CN105965007B - A kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings - Google Patents

A kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings Download PDF

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Publication number
CN105965007B
CN105965007B CN201610341527.XA CN201610341527A CN105965007B CN 105965007 B CN105965007 B CN 105965007B CN 201610341527 A CN201610341527 A CN 201610341527A CN 105965007 B CN105965007 B CN 105965007B
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atmosphere
powder
speed
sintering
speed steels
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CN105965007A (en
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李松林
欧阳齐
黄雍平
张丰丽
滕浩
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Central South University
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Central South University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • B22F3/101Changing atmosphere
    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/02Making ferrous alloys by powder metallurgy
    • C22C33/0207Using a mixture of prealloyed powders or a master alloy
    • C22C33/0228Using a mixture of prealloyed powders or a master alloy comprising other non-metallic compounds or more than 5% of graphite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention relates to a kind of methods for preparing Powder High-speed Steels;A kind of more particularly to method for preparing Powder High-speed Steels using more atmosphere assisted sinterings.The present invention uniformly mixes pre-alloyed High Speed Steel Powders and additive powder and cold-press moulding, and the sintering to green compact is once completed using vacuum atmosphere, stage middle and later periods nitrogen atmosphere and three stage of argon pressurization atmosphere control climate.Cold stage can eliminate most of hole in green compact using vacuum atmosphere while binder is removed, and obtain higher pre-sintered consistency;Sintering can realize Powder High-speed Steels in-situ preparation nitride strengthening phase in nitrogen atmosphere, improve the mechanical property of sintered state Powder High-speed Steels, and reduce maximum sintering temperature;The pressurization of later stage argon gas atmosphere is sintered, remaining hole can be abolished, further improves the consistency of Powder High-speed Steels.Compared with conventional sintering method, atmosphere assisted sintering technique is easily controllable, expands sintering window while reducing sintering temperature, improves the consistency and mechanical property of Powder High-speed Steels.

