CN107199346B - A kind of industrialized preparation method of nano W/WC composite powder - Google Patents
A kind of industrialized preparation method of nano W/WC composite powder Download PDFInfo
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- CN107199346B CN107199346B CN201710453108.XA CN201710453108A CN107199346B CN 107199346 B CN107199346 B CN 107199346B CN 201710453108 A CN201710453108 A CN 201710453108A CN 107199346 B CN107199346 B CN 107199346B
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- 239000000843 powder Substances 0.000 title claims abstract description 70
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 31
- 239000008103 glucose Substances 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 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 15
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000004615 ingredient Substances 0.000 claims abstract description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract 2
- 239000010941 cobalt Substances 0.000 claims description 11
- 229910017052 cobalt Inorganic materials 0.000 claims description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 11
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 23
- 239000002245 particle Substances 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 7
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 5
- 239000002114 nanocomposite Substances 0.000 abstract description 4
- 238000000713 high-energy ball milling Methods 0.000 abstract description 3
- 239000003870 refractory metal Substances 0.000 abstract description 2
- 238000004663 powder metallurgy Methods 0.000 abstract 1
- 229910052721 tungsten Inorganic materials 0.000 description 16
- 239000010937 tungsten Substances 0.000 description 16
- 238000004321 preservation Methods 0.000 description 10
- 238000002156 mixing Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 238000010792 warming Methods 0.000 description 7
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000956 alloy Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 241000219095 Vitis Species 0.000 description 2
- 235000009754 Vitis X bourquina Nutrition 0.000 description 2
- 235000012333 Vitis X labruscana Nutrition 0.000 description 2
- 235000014787 Vitis vinifera Nutrition 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 229910009043 WC-Co Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
-
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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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- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
一种纳米W/WC复合粉末的工业化制备方法，属于难熔金属和粉末冶金技术领域。以钨氧化物、钴氧化物和葡萄糖为原料，按照钴氧化物：钨氧化物：葡萄糖的质量比为1：(10～85)：(4.5～43)进行配料，首先对钨氧化物、钴氧化物进行高能球磨；然后加入葡萄糖粉末和无水乙醇进行二次球磨；置于真空炉中进行反应，炉内真空度小于10Pa，首先加热至150～180℃保温15～60min，再升温至350～500℃保温2～4h，最后升温至850～1100℃保温2～5h。最后得到钨粉基体上分布碳化钨粉末的纳米复合粉体。所生成的钨粉平均粒径可达几十纳米以下，且粉末粒径分布均匀。
An industrialized preparation method of nano W/WC composite powder belongs to the technical field of refractory metals and powder metallurgy. Using tungsten oxide, cobalt oxide and glucose as raw materials, according to the mass ratio of cobalt oxide:tungsten oxide:glucose is 1:(10～85):(4.5～43), the ingredients are firstly mixed with tungsten oxide, cobalt oxide and tungsten oxide. The oxide is subjected to high-energy ball milling; then glucose powder and absolute ethanol are added for secondary ball milling; the reaction is carried out in a vacuum furnace, the vacuum degree in the furnace is less than 10Pa, firstly heated to 150～180℃ for 15～60min, and then heated to 350 ～500℃ for 2～4h, and finally heat up to 850～1100℃ for 2～5h. Finally, a nanocomposite powder in which the tungsten carbide powder is distributed on the tungsten powder matrix is obtained. The average particle size of the generated tungsten powder can reach several tens of nanometers or less, and the particle size distribution of the powder is uniform.
Description
Technical field
The present invention relates to a kind of W powder for quickly preparing nanoscale be matrix, the W/WC of a small amount of WC powder Dispersed precipitate is answered
The industrialized process for preparing for closing powder, belongs to refractory metal and powder metallurgical technology.
