CN106825599A - A kind of preparation method of the WC Co nanometer powders for adding grain growth inhibitor - Google Patents

A kind of preparation method of the WC Co nanometer powders for adding grain growth inhibitor Download PDF

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CN106825599A
CN106825599A CN201710038790.6A CN201710038790A CN106825599A CN 106825599 A CN106825599 A CN 106825599A CN 201710038790 A CN201710038790 A CN 201710038790A CN 106825599 A CN106825599 A CN 106825599A
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grain growth
growth inhibitor
preparation
nanometer powders
nitrate
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CN106825599B (en
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秦明礼
陈铮
陈鹏起
赵尚杰
鲁慧峰
吴昊阳
贾宝瑞
曲选辉
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University of Science and Technology Beijing USTB
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor

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Abstract

The invention provides a kind of preparation method of the WC Co nanometer powders for adding grain growth inhibitor, belong to powder metallurgy powder preparing technical field.Specifically preparation method is：With ammonium metatungstate, cobalt nitrate, fuel, ammonium nitrate, the slaine of the grain growth inhibitor of required addition and organic carbon source as raw material; oxide/carbon composite powder is prepared using low-temperature combustion synthesis, then carrying out being carbonized under atmosphere protection or under vacuum obtains the WC Co nanometer powders of grain growth inhibitor doping.The low-temperature combustion synthesis that the present invention is used belongs to liquid phase synthesizing method, can reach the other mixing of molecular level, and the diffusion path that this allows for carbonaceous in carbonisation is short, and reaction temperature and time requirement are relatively low.The raw material of other this method is simple and easy to get, and equipment is simple, and technique is quick, is appropriate for large-scale production.

