CN101323925A - Tungsten carbide material with Ni3Al as cementing phase and preparation thereof - Google Patents

Tungsten carbide material with Ni3Al as cementing phase and preparation thereof Download PDF

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Publication number
CN101323925A
CN101323925A CNA2008100290206A CN200810029020A CN101323925A CN 101323925 A CN101323925 A CN 101323925A CN A2008100290206 A CNA2008100290206 A CN A2008100290206A CN 200810029020 A CN200810029020 A CN 200810029020A CN 101323925 A CN101323925 A CN 101323925A
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sintering
powder
tungsten carbide
electric current
preparation
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李小强
李元元
郭亮
屈盛官
邵明
夏伟
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South China University of Technology SCUT
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South China University of Technology SCUT
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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Abstract

The invention relates to a plastic forming technique and a powder metallurgy technique and provides a tungsten carbide material which adopts Ni3Al as binder phase and a preparation method thereof. The tungsten carbide material adopts toughening intermetallic compound Ni3Al to substitute cobalt with traditional binder phase and contains the following components according to mass percentage: 86 to 95 percent of WC, 5 to 14 percent of toughening Ni3Al. The preparation method comprises the steps: ball grinding is carried out to the raw materials according to the percentages until the size of WC powder crystal grain is thinned to be less than 100nm; current rapid sintering method is adopted to form solidified ball grinding powder, and the conditions of current rapid sintering process are as follows: types of sintering current: square wave pulsed current or constant current; sintering pressure: 10MPa to 50MPa; sintering time: 2 to 8 minutes. The plastic forming technique, the powder metallurgy technique and the tungsten carbide material of the invention can not only save strategic material cobalt, reduce material cost, but also effectively improve the performance of high temperature resistant and corrosion resistant performance of the material and have good promotion and application prospect.