Background technique
Tungsten is because having high density, high-melting-point, low thermal coefficient of expansion, excellent electrical and thermal conductivity performance and good corrosion-resistant
Performance and be widely used in industrial circle.Using tungsten or its carbide as the composite material of matrix, such as: WC-Co hard alloy, W-
Ni-Fe high-density alloy, W-Cu alloy etc. have become the indispensable important materials of many high-tech areas, such as microelectronics work
Industry, fine chemistry industry, sufacing, aerospace etc..The performance of tungsten-bast alloy and the performance of W powder are closely related.As of tungsten powder
When particle size is reduced to ultra-fine and nanoscale, good sintering characteristic, the block of preparation are shown with the tungsten-bast alloy that it is prepared
Body material has high toughness, compressive strength, thermal shock resistance etc..However, the skill of the nano-tungsten powder of China's mass production at present
Art is still immature, and the enterprise of external only a few countries can produce nano-tungsten powder.Therefore, break and controlled by external a small number of manufacturers
The situation in international nano-tungsten powder and Related product market is made, it is particularly important for preparing nano-tungsten powder with independent intellectual property rights
R&D direction.
Further, since the brittleness of tungsten is larger, integral strength and wearability are poor；And stable carbide (WC) tool of tungsten
There is the advantages of high rigidity, high-wearing feature, high corrosion-resistant, therefore, Dispersed precipitate nano WC powder particle is formed in nano-tungsten powder
W/WC composite granule, for enhancing the room temperature and mechanical behavior under high temperature, expansion engineer application field, the important dress of raising of tungsten-bast alloy
Standby service life has key effect.
Summary of the invention
The present invention be for current nano-tungsten powder and Related product in the industrial production the technical issues of, provide one kind
The industrialized process for preparing of simple and easy to control, strong operability nanometer W/WC composite powder.
The method of preparation nanometer W/WC composite powder provided by the invention, which comprises the following steps:
(1) using tungsten oxide, cobalt/cobalt oxide and glucose as raw material, according to cobalt/cobalt oxide: tungsten oxide: the matter of glucose
Amount than be 1:(10~85): (4.5~43) carry out ingredient, first to tungsten oxide, cobalt/cobalt oxide carry out high-energy ball milling, abrading-ball with
Powder quality ratio is 3:1~10:1, and using dehydrated alcohol as abrasive media, abrasive media and volume of material ratio are 1:1, and ball mill turns
Speed is 100~500r/min, and Ball-milling Time is 60~80h.
(2) glucose powder is added in the mixed powder that step (1) obtains, and is incorporated the nothing with the isometric ratio of glucose
Water-ethanol carries out secondary ball milling, and rotational speed of ball-mill is 50~80r/min, and Ball-milling Time is 10~20h.
(3) powder that step (2) obtains is placed in vacuum drying oven and is reacted, in furnace vacuum degree be less than 10Pa, first plus
Heat is to 150~180 DEG C of 15~60min of heat preservation, then is warming up to 350~500 DEG C of 2~4h of heat preservation, is finally warming up to 850~1100 DEG C
Keep the temperature 2~5h.
Molal quantity of the molal quantity of carbon greater than oxygen in tungsten oxide, cobalt/cobalt oxide in general glucose.
The process flow of this method and principle are: using tungsten oxide, cobalt/cobalt oxide and glucose powder as raw material, using point
After oxide powder particle is first sufficiently milled to nanoscale by step ball-milling technology, glucose powder is added at the low rotational speed and carries out ball
Mill mixing is decomposed in Process During High Energy Ball Milling to avoid glucose, then mixed-powder is placed under vacuum condition and carries out in-situ reducing
Carburizing reagent.It is first heated to glucose fusing and decomposition temperature in reaction process, there is very high surface using nanometer powder
Can, in the spontaneous cladding of nano-oxide particle surface after glucose fusing；In addition, after breakdown of glucose temperature, carbon source
It is evenly distributed in oxide powder particle surface.At a temperature of reduction and carbonization, the oxide of tungsten and the oxide of cobalt are reduced
At tungsten, cobalt, and by the acceleration diffusion of cobalt, part tungsten is carbonized to form tungsten carbide, finally obtains and is distributed on tungsten powder matrix
The composite nano-powder of tungsten-carbide powder.
It is an object of that present invention to provide a kind of systems for the composite powder that tungsten carbide is distributed on nanometer tungsten basal body simple and easy to control
Preparation Method is suitable for industrialized production.