Description

A kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings
Technical field
The present invention relates to a kind of methods for preparing Powder High-speed Steels;It is more particularly to a kind of using the preparation of more atmosphere assisted sinterings The method of Powder High-speed Steels.
Background technology
Powder High-speed Steels are by shaping and being sintered or subsequent processing is and manufactured high speed steel high-speed steel attritive powder Product (abbreviation PM HSS).Powder High-speed Steels have the characteristics such as segregation-free, crystal grain is tiny, inclusion content is few, even tissue, because This its mechanical property such as hardness, intensity, toughness etc. are substantially better than common high-speed steel prepared by traditional melting-casting forging method, extensively Applied to lathe tool, milling cutter, gear hob, drill bit, mold and other high temperature resistants and wear-resisting spare part.
Shaping and sintering are the key that determine high-speed steel shape and performance preparation process.The shaping of conventional powder high-speed steel and Sintering technology has the technologies such as hot pressing, hot isostatic pressing, powder injection forming, molding/sintering.Hot pressing can be obtained close to fully dense Powder High-speed Steels, but hot-press equipment is complicated, cost is higher;Hot isostatic pressing technique can obtain high density and uniformly tiny, more The carbide tissue of distribution is dissipated, Powder High-speed Steels properties of product are high, but hot isostatic apparatus investment is big, is only suitable for preparing big ruler Very little product;Powder Injection Molding Technology can improve stock utilization, reduce amount of machining, but can only prepare the smaller production of size Product, and the binding agent removing time is long;To be slightly above the liquidus temperature of solidus in molding/sintering technology generally use vacuum atmosphere Sintering, i.e. vacuum-sintering, this method can prepare complex-shaped powder metallurgy parts, have significantly compared with technologies such as hot isostatic pressings Cost advantage has good development prospect.But molding/sintering technology sintering temperature is high, sintering range (sintering window) The consistency that narrow and vacuum-sintering obtains is less high (generally below the 98% of real density), cause mechanical property less than hot pressing and Powder High-speed Steels prepared by the technologies such as hot isostatic pressing.
The content of the invention
For conventional moulded/sintering process, there are sintering temperature is high, sintering window narrows, sintered density are relatively low, mechanical property The deficiencies of not high enough, the present invention provides a kind of methods for preparing Powder High-speed Steels using more atmosphere assisted sinterings.
A kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;High-speed steel raw material powder is suppressed After shaping, carry out that atmosphere is once sintered to obtain high-speed steel by changing under vacuum atmosphere, under nitrogen containing atmosphere, high-pressure atmosphere successively Product.
A kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;By master alloy powder and additive After mixing, high-speed steel raw material powder is obtained;The master alloy powder is commercially available High Speed Steel Powders;The additive is carbon dust And zinc stearate.
Preferably, a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;The height In fast powdered steel, the content of vanadium is more than or equal to 3wt.%.As further preferred embodiment, the granularity of the High Speed Steel Powders is small In equal to 100 mesh, and oxygen content is less than 1000ppm.As further preferred embodiment, the High Speed Steel Powders are selected from height Fast steel T15 powder, high-speed steel T42 powder, high-speed steel M4 powder, high-speed steel M3:One kind in the high V content powder such as 2.
Preferably, a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;Carbon dust Dosage is 0.1~0.5wt.% of master alloy powder gross mass;The dosage of zinc stearate for master alloy powder gross mass 0.6~ 1wt%.
Preferably;A kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;The carbon Powder is the aquadag that granularity is 1~3 μm.
A kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;During compression moulding, pressure is controlled For 600~800MPa.
Preferably, a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;It is described true Air atmosphere is the atmosphere that vacuum degree is less than or equal to 1Pa.As further preferred embodiment, sintering temperature of the green compact under vacuum atmosphere It spends for 1000~1040 DEG C.
Preferably, a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;It is described to contain Blanket of nitrogen is nitrogen atmosphere;The pressure of the nitrogen atmosphere is 0.01~1bar.As further preferred embodiment, green compact is in nitrogen Under gas atmosphere 30~60min is sintered in 1150~1200 DEG C.
Preferably, a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;The height Atmosphere of calming the anger is argon gas atmosphere;The pressure of the argon gas atmosphere is 5~20MPa.As further preferred embodiment, green compact is in argon gas Under atmosphere 10~30min is sintered in 10-50 DEG C of Powder High-speed Steels solidus more than (such as 1230~1270 DEG C).
Preferably, a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings of the present invention;Including under State step:
Step 1,
High Speed Steel Powders and additive are placed in V-type batch mixer and are uniformly mixed;In the High Speed Steel Powders, the content of vanadium More than or equal to 3wt.%;The additive is carbon dust and zinc stearate;The dosage of the carbon dust is High Speed Steel Powders gross mass 0.1~0.5%;The dosage of zinc stearate is the 0.6~1% of High Speed Steel Powders gross mass;
Step 2
Mixed powder is molded using pressing machine die, and pressure is 600~800MPa;
Step 3
