CN108409327A - A kind of method of carbothermic method synthesis WC base nano composite powders - Google Patents
A kind of method of carbothermic method synthesis WC base nano composite powders Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000009826 distribution Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001935 vanadium oxide Inorganic materials 0.000 claims abstract description 7
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 6
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- 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 6
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 6
- 229910052786 argon Inorganic materials 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 5
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims description 8
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 8
- 238000003763 carbonization Methods 0.000 claims description 6
- 238000010189 synthetic method Methods 0.000 claims description 5
- URYQJPFTRVWTAG-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].[W+4] Chemical compound [O-2].[O-2].[Ti+4].[W+4] URYQJPFTRVWTAG-UHFFFAOYSA-N 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 description 15
- 239000000956 alloy Substances 0.000 description 15
- 239000002131 composite material Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 235000013339 cereals Nutrition 0.000 description 7
- 229910009043 WC-Co Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5626—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on tungsten carbides
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
Abstract
A kind of method of carbothermic method synthesis WC base nano composite powders, feature include the following steps：A, nanometer tungsten oxide 6.41 g ~ 7.58 g, 0.65 ~ 0.76g of nanometer cobalt oxide, vanadium oxide nanoparticle, nano chromium oxide mixture 0.048g ~ 0.057g, nanometer carbon reducing agent 1.60g ~ 2.90 g are taken by weight, they are placed in batch mixer, using the method for wet mixing, after being sufficiently mixed, mixture is made.B, mixture obtained by step a is placed in drying box, dry 1h ~ 3h under the conditions of 200 DEG C.C, the mixture after will be dry obtained by step b is placed in high temperature reaction stove, and under the conditions of vacuum or argon gas atmosphere, average grain diameter is made<The WC base nano composite powders of 100nm, even particle size distribution.The present invention is easy with preparation process, the period is short, low energy consumption, and cost can be greatly lowered, and is suitble to industrial production.
Description
Technical field
The present invention relates to a kind of methods that carbothermic method synthesizes WC base nano composite powders, and it is multiple to belong to nanometer metal ceramic
Close Preparation Technique of Powders field.
Background technology
In recent years, ultra-fine/nanometer WC-Co composite powder because of its excellent physical mechanical property be widely used in ultra-fine/is received
The fields such as the preparation of rice cemented carbide, thermal spraying, metal Quick-forming, surface mount, material surface strengthening.Such as nano WC-Co
More carefully, evenly, mechanical property is good, makes for the hard alloy crystal grain that hard alloy prepared by composite powder is prepared than conventional hybrid material
Use long lifespan.Hard alloy occupies importantly in fields such as modern tool material, wear-resistant material, high temperature resistant and resistant materials
Position, largely instead of high-speed steel, causes the technological revolution of metal cutting process industry, is known as " industrial tooth
Tooth ".Wherein, WC-Co hard alloy main component WC hardness is quite high, has between Binder Phase Co and WC good
Wetability, contact angle is essentially 0 DEG C, therefore WC-Co composite materials are formed in the case of stress by carbide particle
Skeleton can bear prodigious stress, show high intensity, and absorb energy by deformation as the Co of Binder Phase, inhibit
Crack growth shows preferable fracture toughness.Thus, WC-Co series hard metals account for the half of entire hart metal product with
On.
Modern industry is higher and higher to the performance requirement of hard alloy, and the crystallite dimension of WC is smaller in hard alloy, glues
Tie the mean free path of phase Co（That is the thickness of hard phase WC intercrystallines cobalt layers）Shorter, the hardness and strength of alloy are higher.
WC crystal grain is 0.5 μm of ultra-fine cemented carbide below because it is with excellent comprehensive performance, in difficult-to-machine material field, micro-
It is used widely in the fields such as electronics industry, precision die processing industry, timber processing, medicine.WC crystal grain is in 100nm or less
Nano hard alloy have more excellent performance.Therefore, it has become various countries in " refractory metal and hard material " field
One of the hot spot that scientist competitively studies.The crucial technology of preparing of one of ultra-fine cemented carbide is the preparation of powder, alloy
Crystallite dimension is dependent firstly on the granular size of powder, prepares that particle is tiny, even-grained powder is to prepare ultra-fine hard
The necessary condition of alloy.Theory and practice shows when the WC grain size of WC-Co alloys is reduced to sub-micron or less, material
Hardness, toughness, intensity, the wearability of material can be improved, while the sintering temperature reached needed for densification completely is relatively low.Cause
This, a main trend of current cemented carbide industry is had become from conventional rigid alloy to ultra-fine or nano hard alloy development.