Description

A kind of preparation method of the WC-Co nanometer powders for adding grain growth inhibitor
Technical field
The invention belongs to field of powder metallurgy, the method for being related to prepare WC-Co nanometer powders, more particularly to a kind of addition is brilliant The square preparation method of the WC-Co nanometer powders of the big inhibitor of grain length.
Background technology
WC-Co hard alloy has high intensity, high rigidity, high thermoconductivity, high temperature resistant and corrosion-resistant etc. a series of excellent Performance, thus it achieves extensive use in industrial circles such as metal cutting process, rock drilling mining, mould, wear parts. Research shows that the crystal grain for refining WC-Co hard alloy can effectively improve its mechanical performance.And to prepare the WC- of Ultra-fine Grained Co hard alloy first has to prepare Ultra-fine WC-Co Cemented Carbide powder.Traditional WC-Co nanosized hardmetal powders that prepare Method mainly has the method such as ball-milling method and self-propagating high-temperature combustion method (SHS).(the Journal ofAlloy and such as Song Compounds, 458 (2008), 366-371.) with WO2.9、Co3O4It is raw material with carbon black, by being carbonized after ball milling mixing It is the ultra-fine cemented carbide powder of 300nm that average grain size is obtained.(the Materials Letters, 158 such as Zaitsev (2015), 329-332.) WC powder first is prepared using SHS methods, obtained WC powder is mixed with Co powder by ball milling then Superfine WC-Co powder is obtained.
But, due to the generation of liquid phase during sintering, crystal grain can grow up rapidly WC-Co hard alloy, so that shadow Ring its mechanical performance.Addition grain growth inhibitor is a kind of method that crystal grain is grown up during effective suppression is sintered, crystal grain Inhibitor of growing up mainly has VC, Cr3C2, NbC, TiC, TaC, ZrC etc..And grain growth inhibitor can be evenly dispersed in The performance of hard alloy served in WC-Co nanosized hardmetal powders conclusive.So far, most additions is used The method of grain growth inhibitor is ball-milling method, but ball-milling method is difficult to be evenly dispersed in a small amount of grain growth inhibitor In WC-Co nanosized hardmetal powders, the uneven dispersion of inhibitor can cause in sintering process WC phases in Binder Phase not Uniform dissolution, so as to cause the abnormal growth of crystal grain, uneven microscopic structure inevitably damages the performance of hard alloy.
Usually, wet chemical method is considered as that prepared composition is accurate, finely dispersed nano material effective ways. Nan Lin etc. (Scripta Materialia, 67 (2012), 826-829.) are prepared for WO using the mode of co-precipitation3-V2O5 Core shell structure powder, then by itself and carbon black and Co3O4Carbonization obtains WC-VC-Co nanometer powders after being mixed.Hua Lin Deng (Ceramics International, 39 (2013), 9671-9675.) forerunner is prepared with Hydrothermal Synthesiss and spray drying process Body, has then prepared WC-VC-Co nanometer powders by carbon thermal reduction in situ.(the Ceramics such as Mardali International, 42 (2016), 9382-9386.) presoma is prepared using sol-gal process, then by gel in hydrogen The WC-Co nanometer powders of VC doping are prepared in middle calcining.But or these preparation method energy consumptions are larger, time loss is more long, Preparation method is cumbersome, and scale is smaller, is not suitable for and large-scale production.So, develop a kind of simple and efficient preparation and add Plus the method for the WC-Co nanometer powders of grain growth inhibitor has critically important scientific meaning.
The content of the invention
It is an object of the invention to according in the middle of prior art or energy consumption is larger, time loss is more long, or preparation method is numerous It is trivial, it is not suitable for the shortcoming with large-scale production, there is provided a kind of simple and quick addition grain growth inhibitor WC-Co nanometer powders Preparation method,
The present invention is comprised the following specific steps that：
(1) presoma is prepared using low-temperature combustion synthesis.Preparing the process of presoma is：By ammonium metatungstate, cobalt nitrate, Fuel, ammonium nitrate are dissolved in deionized water by certain molar ratio and are configured to the aqueous solution, and aequum is added in aqueous Grain growth inhibitor slaine and organic carbon source, dissolve it.Solution being heated to, combustion reaction occurs, obtains fluffy Precursor powder.
(2) the precursor powder grinding that will be obtained, is then placed in being carbonized in tube furnace or vacuum drying oven, you can added Plus the WC-Co nanometer powders of grain growth inhibitor.
Fuel in step (1) is at least one in glycine, urea, EDTA, thiocarbamide.
The grain growth inhibitor slaine of the required addition in step (1) is chromic nitrate, ammonium molybdate, ammonium vanadate, nitric acid At least one in niobium acyl, nitric acid tantalum acyl, lanthanum nitrate, yttrium nitrate.