Characteristic and advantage of the invention is as follows:
The method for industrially preparing tungsten powder at present mainly passes through H2、CH4Or the gases such as Co carry out high temperature to tungsten oxide powder
, however, tungsten powder granularity obtained by these methods is coarse, and there is considerable risk using above-mentioned reducibility gas in reduction
Property.The present invention compared with these preparation methods, advantage be tungsten powder average grain diameter generated up to tens nanometers hereinafter, and
Powder diameter is evenly distributed；Carbon is generated when glucose reaches decomposition temperature and water vapour, product are safe and environment-friendly.Utilize grape
The characteristics of may occur from body fusing under sugared low temperature, coats oxide, the strong reduction reaction for promoting tungsten oxide.Together
When, by the facilitation that cobalt is carbonized to tungsten, (1000 DEG C of <) produces nano WC powder Dispersed precipitate at a lower temperature
In the composite powder material of nano-tungsten powder, and cobalt is present in composite powder in the form of a small amount of W-Co-C ternary phase.In this method
The partial size of tungsten and tungsten-carbide powder, respective proportion and tungsten carbide production rate etc., can be by reaction temperature and time, original
Glucose content and cobalt oxide content etc. are designed and accurately regulate and control in feed powder.
Detailed description of the invention
The shape appearance figure of gained powder after raw material ball mill mixes in Fig. 1 embodiment of the present invention 1.
Raw material ball grinds shape appearance figure of the mixed powder after glucose coats in Fig. 2 embodiment of the present invention 1.
The shape appearance figure and grain size distribution for the W/WC composite powder that Fig. 3 embodiment of the present invention 2 is prepared, wherein a is real
Apply the displaing micro tissue topography for the tungsten base composite powder that example 2 is prepared；B is the particle size for the composite powder that embodiment 2 is prepared
Distribution map.
The material phase analysis figure for the tungsten base composite powder that Fig. 4 embodiment of the present invention 3 is prepared.
Specific embodiment
Following embodiment further illustrates the present invention, but the present invention is not limited to following embodiments.
Embodiment 1
Weigh 1 kilogram of WO3, 0.012 kilogram of Co3O4With 0.43 kilogram of glucose (C6H12O6), first by WO2.9、Co3O4With
Dehydrated alcohol carries out ball milling mixing, and abrading-ball and powder quality ratio are 10:1, and dehydrated alcohol and volume of material ratio are 1:1, ball mill
Revolving speed is 100r/min, and Ball-milling Time is 60 hours.In oxide powder upon mixing be added glucose powder, and be incorporated with
The dehydrated alcohol of the isometric ratio of glucose powder carries out secondary ball milling, rotational speed of ball-mill 70r/min, Ball-milling Time 15h.It will be upper
It states powder and is placed in vacuum drying oven and reacted, vacuum degree 10Pa is first heated to 160 DEG C of heat preservation 30min, then is warming up to 400
DEG C heat preservation 3h, is finally warming up to 950 DEG C of heat preservation 3h, the nano composite powder of distribution WC is prepared on W matrix, wherein the matter of WC
Amount is than being 10%.Pattern in the present embodiment after raw material powder ball milling mixing is shown in Fig. 1, and the raw material powder after ball milling mixing is through Portugal
Pattern after grape sugar cladding is shown in Fig. 2, and the composition analysis result of the composite powder of preparation is shown in Table 1.
Embodiment 2
Weigh 1 kilogram of WO3, 0.05 kilogram of Co3O4With 0.45 kilogram of glucose (C6H12O6), first by WO3、Co3O4And nothing
Water-ethanol carries out mixing and ball milling, and abrading-ball and powder quality ratio are 5:1, and dehydrated alcohol and volume of material ratio are 1:1, drum's speed of rotation
For 300r/min, Ball-milling Time is 70 hours.Glucose powder, and supplying and grape are added in oxide powder upon mixing
The dehydrated alcohol of the isometric ratio in Icing Sugar end carries out secondary ball milling, rotational speed of ball-mill 80r/min, Ball-milling Time 10h.By above-mentioned powder
End, which is placed in vacuum drying oven, is reacted, vacuum degree 0.1Pa, is first heated to 180 DEG C of heat preservation 15min, then be warming up to 500 DEG C of guarantors
Warm 2h is finally warming up to 1100 DEG C of heat preservation 2h, the nano composite powder that WC is distributed on W matrix is prepared, wherein the quality of WC
Than being 15%.The pattern and particle diameter distribution for the tungsten base composite powder that the present embodiment is prepared are shown in Fig. 3, the composite powder of preparation
Composition analysis result be shown in Table 1.