Invention content
The purpose of the present invention is to provide a kind of synthetic methods of novel nano WC base composite powders, to better meet
Application of the WC bases composite powder in fields such as ultra-fine/nano hard alloy manufacture, material surface strengthening sprayings.What the present invention used
In-situ reducing carbonizatin method, equipment needed for this method is simple, and reaction raw materials are cheap, and preparation process is easy, the period is short, energy consumption
It is low, manufacturing cost can be greatly lowered, ensure that the WC bases composite powder of synthesis is full in granularity, dispersibility, grain shape etc.
Sufficient industrial requirement.
The synthetic method of the WC base nano composite powders of the present invention includes the following steps：
A, nanometer tungsten oxide 6.41 g ~ 7.58 g, 0.65 ~ 0.76g of nanometer cobalt oxide, vanadium oxide nanoparticle, nanometer are taken by weight
Chromium oxide mixture 0.048g ~ 0.057g, the nanometer carbon reducing agent g of 1.60g ~ 2.90, they are placed in batch mixer, are used
After being sufficiently mixed, mixture is made in the method for wet mixing.
B, mixture obtained by step a is placed in drying box, dry 1h ~ 3h under the conditions of 200 DEG C.
C, the mixture after will be dry obtained by step b is placed in high temperature reaction stove, under the conditions of vacuum or argon gas atmosphere,
1000 ~ 1300 DEG C, carbon thermal reduction carbonization is carried out under conditions of 0.5 ~ 2h, average grain diameter is made<100nm, even particle size distribution
WC base nano composite powders.
The nanometer tungsten oxide is any one in nano tungsten trioxide or nanometer titanium dioxide tungsten.
The nanometer cobalt oxide is any one in nano-cobaltic-cobaltous oxide, nanometer cobalt sesquioxide or nano cobaltous oxide
Kind.
The vanadium oxide nanoparticle is any one in nanometer vanadic anhydride, nano vanadium dioxide or nanometer vanadium trioxide
Kind.
The nano chromium oxide is Nanoscale Chromic Oxides.
The nanometer carbon reducing agent is any one in nanometer carbon black or nano active carbon.
The high temperature reaction stove is any one in tube furnace or micro-wave oven.
The present invention compares the existing method for preparing WC base composite powders, has the advantages that：
（1）It is simple for process.Raw material is after batch mixing, drying, you can carries out carbon thermal reduction carbonization, and once completes, simplifies system
Standby technique, it is easy to operate, it is suitble to industrialized production.
（2）Reaction temperature is low, and the reaction time is short, energy saving.With nanometer tungsten oxide, nanometer cobalt oxide, vanadium oxide nanoparticle,
Nano chromium oxide mixture, nanometer carbon reducing agent are raw material, have higher specific surface area, the contact area between particle compared with
Greatly, interface atoms number is more, and interface zone atomic diffusivity is higher so that nano material has higher chemism, can
To accelerate the progress of carbon thermal reduction carburizing reagent.The synthetic method of tradition WC base nano composite powders relatively, this synthetic method can
Reaction temperature is greatly lowered, shorten the reaction time, the effectively save energy.
（3）It has excellent performance：The polynary WC bases nano composite powder generated is reacted, impurity content is few, powder size<100nm,
Epigranular, particle size distribution range is relatively narrow, has broad prospect of application in fields such as hard alloy, electronic material, coating materials.
Specific implementation mode
The present invention is further described below with reference to embodiment：
Embodiment 1：
6.41 g of nano tungsten trioxide, nano-cobaltic-cobaltous oxide 0.76g, 2.77 g of nanometer carbon black, five oxygen of nanometer are taken by weight
Change two vanadium 0.027g, Nanoscale Chromic Oxides 0.030g, they are placed in batch mixer, using wet mixing mode, decentralized medium is
After being sufficiently mixed, mixture is made in absolute ethyl alcohol.Gained mixture is placed in drying box, dry 1h under the conditions of 200 DEG C.
Mixture after drying is placed in tube furnace, under vacuum, carbon is carried out under conditions of 1000 ~ 1300 DEG C, 0.5 ~ 2h
Thermal reduction carbonization, is made average grain diameter<The WC base composite powders of 100nm, even particle size distribution.