Required organic carbon source in step (1) is at least one in glucose, soluble starch, citric acid.
Ammonium metatungstate, cobalt nitrate, fuel and ammonium nitrate molar ratio in step (1) are 1：(2.5~13)：(10~ 15):(15~25).
The amount of the grain growth inhibitor slaine of the addition in step (1) according to needed for inhibitor in final product Mass fraction calculate, mass fraction be 0.1%~5%.
Carburizing temperature is 750~1200 DEG C in step (2), and heating rate is 1~10 DEG C/min, and soaking time is 1~8h. Carburizing atmosphere is nitrogen, hydrogen or argon gas in tube furnace, and carbonization needs furnace pressure to be less than 100Pa in vacuum drying oven.
Technology of the invention has following advantage：
(1) raw material is simple and easy to get, and equipment is simple, and technique is quick, can in a short time prepare substantial amounts of product.
(2) method for preparing presoma uses wet chemical method, each composition to reach the other mixing of molecular level in the solution, Tungsten oxide, cobalt oxide, inhibitor metal oxide and agraphitic carbon are well mixed in the presoma for obtaining, the oxidation of inhibitor metal Thing is dispersed in presoma.
(3) due in presoma oxide particle reach nano-scale, the diffusion path of carbon is short during carbonization, Reaction temperature is low, and the reaction time is short.The final WC-Co nano-powder particles for preparing are tiny, and inhibitor is uniformly dispersed.
(4) composition of Binder Phase and inhibitor can be by adjusting the addition of raw material come freely in WC-Co nanometer powders Regulate and control exactly.
Brief description of the drawings
Fig. 1 is the XRD spectrum of the WC-Co nanometer powders for adding grain growth inhibitor.
Specific embodiment
Embodiment 1
By 9.44g ammonium metatungstates, 5g cobalt nitrate hexahydrates, 4.3g urea, 10g ammonium nitrate, 6.5g glucose and 0.14g vanadic acid Ammonium is put into beaker and adds the solution that appropriate water dissolves are clarified, and the solution is placed on electric furnace and is heated to reaction hair It is raw, obtain fluffy precursor powder.Precursor powder is put into tube furnace and is carbonized, carburizing temperature is 950 DEG C, soaking time It is 2.5h, the rate of heat addition is 8 DEG C/min, and protective atmosphere is argon gas, room temperature is naturally cooled to after the completion of insulation and obtains VC doping WC-Co nanometer powders.
Embodiment 2
By 9.44g ammonium metatungstates, 3.8g cobalt nitrate hexahydrates, 4.3g urea, 10g ammonium nitrate, 6.5g glucose and 0.14g vanadium Sour ammonium is put into the solution in beaker adding appropriate water dissolves to be clarified, and solution is placed on the horse for being previously heated to 260 DEG C Not in stove, question response takes out after occurring and obtains precursor powder.Its body powder is placed and is carbonized in a vacuum furnace, reaction temperature It it is 900 DEG C, soaking time is 1.5h, heating rate is 5 DEG C/min, and vacuum is 100MPa, naturally cools to room temperature and obtains VC The WC-Co nanometer powders of doping.
Embodiment 3
By 18.7g ammonium metatungstates, 7.57g cobalt nitrate hexahydrates, 8.5g urea, 20g ammonium nitrate, 13g glucose and 0.5g nitre Sour chromium is put into the solution in beaker adding appropriate water dissolves to be clarified, and solution is placed on the horse for being previously heated to 245 DEG C Not it is incubated in stove to combustion reaction and is completed, taking-up obtains precursor powder.Precursor powder is ground, is then inserted in tube furnace Carbonization, carburizing temperature is 1000 DEG C, and soaking time is 3h, my 10 DEG C/min of heating rate, naturally cools to room temperature and obtains Cr3C2 The WC-Co nanometer powders of doping.
Embodiment 4
By 9.44g ammonium metatungstates, 6.4g cobalt nitrate hexahydrates, 4.3g urea, 10g ammonium nitrate, 6.5g glucose, 0.6g nitric acid Chromium and 0.1g ammonium vanadate are put into the solution in beaker adding appropriate water dissolves to be clarified, and the solution is placed on electric furnace and is added Heat to reaction occurs, and obtains fluffy precursor powder.Precursor powder is put into tube furnace and is carbonized, carburizing temperature is 950 DEG C, soaking time is 3h, and the rate of heat addition is 5 DEG C/min, and protective atmosphere is nitrogen, room temperature is naturally cooled to after the completion of insulation and is obtained VC, Cr3C2The WC-Co nanometer powders of doping.
Embodiment 5
By 18.7g ammonium metatungstates, 7.57g cobalt nitrate hexahydrates, 8.5g urea, 20g ammonium nitrate, 13g glucose and 1.2g nitre Sour yttrium is put into the solution in beaker adding appropriate water dissolves to be clarified, and solution is placed on the horse for being previously heated to 250 DEG C Not it is incubated in stove to combustion reaction and is completed, taking-up obtains precursor powder.Precursor powder is ground, is then inserted in tube furnace Carbonization, carburizing temperature is 900 DEG C, and soaking time is 2h, and heating rate is 5 DEG C/min, naturally cools to room temperature and obtains Y2O3Doping WC-Co nanometer powders.

