for preparing tungsten oxide with array micro/nano structure |
| CN112408485B (en) * | 2020-11-26 | 2023-02-03 | 江西理工大学 | Method for preparing tungsten oxide with array micro/nano structure |
| CN113184853A (en) * | 2021-05-26 | 2021-07-30 | 崇义章源钨业股份有限公司 | Superfine tungsten carbide powder and preparation method and application thereof |
| CN117845088A (en) * | 2024-03-06 | 2024-04-09 | 崇义章源钨业股份有限公司 | Binding phase-free hard alloy and preparation method thereof |
| CN117845088B (en) * | 2024-03-06 | 2024-05-28 | 崇义章源钨业股份有限公司 | Binding phase-free hard alloy and preparation method thereof |
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