Description

A kind of with Ni 3Al is the tungsten carbide material of phase and preparation method thereof that bonds
Technical field
The present invention relates to plastic forming technology and powder metallurgy technology, specifically be meant a kind of low cost, high-performance, with Ni 3Al is the tungsten carbide material of phase and preparation method thereof that bonds.
Background technology
Existing wolfram varbide (WC) based hard alloy material, mainly by matrix wolfram varbide and bonding mutually cobalt form, and mainly adopt preliminary shaping and radiation heating sintering process to be prepared.Cobalt belongs to the national strategy resource, cost an arm and a leg, and its hot strength, high temperature creep drag and corrosion resistance nature is relatively low, thereby has limited to a certain extent with the application of cobalt as bonding phase carboloy.Because the radiation heating sintering process time is long, energy consumption is big, sintering temperature is higher, and organizing of the agglomerated material of acquisition is thicker, the agglomerated material performance is on the low side again; In addition, owing to do not have sintering pressure in the sintering process, the dimensional precision difficulty that causes controlling agglomerated material is bigger, has also limited the application of such material to a certain extent.
Plum is bright just to equal the article " Ni that delivered on volume the 1st phase " Wuhan Polytechnical Univ's journal " in 1996 the 18th 3The order of Al, fragility and plasticity " and the Chen Jin smoke tree equal the article " Ni that delivered on volume the 1st phase " material Leader " in 2006 the 20th 3The research of Al base alloy with use progress " point out Ni 3The Al intermetallic compound not only has high hard, the high-strength and excellent corrosion resistance nature under the room temperature, and has excellent hot strength and high temperature creep drag, the positive temperature effect that particularly has peak temperature (800～1000 ℃) following intensity and hardness; By to Ni 3Add the right amount of boron element among the Al, this intermetallic compound also has good temperature-room type plasticity and toughness.Rope advances the article that equality delivers on calendar year 2001 the 22nd volume the 6th phase " welding journal " " adds WC and improves Ni 3The welding property of Al " in point out Ni 3Al also has good wettability to wolfram varbide.In addition, Ni 3The moiety of Al is nickel, aluminium, and resource is than horn of plenty, and especially the price of aluminium is very cheap; The Ni that generates by nickel-aluminium reaction in the sintering process 3The Al intermetallic compound can suppress growing up of tungsten carbide crystal grain, the refinement sintering structure.Therefore prediction theoretically is to add the toughness reinforcing Ni of boron 3Al replaces the bonding phase of cobalt as wolfram varbide, can improve its hardness, corrosion resistance nature, hot strength and high temperature creep drag in the room-temperature mechanical property that does not weaken the sintered state carbon tungsten alloy, and application prospect is boundless.But give full play to toughness reinforcing Ni 3Al is the performance advantage of carboloy of bonding phase, and makes its industrialization, still needs by composition proportion and the preparation technology who deeply gropes alloy material, suppresses growing up and reducing the porosity of sintered alloy material of tungsten carbide crystal grain in the sintering process.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art part, provide a kind of with toughness reinforcing Ni 3The Al intermetallic compound replaces the tungsten carbide material of strategic resource cobalt as the bonding phase.
The present invention also aims to combine, a kind of over-all properties that can further improve material be provided, simplify technology by reasonable component design and optimal preparation technology, reduction material produce cost with toughness reinforcing Ni 3The Al intermetallic compound is the preparation method of the tungsten carbide material of bonding phase.
A kind of with Ni 3Al is characterized in that in this material mixture ratio with toughness reinforcing Ni for the tungsten carbide material of bonding phase 3The Al intermetallic compound replaces the cobalt of tradition bonding phase, and its component and mass percentage content thereof are as follows: WC 86～95%, toughness reinforcing Ni 3Al5-14%, all the other are inevitable trace impurity.
For realizing the present invention better, described toughness reinforcing Ni 3Al component and mass percentage content thereof are: Ni 86.65%, Al12.92%, and B 0.43%.
Above-mentioned is this with Ni 3Al is characterized in that for the preparation method of the tungsten carbide material of bonding phase this method comprises the steps:
Step 1: the composition design of tungsten carbide base carbide alloy powder
WC, Ni, Al and B powder are carried out proportioning: WC 86～95%, Ni4.33-12.13%, Al 0.65-1.81%, B 0.02-0.06% by following mass percent consumption, and all the other are inevitable trace impurity;
Step 2: high-energy ball milling prepares cemented carbide powder
Feed intake by above-mentioned raw materials powder quality per-cent consumption and to carry out ball milling, WC powder crystal grain is refined to 100nm at least in ball-milled powder;
Step 3: electric current sintering ball-milled powder
With the Wimet ball-milled powder that the is refined to 100nm at least electric current sintering mould of packing into, adopt the electric current Fast Sintering, electric current Fast Sintering processing condition are as follows:
The sintering current type: square-wave pulse is or/and continuous current;
Sintering pressure: 10MPa～50MPa;
Sintering time: 2～8 minutes.
The present invention compared with prior art has the following advantages:
1, adopting the tungsten carbide material of the present invention's preparation is tungsten carbide base carbide alloy, has realized with toughness reinforcing Ni 3The Al intermetallic compound replaces traditional cobalt as the bonding phase, the tungsten carbide base carbide alloy of cobalt binder phase commonly used in the present industrial production, because of the aluminium price is cheap more than cobalt, thereby reduced the material cost of Wimet, the use of also having saved national strategy resource cobalt simultaneously.
2, adopt the tungsten carbide base carbide alloy of the present invention's preparation, its bonding is toughness reinforcing Ni mutually 3The Al intermetallic compound.Add the toughness reinforcing Ni of boron 3Al has good temperature-room type plasticity and toughness, and makes wolfram varbide have good wettability.Toughness reinforcing Ni 3Al compares with cobalt, not only have more high rigidity under the room temperature, more high strength and more excellent corrosion resistance nature, and have more excellent hot strength and high temperature creep drag, particularly have the positive temperature effect of peak temperature (800～1000 ℃) following intensity and hardness.In addition, the Ni that generates by nickel-aluminium reaction in the sintering process 3Al intermetallic compound also tool suppresses the effect that tungsten carbide crystal grain is grown up.Thereby in the room-temperature mechanical property that does not weaken the sintered state carbon tungsten alloy, its hardness, corrosion resistance nature, hot strength and high temperature creep drag have been improved.