Claims (7)

1. it is a kind of add grain growth inhibitor WC-Co nanometer powders preparation method, it is characterised in that preparation process is as follows：
(1) presoma is prepared using low-temperature combustion synthesis, preparing the process of presoma is：By ammonium metatungstate, cobalt nitrate, combustion Material, ammonium nitrate are dissolved in by certain molar ratio and the aqueous solution are configured in deionized water, are added in aqueous the desired amount of The slaine and organic carbon source of grain growth inhibitor, dissolve it；Solution being heated to, combustion reaction occurs, obtains fluffy Precursor powder；
(2) the precursor powder grinding that will be obtained, is then placed in being carbonized in tube furnace or vacuum drying oven, you can obtain addition brilliant The WC-Co nanometer powders of the big inhibitor of grain length.
2. a kind of preparation method of the WC-Co nanometer powders for adding grain growth inhibitor as claimed in claim 1, its feature exists Fuel in step (1) is at least one in glycine, urea, EDTA, thiocarbamide.
3. a kind of preparation method of the WC-Co nanometer powders for adding grain growth inhibitor as claimed in claim 1, its feature exists The grain growth inhibitor slaine of the required addition in step (1) is chromic nitrate, ammonium molybdate, ammonium vanadate, nitric acid niobium acyl, nitre At least one in sour tantalum acyl, lanthanum nitrate, yttrium nitrate.
4. a kind of preparation method of the WC-Co nanometer powders for adding grain growth inhibitor as claimed in claim 1, its feature exists Required organic carbon source in step (1) is at least one in glucose, soluble starch, citric acid.
5. a kind of preparation method of the WC-Co nanometer powders for adding grain growth inhibitor as claimed in claim 1, its feature exists Ammonium metatungstate, cobalt nitrate, fuel and ammonium nitrate molar ratio in step (1) are 1：(2.5~13)：(10~15):(15~ 25)。
6. a kind of preparation method of the WC-Co nanometer powders for adding grain growth inhibitor as claimed in claim 1, its feature exists The amount of the grain growth inhibitor slaine of the addition in step (1) quality of inhibitor in final product according to needed for Fraction is calculated, and mass fraction is 0.1%~5%.
7. a kind of preparation method of the WC-Co nanometer powders for adding grain growth inhibitor as claimed in claim 1, its feature exists Carburizing temperature is 750~1200 DEG C in step (2), and heating rate is 1~10 DEG C/min, and soaking time is 1~8h；Tube furnace Middle carburizing atmosphere is nitrogen, hydrogen or argon gas, and carbonization needs furnace pressure to be less than 100Pa in vacuum drying oven.
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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107790738A (en) * 2017-10-18 2018-03-13 北京科技大学 It is a kind of to prepare a nanometer method for W Re alloy powders
CN109126844A (en) * 2018-08-31 2019-01-04 厦门理工学院 A kind of molybdenum carbide nanometer sheet and its preparation method and application
CN109500386A (en) * 2018-12-17 2019-03-22 石家庄铁道大学 Heterogeneous core-shell structure composite powder and preparation method thereof
CN109675598A (en) * 2019-03-04 2019-04-26 合肥工业大学 A kind of preparation method of the nickel tungsten carbide composite nano-powder as elctro-catalyst
CN110629094A (en) * 2018-06-25 2019-12-31 中国科学院苏州纳米技术与纳米仿生研究所 Carbon-nitrogen compound grain refiner and preparation method and application thereof
CN110756796A (en) * 2018-07-25 2020-02-07 石家庄铁道大学 Composite powder with core-shell structure and preparation method thereof
CN111842920A (en) * 2020-08-04 2020-10-30 厦门理工学院 Nanoscale high-performance hard alloy inhibitor and preparation method thereof
CN111893339A (en) * 2020-08-06 2020-11-06 合肥工业大学 Method for preparing high-performance WC-8Co-Y2O3 hard alloy by wet chemical method
CN111979462A (en) * 2020-08-21 2020-11-24 合肥工业大学 WC-MoC-Co-Y2O3 hard alloy with high hardness and preparation method thereof
CN112250442A (en) * 2020-09-30 2021-01-22 北京科技大学 Preparation method of high-toughness binderless nanocrystalline hard alloy
CN113416862A (en) * 2021-06-04 2021-09-21 合肥工业大学 Preparation method of hard alloy and hard alloy prepared by adopting same
CN113502596A (en) * 2021-06-28 2021-10-15 南通大学 Self-supporting MgTiO3Nano fiber chemical warfare agent degradation material and preparation method thereof
CN114029496A (en) * 2021-10-12 2022-02-11 南昌大学 Preparation method of novel superfine molybdenum-rhenium alloy powder
CN116969763A (en) * 2023-09-25 2023-10-31 成都先进金属材料产业技术研究院股份有限公司 Graphene-toughened non-bonding-phase WC-based hard alloy and preparation method thereof