Embodiment 2：
7.58 g of nanometer titanium dioxide tungsten, nanometer cobalt sesquioxide 0.65g, 1.72 g of nano active carbon, nanometer two are taken by weight
Vanadium oxide 0.020g, Nanoscale Chromic Oxides 0.028g, they are placed in batch mixer, and using wet mixing mode, decentralized medium is
After being sufficiently mixed, mixture is made in anhydrous propanone.Gained mixture is placed in drying box, dry 2h under the conditions of 200 DEG C.
Mixture after drying is placed in micro-wave oven, under the conditions of argon gas atmosphere, under conditions of 1000 ~ 1300 DEG C, 0.5 ~ 2h into
Row carbon thermal reduction is carbonized, and average grain diameter is made<The WC base composite powders of 100nm, even particle size distribution.
Embodiment 3：
7.50 g of nano tungsten trioxide, nano cobaltous oxide 0.70g, 1.65 g of nanometer carbon black, nanometer three is taken to aoxidize by weight
Two vanadium 0.020g, Nanoscale Chromic Oxides 0.030g, they are placed in batch mixer, and using wet mixing mode, decentralized medium is nothing
After being sufficiently mixed, mixture is made in water-ethanol.Gained mixture is placed in drying box, dry 3h under the conditions of 200 DEG C.It will
Mixture after drying is placed in tube furnace, under vacuum, carbon heat is carried out under conditions of 1000 ~ 1300 DEG C, 0.5 ~ 2h
Average grain diameter is made in reduction and carbonization<The WC base composite powders of 100nm, even particle size distribution.
Embodiment 4：
6.45 g of nanometer titanium dioxide tungsten, nanometer cobalt sesquioxide 0.68g, 2.90 g of nano active carbon, nanometer five are taken by weight
V 2 O 0.037g, Nanoscale Chromic Oxides 0.020g, they are placed in batch mixer, using wet mixing mode, decentralized medium
For anhydrous propanone, after being sufficiently mixed, mixture is made.Gained mixture is placed in drying box, it is dry under the conditions of 200 DEG C
1.5h.Mixture after drying is placed in micro-wave oven, under the conditions of argon gas atmosphere, in 1000 ~ 1300 DEG C, the condition of 0.5 ~ 2h
Average grain diameter is made in lower progress carbon thermal reduction carbonization<The WC base composite powders of 100nm, even particle size distribution.
Claims (7)
1. a kind of method of carbothermic method synthesis WC base nano composite powders, it is characterised in that：The synthetic method include with
Lower step：
A, nanometer tungsten oxide 6.41 g ~ 7.58 g, 0.65 ~ 0.76g of nanometer cobalt oxide, vanadium oxide nanoparticle, nanometer are taken by weight
Chromium oxide mixture 0.048g ~ 0.057g, the nanometer carbon reducing agent g of 1.60g ~ 2.90, they are placed in batch mixer, are used
After being sufficiently mixed, mixture is made in the method for wet mixing；
B, mixture obtained by step a is placed in drying box, dry 1h ~ 3h under the conditions of 200 DEG C；
C, the mixture after will be dry obtained by step b is placed in high temperature reaction stove, under the conditions of vacuum or argon gas atmosphere, 1000
~ 1300 DEG C, carbon thermal reduction carbonization is carried out under conditions of 0.5 ~ 2h, average grain diameter is made<The WC bases of 100nm, even particle size distribution
Nano composite powder.
2. nanometer tungsten oxide is any one in nano tungsten trioxide or nanometer titanium dioxide tungsten according to claim 1.
3. nanometer cobalt oxide is nano-cobaltic-cobaltous oxide, nanometer cobalt sesquioxide or nano oxidized Asia according to claim 1
Any one in cobalt.
4. vanadium oxide nanoparticle is nanometer vanadic anhydride, nano vanadium dioxide or the oxidation of nanometer three two according to claim 1
Any one in vanadium.
5. nano chromium oxide is Nanoscale Chromic Oxides according to claim 1.
6. nanometer carbon reducing agent is any one in nanometer carbon black or nano active carbon according to claim 1.
7. high temperature reaction stove is any one in tube furnace or micro-wave oven according to claim 1.
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| CN110257658A (en) * | 2019-07-27 | 2019-09-20 | 河南工业大学 | A kind of synthesis and application of polynary WC based composites |
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