The sample suppressed first is sintered to liquid phase in 1000~1040 DEG C in atmosphere of the vacuum degree less than or equal to 1Pa to open Begin to be formed;Nitrogen is then passed to, and it is 0.01~1bar to control sintering pressure in stove;Then green compact is heated to 1150~1200 DEG C and keep the temperature 30~60min, be preferably 60min;Then 10-50 DEG C (such as 1230 of Powder High-speed Steels solidus more than is warming up to again ~1270 DEG C), it is 5~20MPa to be passed through air pressure in argon gas to stove, is preferably 10~30min of heat preservation, cooling, release after 30min; Obtain Powder High-speed Steels material.
The present invention suppresses the green body of variously-shaped complexity by being commonly molded.
Principle and advantage
The present invention is by being sintered vacuum atmosphere early period, intermediate and final stages of sintering stage nitrogen atmosphere and sintering later stage argon pressurization gas The synergistic effect of the triphasic control climate of atmosphere can obtain consistency higher Powder High-speed Steels, while can also improve powder height The mechanical property of fast steel sintered body.
Vacuum atmosphere of the present invention can fully reduce the oxide in Powder High-speed Steels green compact, and acceleration of sintering carries out.
Stage middle and later periods of the invention, which passes to nitrogen atmosphere, can utilize N2Substitute the part carbon in high-speed steel green body, and and vanadium Form vanadium nitride or vanadium carbide nitride hardening constituent, vanadium nitride or vanadium carbide nitride can pinning crystal boundary may also suppress crystal grain and grow up;And it replaces Carbon separate out out is diffused into matrix, and the solidus temperature that can reduce matrix is conducive to be densified.Nitrogen atmosphere is burnt simultaneously Knot can realize Powder High-speed Steels in-situ preparation nitride strengthening phase, improve the mechanical property of Powder High-speed Steels, reduce most high fever Junction temperature;
The present invention is destroyed residual porosity wall by the effect of gas pressure using argon pressurization atmosphere in the sintering later stage, is promoted Liquid phase flows and atoms permeating carries out, and achievees the effect that further improve green density.
The present invention achieves unexpected effect, has obtained consistency by the synergistic effect of each sintering stage in a word High, the Powder High-speed Steels sintered body of good mechanical performance.
Specific embodiment
Embodiment 1
Step 1, master alloy powder and additive are placed in V-type batch mixer and are uniformly mixed.Wherein master alloy powder is city Common M3 on face:2 High Speed Steel Powders, additive is carbon dust, zinc stearate, and dosage is respectively compared with master alloy total amount: Carbon dust 0.1wt.% and zinc stearate 0.6wt.%.
Step 2, mixed powder is molded to preforming, pressure 600MPa using forcing press.
Step 3, the sample suppressed is first sintered 60min, green compact heating under 1Pa vacuum atmospheres at a temperature of 1000 DEG C To 1070 DEG C of nitrogen for being passed through 1bar (in-situ preparation for promoting nitride strengthening phase), then green compact is heated to 1150 DEG C and is kept the temperature Then 60min is warming up to 1230 DEG C again, be passed through a certain amount of argon gas and keep the temperature 30min, and holding furnace pressure is 5MPa, finally Release cools to room temperature with the furnace.The consistency of sintered state high-speed steel reaches 98.7% after tested, and hardness reaches 58HRC.
Comparative example 1
Other conditions are consistent with embodiment, the difference is that:Using vacuum-sintering during sintering;It is sintered after tested The consistency of state high-speed steel is only 97.3%, and hardness is only 52HRC.
Embodiment 2
Step 1, master alloy powder and additive are placed in V-type batch mixer and are uniformly mixed.Wherein master alloy powder is city Common M3 on face:2 High Speed Steel Powders, additive is carbon dust, zinc stearate, and dosage is respectively compared with master alloy total amount: Carbon dust 0.4wt% and zinc stearate 1wt%.
Step 2, mixed powder is molded to preforming, pressure 800MPa using forcing press.
Step 3, by the sample suppressed first 10-2It is sintered under Pa vacuum atmospheres, green compact is heated to what liquid phase initially formed Lead to the nitrogen (in-situ preparation for promoting nitride strengthening phase) of 0.2bar during temperature, then green compact is heated to 1200 DEG C and is kept the temperature Then 60min is warming up to 1270 DEG C again, be passed through a certain amount of argon gas and keep the temperature 30min, and holding furnace pressure is 20MPa, finally Release cools to room temperature with the furnace.The consistency of sintered state high-speed steel reaches 99.5% after tested, and hardness reaches 54HRC.
Comparative example 2
Other conditions are consistent with embodiment 2, the difference is that:It is not sintered using nitrogen atmosphere;Sintered state after tested The consistency of high-speed steel is only 98.1%, and hardness is only 51HRC.
Embodiment 3
Step 1, master alloy powder and additive are placed in V-type batch mixer and are uniformly mixed.Wherein master alloy powder is city Common T15 High Speed Steel Powders on face, additive is carbon dust, zinc stearate, and dosage is respectively compared with master alloy total amount:Carbon Powder 0.4wt% and zinc stearate 0.8wt%.
Step 2, mixed powder is molded to preforming, pressure 800MPa using forcing press.
Step 3, by the sample suppressed first 10-1It is sintered under Pa vacuum atmospheres, green compact is heated to what liquid phase initially formed Lead to the nitrogen (in-situ preparation for promoting nitride strengthening phase) of 0.5bar during temperature, then green compact is heated to 1180 DEG C and is kept the temperature Then 60min is warming up to 1250 DEG C again, be passed through a certain amount of argon gas and keep the temperature 30min, and holding furnace pressure is 10MPa, finally Release cools to room temperature with the furnace.The consistency of sintered state high-speed steel reaches 99.2% after tested, and hardness reaches 56HRC.
Comparative example 3
Other conditions are consistent with embodiment 3, the difference is that:It is sintered always using high-pressure atmosphere;It is sintered after tested The consistency of state high-speed steel is only 97.8%, and hardness is only 54HRC.