3, the electric current sintering technology that adopts of the present invention, in order to the electricity consumption sintering process time short and sintering temperature is relatively low and sintering process in the Ni that forms between nickel-aluminium 3The Al intermetallic compound can suppress characteristics such as growing up of tungsten carbide crystal grain, and the refinement sintering structure obtains ultra-fine crystalline substance even nanocrystalline material, and utilizes sintering pressure to improve sintered density.Compare with traditional radiation heating sintering process, adopt the electric current sintering method not only the thermo-efficiency height, sintering temperature is low, sintering time is short, sintered state organize more tiny even, porosity is low, and the shape and size precision of sintered compact is easy to control, in addition, powder forming and sintering integratedization, do not need preliminary shaping, the material preparation process route is simplified, and can reduce the material preparation cost.
4, the over-all properties of the material of the present invention's preparation is higher than the similar alloy that adopts traditional radiation addition sintering method preparation, is a kind of comparatively ideal cutter material.
5, to sum up, the material of the present invention's preparation has good popularizing application prospect.
Embodiment
The invention will be further described by following embodiment, but embodiments of the present invention are not limited only to this.
Embodiment 1:
Step 1: the composition design of tungsten carbide base carbide alloy powder
WC, Ni, Al and B powder are carried out proportioning by following mass percent consumption:
WC：95.00％，
Ni：4.33％，
Al：0.65％，
B：0.02％，
Contain inevitable trace impurity.
The WC powder that the WC raw material adopts blue tungsten powder to produce along the hydrogen reduction carborization, the about 3 μ m of its average particulate diameter, about 0.5～0.8 μ m of crystal grain; Ni, Al and B add with simple substance form, the about 75 μ m of powder flat diameter particle diameter, and purity is greater than 99.9%.
Step 2: high-energy ball milling prepares cemented carbide powder
Carry out the disposable ball milling that feeds intake by above-mentioned powder stock mass percent consumption.Mechanical milling process is finished in planetary ball mill, and the abrading-ball material adopts the WC Wimet, and ratio of grinding media to material is 10: 1, and ball milling speed is 266r/min, and adopts high-purity Ar gas as protective atmosphere.The ball milling time is 50 hours, and this moment, WC powder crystal grain was refined to below the 100nm.
Step 3: electric current sintering ball-milled powder
20g is refined to Wimet ball-milled powder below the 100nm, and the diameter of packing into is to carry out the electric current Fast Sintering in the ceramic post sintering mould of φ 20mm, and electric current Fast Sintering processing condition are as follows:
By applying 2 minutes square wave pulsed current earlier, and then apply 6 minutes continuous currents again powder is carried out Fast Sintering.Wherein, the peak value of pulsed current, base value, frequency and dutycycle are respectively 3000A, 360A, 50Hz and 55%, and continuous current is 1500A.In the whole process of energising sintering, body of powder is applied the 30MPa sintering pressure by positive and negative electrode.
The density of the WC based hard alloy material that obtains through 8 minutes sintering is 14.5g/cm 3, the about 250nm of the grain-size of WC, normal temperature hardness and bending strength are respectively 1940HV and 4003MPa.
Embodiment 2:
Step 1: the composition design of tungsten carbide base carbide alloy powder
WC, Ni, Al and B powder are carried out proportioning by following mass percent consumption:
WC：86.00％，
Ni：12.13％，
Al：1.81％，
B：0.06％，
Contain inevitable trace impurity.
The WC powder that the WC raw material adopts blue tungsten powder to produce along the hydrogen reduction carborization, the about 3 μ m of its average particulate diameter, about 0.5～0.8 μ m of crystal grain; Ni, Al and B add with simple substance form, the about 75 μ m of powder flat diameter particle diameter, and purity is greater than 99.9%.
Step 2: high-energy ball milling prepares cemented carbide powder
Carry out the disposable ball milling that feeds intake by above-mentioned powder stock mass percent consumption.Mechanical milling process is finished in planetary ball mill, and the abrading-ball material adopts the WC Wimet, and ratio of grinding media to material is 10: 1, and ball milling speed is 266r/min, and adopts high-purity Ar gas as protective atmosphere.The ball milling time is 50 hours, and this moment, WC powder crystal grain was refined to below the 100nm.
Step 3: electric current sintering ball-milled powder
20g is refined to Wimet ball-milled powder below the 100nm, and the diameter of packing into is to carry out the electric current Fast Sintering in the ceramic post sintering mould of φ 20mm, and electric current Fast Sintering processing condition are as follows:
By applying 2 minutes square wave pulsed current.Wherein, the peak value of pulsed current, base value, frequency and dutycycle are respectively 3000A, 360A, 50Hz and 65%.In the whole process of energising sintering, body of powder is applied the 50MPa sintering pressure by positive and negative electrode.
The density of the WC based hard alloy material that obtains through 2 minutes sintering is 14.3g/cm 3, the about 240nm of the grain-size of WC, normal temperature hardness and bending strength are respectively 1850HV and 4115MPa.
Embodiment 3:
Step 1: the composition design of tungsten carbide base carbide alloy powder
WC, Ni, Al and B powder art are carried out proportioning by following mass percent consumption:
WC：90.00％，
Ni：8.67％，
Al：1.29％，
B：0.04％，
Contain inevitable trace impurity.
The WC powder that the WC raw material adopts blue tungsten powder to produce along the hydrogen reduction carborization, the about 3 μ m of its average particulate diameter, about 0.5～0.8 μ m of crystal grain; Ni, Al and B add with simple substance form, the about 75 μ m of powder flat diameter particle diameter, and purity is greater than 99.9%.
Step 2: high-energy ball milling prepares cemented carbide powder
Carry out the disposable ball milling that feeds intake by above-mentioned powder stock mass percent consumption.Mechanical milling process is finished in planetary ball mill, and the abrading-ball material adopts the WC Wimet, and ratio of grinding media to material is 10: 1, and ball milling speed is 266r/min, and adopts high-purity Ar gas as protective atmosphere.The ball milling time is 50 hours, and this moment, WC powder crystal grain was refined to below the 100nm.
Step 3: electric current sintering ball-milled powder
20g is refined to Wimet ball-milled powder below the 100nm, and the diameter of packing into is to carry out the electric current Fast Sintering in the ceramic post sintering mould of φ 20mm, and electric current Fast Sintering processing condition are as follows:
By applying 6 minutes 1550A continuous current.In the whole process of energising sintering, body of powder is applied the 10MPa sintering pressure by positive and negative electrode.The density of the WC based hard alloy material that obtains through 6 minutes sintering is 14.4g/cm 3, the about 280nm of the grain-size of WC, normal temperature hardness and bending strength are respectively 1870HV and 3868MPa.