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CN101760685A (en) * 2008-12-25 2010-06-30 北京有色金属研究总院 Superfine WC-Co cemented carbide containing rare-earth elements and preparation method thereof
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Cited By (20)

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CN107790738A (en) * 2017-10-18 2018-03-13 北京科技大学 It is a kind of to prepare a nanometer method for W Re alloy powders
CN107790738B (en) * 2017-10-18 2019-10-22 北京科技大学 A method of preparing a nanometer W-Re alloy powder
CN110629094A (en) * 2018-06-25 2019-12-31 中国科学院苏州纳米技术与纳米仿生研究所 Carbon-nitrogen compound grain refiner and preparation method and application thereof
CN110756796B (en) * 2018-07-25 2021-08-27 石家庄铁道大学 Composite powder with core-shell structure and preparation method thereof
CN110756796A (en) * 2018-07-25 2020-02-07 石家庄铁道大学 Composite powder with core-shell structure and preparation method thereof
CN109126844A (en) * 2018-08-31 2019-01-04 厦门理工学院 A kind of molybdenum carbide nanometer sheet and its preparation method and application
CN109126844B (en) * 2018-08-31 2021-05-25 厦门理工学院 Molybdenum carbide nanosheet and preparation method and application thereof
CN109500386A (en) * 2018-12-17 2019-03-22 石家庄铁道大学 Heterogeneous core-shell structure composite powder and preparation method thereof
CN109675598A (en) * 2019-03-04 2019-04-26 合肥工业大学 A kind of preparation method of the nickel tungsten carbide composite nano-powder as elctro-catalyst
CN109675598B (en) * 2019-03-04 2022-03-11 合肥工业大学 Preparation method of nickel tungsten carbide nano composite powder used as electrocatalyst
CN111842920A (en) * 2020-08-04 2020-10-30 厦门理工学院 Nanoscale high-performance hard alloy inhibitor and preparation method thereof
CN111893339A (en) * 2020-08-06 2020-11-06 合肥工业大学 Method for preparing high-performance WC-8Co-Y2O3 hard alloy by wet chemical method
CN111979462A (en) * 2020-08-21 2020-11-24 合肥工业大学 WC-MoC-Co-Y2O3 hard alloy with high hardness and preparation method thereof
CN112250442A (en) * 2020-09-30 2021-01-22 北京科技大学 Preparation method of high-toughness binderless nanocrystalline hard alloy
CN112250442B (en) * 2020-09-30 2021-08-24 北京科技大学 Preparation method of high-toughness binderless nanocrystalline hard alloy
CN113416862A (en) * 2021-06-04 2021-09-21 合肥工业大学 Preparation method of hard alloy and hard alloy prepared by adopting same
CN113502596A (en) * 2021-06-28 2021-10-15 南通大学 Self-supporting MgTiO3Nano fiber chemical warfare agent degradation material and preparation method thereof
CN114029496A (en) * 2021-10-12 2022-02-11 南昌大学 Preparation method of novel superfine molybdenum-rhenium alloy powder
CN116969763A (en) * 2023-09-25 2023-10-31 成都先进金属材料产业技术研究院股份有限公司 Graphene-toughened non-bonding-phase WC-based hard alloy and preparation method thereof
CN116969763B (en) * 2023-09-25 2023-12-12 成都先进金属材料产业技术研究院股份有限公司 Graphene-toughened non-bonding-phase WC-based hard alloy and preparation method thereof

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