Claims (8)

  1. A kind of 1. method for preparing Powder High-speed Steels using more atmosphere assisted sinterings;It is characterized in that:By high-speed steel raw material powder After compression moulding, by the way that sintering atmosphere in stove is controlled to be sintered successively under vacuum, nitrogenous, high-pressure atmosphere, once sintered To the Powder High-speed Steels of the high fine and close nitrogenate hardening constituent of high-performance;
    The vacuum atmosphere is the atmosphere that vacuum degree is less than or equal to 1Pa;Sintering temperature of the green compact under vacuum atmosphere for 1000~ 1040℃;
    The nitrogen containing atmosphere is nitrogen atmosphere;The pressure of the nitrogen atmosphere is 0.01~1bar;Green compact in a nitrogen atmosphere in 1150~1200 DEG C of 30~60min of sintering;
    The high-pressure atmosphere is argon gas atmosphere;The pressure of the argon gas atmosphere is 5~20MPa;Green compact is under an argon atmosphere in powder Last 10-50 DEG C of 10~30min of sintering of high-speed steel solidus more than.
  2. 2. a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings according to claim 1;It is characterized in that: By master alloy powder and additive after mixing, high-speed steel raw material powder is obtained;The master alloy powder is commercially available high-speed steel Powder;The additive is carbon dust and zinc stearate.
  3. 3. a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings according to claim 2;It is characterized in that: In the High Speed Steel Powders, the content of vanadium is more than or equal to 3wt.%.
  4. 4. a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings according to claim 3;It is characterized in that: The granularity of the High Speed Steel Powders is less than or equal to 100 mesh, and oxygen content is less than 1000ppm.
  5. 5. a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings according to claim 2;It is characterized in that: The dosage of carbon dust is the 0.1~0.5% of master alloy powder gross mass;The dosage of zinc stearate is master alloy powder gross mass 0.6~1%.
  6. 6. a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings according to claim 2;It is characterized in that: The carbon dust is the aquadag that granularity is 1~3 μm.
  7. 7. a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings according to claim 1;It is characterized in that: During compression moulding, it is 600~800MPa to control pressure.
  8. 8. a kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings according to claim 1;It is characterized in that:
    Comprise the following steps:
    Step 1
    High Speed Steel Powders and additive are placed in V-type batch mixer and are uniformly mixed;In the High Speed Steel Powders, the content of vanadium is more than Equal to 3wt.%;The additive is carbon dust and zinc stearate;The dosage of the carbon dust for High Speed Steel Powders gross mass 0.1~ 0.5%;The dosage of zinc stearate is the 0.6~1% of High Speed Steel Powders gross mass;
    Step 2
    Mixed powder is molded using pressing machine die, and pressure is 600~800MPa;
    Step 3
    The sample suppressed is first sintered into liquid phase in 1000~1040 DEG C in atmosphere of the vacuum degree less than or equal to 1Pa and starts shape Into;Nitrogen is then passed to, and it is 0.01~1bar to control sintering pressure in stove;Then green compact is heated to 1150~1200 DEG C simultaneously Keep the temperature 30~60min;Then be warming up to 10-50 DEG C of Powder High-speed Steels solidus more than again, be passed through in argon gas to stove air pressure for 5~ 20MPa, after keeping the temperature 10~30min, cooling, release obtain sintered state Powder High-speed Steels.
CN201610341527.XA 2016-05-20 2016-05-20 A kind of method for preparing Powder High-speed Steels using more atmosphere assisted sinterings Expired - Fee Related CN105965007B (en)

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Publication number Priority date Publication date Assignee Title
CN108746647A (en) * 2018-06-27 2018-11-06 北京金物科技发展有限公司 A kind of preparation method and Powder High-speed Steels of Powder High-speed Steels
CN109570487B (en) * 2018-12-13 2020-12-29 浙江精瑞工模具有限公司 Preparation method of powder high-speed steel
CN114101674B (en) * 2021-11-04 2024-03-22 金上晋科技(东莞)有限公司 Method for improving strength and corrosion resistance of austenitic stainless steel powder injection molding finished product
CN114082950B (en) * 2021-11-04 2024-04-16 金上晋科技(东莞)有限公司 Method for improving mechanical properties of SUS630 stainless steel injection molding finished product

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CN103157796A (en) * 2013-04-10 2013-06-19 湖南环宇粉末冶金有限公司 Method of forming powder metallurgy tool steel
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