Claims (3)

1, a kind of with Ni 3Al is characterized in that in this material mixture ratio with toughness reinforcing Ni for the tungsten carbide material of bonding phase 3The Al intermetallic compound replaces the cobalt of tradition bonding phase, and its component and mass percentage content thereof are as follows: WC 86～95%, toughness reinforcing Ni 3Al 5-14%, all the other are inevitable trace impurity.
2, according to claim 1 a kind of with Ni 3Al is characterized in that described toughness reinforcing Ni for the tungsten carbide material of bonding phase 3Al component and mass percentage content thereof are: Ni 86.65%, and Al 12.92%, and B 0.43%.
3, claim 1 is described a kind of with Ni 3Al is characterized in that for the preparation method of the tungsten carbide material of bonding phase this method comprises the steps:
Step 1: the composition design of tungsten carbide base carbide alloy powder
WC, Ni, Al and B powder are carried out proportioning: WC 86～95%, Ni4.33-12.13%, Al 0.65-1.81%, B 0.02-0.06% by following mass percent consumption, and all the other are inevitable trace impurity;
Step 2: high-energy ball milling prepares cemented carbide powder
Feed intake by above-mentioned raw materials powder quality per-cent consumption and to carry out ball milling, WC powder crystal grain is refined to 100nm at least in ball-milled powder;
Step 3: electric current sintering ball-milled powder
With the ball-milled powder electric current sintering mould of packing into, adopt the electric current Fast Sintering, electric current Fast Sintering processing condition are as follows:
The sintering current type: square-wave pulse is or/and continuous current;
Sintering pressure: 10MPa～50MPa;
Sintering time: 2～8 minutes.
CNA2008100290206A 2008-06-25 2008-06-25 Tungsten carbide material with Ni3Al as cementing phase and preparation thereof Pending CN101323925A (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102140603A (en) * 2011-03-24 2011-08-03 株洲硬质合金集团有限公司 Hard alloy using nickel-aluminum intermetallic compound Ni3Al as bonding phase and preparation method thereof
CN102154582A (en) * 2011-05-27 2011-08-17 株洲硬质合金集团有限公司 Hard alloy taking nickel-aluminium intermetallic compound Ni3Al as binding phase and preparation method
CN102162058A (en) * 2011-04-07 2011-08-24 株洲硬质合金集团有限公司 Hard alloy taking nickel-aluminum intermetallic compound Ni3Al as binding phase and preparation method thereof
CN105154707A (en) * 2015-10-26 2015-12-16 河海大学 Preparation method and application of wolfram carbide (WC) composite
CN105907997A (en) * 2016-06-02 2016-08-31 华南理工大学 In-situ synthesis nano Al2O3 and toughened WC-Ni3Al composite material and preparation method thereof
CN106319271A (en) * 2016-10-28 2017-01-11 成都理工大学 Preparation method for hard alloy in-situ generated by Ni3Al in binding phase
CN106367652A (en) * 2016-09-18 2017-02-01 广东工业大学 Cemented carbide particle, preparing method of cemented carbide particle, cemented carbide and preparing method of cemented carbide
CN106498257A (en) * 2016-10-28 2017-03-15 成都理工大学 In-situ preparation contains Ni3The preparation method of the hard alloy of the Binder Phase of Al
CN106521207A (en) * 2016-10-28 2017-03-22 成都理工大学 Method for preparing hard alloy capable of resisting high temperature softening
CN106591747A (en) * 2016-12-14 2017-04-26 华南理工大学 Beta-Si3N4 whisker and Ni3Al binding phase synergistic toughened WC composite and preparation method thereof
CN106636835A (en) * 2016-10-28 2017-05-10 成都理工大学 Preparation method for hard alloy containing intermetallic compound bonding phase
CN108588462A (en) * 2018-06-14 2018-09-28 陕西理工大学 Complex phase is total to the preparation method of enhancing hard alloy material
WO2019078109A1 (en) * 2017-10-19 2019-04-25 株式会社リード Hard sintered body and rotary tool using same