Embodiment 3
Weigh 1 kilogram of WO2.9, 0.1 kilogram of Co3O4With 0.5 kilogram of glucose (C6H12O6), first by WO2.9、Co3O4Powder
Mixing and ball milling is carried out with dehydrated alcohol, and the mass ratio of abrading-ball and powder is 3:1, and the volume ratio of dehydrated alcohol and material is 1:1, ball
Mill speed is 500r/min, and Ball-milling Time is 80 hours.Glucose powder is added in oxide powder upon mixing, and matches
Enter and carries out secondary ball milling, rotational speed of ball-mill 50r/min, Ball-milling Time 20h with the dehydrated alcohol of the isometric ratio of glucose powder.
Above-mentioned powder is placed in vacuum drying oven and is reacted, vacuum degree 0.02Pa is first heated to 150 DEG C of heat preservation 60min, then heats up
To 350 DEG C of heat preservation 4h, 850 DEG C of heat preservation 5h are finally warming up to, the nano composite powder for being distributed WC on W matrix is prepared, wherein
The mass ratio of WC is 20%.The object phase testing result for the tungsten base composite powder that the present embodiment is prepared is shown in Fig. 4, the present embodiment
The composition analysis result for the tungsten base composite powder being prepared is shown in Table 1.
The composition analysis result for the nanometer tungsten base composite powder being prepared in the different embodiments of table 1
Claims (3)
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| CN108262485B (en) * | 2018-02-25 | 2020-11-27 | 北京工业大学 | A kind of industrialized in-situ synthesis method of W-based composite powder that can add WC strengthening phase |
| CN113441728A (en) * | 2021-06-28 | 2021-09-28 | 北京理工大学 | Preparation method of high-uniformity ultrafine/nano tungsten powder |
| CN114713833B (en) * | 2022-03-10 | 2024-03-22 | 崇义章源钨业股份有限公司 | Spherical tungsten-based composite powder based on in-situ reduction and preparation method thereof |
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| CN101624673A (en) * | 2009-08-14 | 2010-01-13 | 北京工业大学 | Industrialized preparation method of WC-Co hard alloy with low cost and high performance |
| CN103131999A (en) * | 2013-03-14 | 2013-06-05 | 浙江亚通冶金科技有限公司 | Wolfram carbide-cobalt-carbon composite powder for hot spraying and preparation method thereof |
| CN105648383A (en) * | 2016-01-12 | 2016-06-08 | 江西理工大学 | Preparing method for WC-Co composite powder for thermal spraying |
| CN106350721A (en) * | 2016-09-05 | 2017-01-25 | 中南大学 | Preparation method of high-performance WC-Co cemented carbide of plate-like grain structure |
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| KR100626224B1 (en) * | 2004-02-14 | 2006-09-20 | 재단법인서울대학교산학협력재단 | Solid solution powder, its manufacturing method, the powder for cermet containing the said solid solution powder, its manufacturing method, and cermet using the said powder for cermet |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101624673A (en) * | 2009-08-14 | 2010-01-13 | 北京工业大学 | Industrialized preparation method of WC-Co hard alloy with low cost and high performance |
| CN103131999A (en) * | 2013-03-14 | 2013-06-05 | 浙江亚通冶金科技有限公司 | Wolfram carbide-cobalt-carbon composite powder for hot spraying and preparation method thereof |
| CN105648383A (en) * | 2016-01-12 | 2016-06-08 | 江西理工大学 | Preparing method for WC-Co composite powder for thermal spraying |
| CN106350721A (en) * | 2016-09-05 | 2017-01-25 | 中南大学 | Preparation method of high-performance WC-Co cemented carbide of plate-like grain structure |
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