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102140603B (en) * 2011-03-24 2012-12-19 株洲硬质合金集团有限公司 Preparation method of hard alloy using nickel-aluminum intermetallic compound Ni3Al as bonding phase
CN102140603A (en) * 2011-03-24 2011-08-03 株洲硬质合金集团有限公司 Hard alloy using nickel-aluminum intermetallic compound Ni3Al as bonding phase and preparation method thereof
CN102162058A (en) * 2011-04-07 2011-08-24 株洲硬质合金集团有限公司 Hard alloy taking nickel-aluminum intermetallic compound Ni3Al as binding phase and preparation method thereof
CN102162058B (en) * 2011-04-07 2012-10-10 株洲硬质合金集团有限公司 Hard alloy taking nickel-aluminum intermetallic compound Ni3Al as binding phase and preparation method thereof
CN102154582A (en) * 2011-05-27 2011-08-17 株洲硬质合金集团有限公司 Hard alloy taking nickel-aluminium intermetallic compound Ni3Al as binding phase and preparation method
CN102154582B (en) * 2011-05-27 2013-01-30 株洲硬质合金集团有限公司 Preparation method of hard alloy taking nickel-aluminium intermetallic compound Ni3Al as binding phase
CN105154707A (en) * 2015-10-26 2015-12-16 河海大学 Preparation method and application of wolfram carbide (WC) composite
CN105907997A (en) * 2016-06-02 2016-08-31 华南理工大学 In-situ synthesis nano Al2O3 and toughened WC-Ni3Al composite material and preparation method thereof
CN106367652B (en) * 2016-09-18 2018-05-18 广东工业大学 A kind of hard alloy particle and preparation method thereof and hard alloy and preparation method thereof
CN106367652A (en) * 2016-09-18 2017-02-01 广东工业大学 Cemented carbide particle, preparing method of cemented carbide particle, cemented carbide and preparing method of cemented carbide
CN106319271A (en) * 2016-10-28 2017-01-11 成都理工大学 Preparation method for hard alloy in-situ generated by Ni3Al in binding phase
CN106521207A (en) * 2016-10-28 2017-03-22 成都理工大学 Method for preparing hard alloy capable of resisting high temperature softening
CN106636835A (en) * 2016-10-28 2017-05-10 成都理工大学 Preparation method for hard alloy containing intermetallic compound bonding phase
CN106319271B (en) * 2016-10-28 2018-01-30 成都理工大学 Ni in Binder Phase3The generated in-situ hard alloy preparation methods of Al
CN106498257A (en) * 2016-10-28 2017-03-15 成都理工大学 In-situ preparation contains Ni3The preparation method of the hard alloy of the Binder Phase of Al
CN106591747A (en) * 2016-12-14 2017-04-26 华南理工大学 Beta-Si3N4 whisker and Ni3Al binding phase synergistic toughened WC composite and preparation method thereof
WO2019078109A1 (en) * 2017-10-19 2019-04-25 株式会社リード Hard sintered body and rotary tool using same
CN108588462A (en) * 2018-06-14 2018-09-28 陕西理工大学 Complex phase is total to the preparation method of enhancing hard alloy material

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Open date: 20081217