CN111705251A - Method for improving toughness of hard alloy - Google Patents

Method for improving toughness of hard alloy Download PDF

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Publication number
CN111705251A
CN111705251A CN202010701404.9A CN202010701404A CN111705251A CN 111705251 A CN111705251 A CN 111705251A CN 202010701404 A CN202010701404 A CN 202010701404A CN 111705251 A CN111705251 A CN 111705251A
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China
Prior art keywords
temperature
parts
hard alloy
toughness
sintering
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CN202010701404.9A
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Chinese (zh)
Inventor
叶惠明
叶少良
诸优明
叶戈
廖晓虹
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Guangdong Zhengxin Hard Material Technology Research And Development Co ltd
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Guangdong Zhengxin Hard Material Technology Research And Development Co ltd
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Priority to CN202010701404.9A priority Critical patent/CN111705251A/en
Publication of CN111705251A publication Critical patent/CN111705251A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/08Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/067Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder

Abstract

The invention discloses a method for improving the toughness of hard alloy, which comprises the following steps: wet milling to prepare powder, taking 70-85 parts of tungsten carbide, 10-25 parts of hydrofluoric acid, 5-11 parts of Co, 3-15 parts of titanium carbide and 6-8 parts of nickel according to parts by weight, mixing, adding into a wet mill, and ball-milling for 55-70 hours; then, sieving the mixed slurry with a 350-mesh sieve, discharging and precipitating, and separating a supernatant medium; drying, adding low-melting-point paraffin into the mixed slurry, stirring to dry the mixed slurry, then sieving with a 400-mesh sieve, and filtering to remove impurities; forming, namely adding the dried material into a mixer, adding a forming agent, uniformly stirring, and then performing compression forming to obtain blank hard alloy; and sintering the blank hard alloy, and cooling after sintering to obtain the finished hard alloy. The invention effectively improves the toughness of the hard alloy, is not easy to crack, has the characteristics of high strength and high hardness, has excellent wear resistance and thermal fatigue resistance, and is suitable for stable work in severe environment.

Description

Method for improving toughness of hard alloy
Technical Field
The invention belongs to the technical field of hard alloy processing, and particularly relates to a method for improving toughness of hard alloy.
Background
The high-strength tough hard alloy material is a novel product, and the product not only has the stability of the hard alloy material, but also has the characteristics of high strength and high hardness, and has stable working performance. Various indexes accord with the stability of hard alloy, and the wholeness can be superior, and the structure is special, has its unique positive meaning again, and stable performance in addition, can open up a new way in future market, win the biggest market. The existing processing method is difficult to achieve high strength and high hardness, requires stable performance of an alloy machine body, is not easy to damage when working in a stamping friction environment, and has high stability.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for improving the toughness of hard alloy.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method of increasing the toughness of cemented carbide comprising the steps of:
wet milling to prepare powder, taking 70-85 parts of tungsten carbide, 10-25 parts of hydrofluoric acid, 5-11 parts of Co, 3-15 parts of titanium carbide and 6-8 parts of nickel according to parts by weight, mixing, adding into a wet mill, and ball-milling for 55-70 hours; then, sieving the mixed slurry with a 350-mesh sieve, discharging and precipitating, and separating a supernatant medium;
drying, adding low-melting-point paraffin into the mixed slurry, stirring to dry the mixed slurry, then sieving with a 400-mesh sieve, and filtering to remove impurities;
forming, namely adding the dried material into a mixer, adding a forming agent, uniformly stirring, and then performing compression forming to obtain blank hard alloy;
and sintering the blank hard alloy, and cooling after sintering to obtain the finished hard alloy.
The tungsten carbide comprises particles of two particle size sizes with an average particle size of 3 μm and 6 μm.
When the wet milling is carried out to prepare powder, solvent oil is added, and the amount of the added solvent oil is 20-30% of the total amount of tungsten carbide, hydrofluoric acid, Co, titanium carbide and nickel.
During sintering, a three-section heating mode is adopted under the argon atmosphere condition;
in the first stage, under the pressure condition of 10-15 MPa, the temperature is raised from room temperature to 500 ℃ at the temperature raising speed of 3-5 ℃/min, and the temperature is kept constant for 30-60 min;
in the second stage, the temperature is increased from 500 ℃ to 1000-1100 ℃ at the temperature increase speed of 8-10 ℃/min, and the temperature is kept for 30-60 min at constant temperature;
and in the third stage, the temperature is increased from 1000-1100 ℃ to 1500-1550 ℃ at the temperature increase speed of 3-5 ℃/min, and the temperature is kept for 30-45 min at constant temperature.
The sintering is a vacuum sintering method, a low-pressure sintering method or a plasma sintering method.
The forming agent is fully refined paraffin with the melting point of 58 ℃.
The titanium carbide has a fisher's average particle size of 1.5 um.
The invention effectively improves the toughness of the hard alloy, is not easy to crack, has the characteristics of high strength and high hardness, has excellent wear resistance and thermal fatigue resistance, and is suitable for stable work in severe environment.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to further understand the features and technical means of the invention and achieve specific objects and functions.
Example one
A method of increasing the toughness of cemented carbide comprising the steps of:
wet milling to prepare powder, taking 70 parts of tungsten carbide, 10 parts of hydrofluoric acid, 5 parts of Co, 3 parts of titanium carbide and 6 parts of nickel according to parts by weight, mixing, adding into a wet mill, and ball-milling for 55 hours; and then, sieving the mixed slurry with a 350-mesh sieve, discharging and precipitating, and separating a supernatant medium.
Drying, adding low-melting-point paraffin into the mixed slurry, stirring to dry the mixed slurry, then sieving with a 400-mesh sieve, and filtering to remove impurities.
And (3) forming, namely adding the dried material into a mixer, adding a forming agent, uniformly stirring, and then performing compression forming to obtain the blank hard alloy.
And sintering the blank hard alloy, and cooling after sintering to obtain the finished hard alloy.
The tungsten carbide comprises particles of two particle size sizes with an average particle size of 3 μm and 6 μm.
When the wet milling is carried out to prepare powder, solvent oil is added, and the amount of the added solvent oil is 20% of the total amount of tungsten carbide, hydrofluoric acid, Co, titanium carbide and nickel.
During sintering, a three-section heating mode is adopted under the argon atmosphere condition;
in the first stage, under the pressure condition of 10MPa, the temperature is raised from room temperature to 500 ℃ at the temperature raising speed of 3 ℃/min, and the temperature is kept for 30min at constant temperature.
In the second stage, the temperature is raised from 500 ℃ to 1000 ℃ at the temperature raising speed of 8 ℃/min, and the temperature is kept for 30min at constant temperature.
In the third stage, the temperature is raised from 1000 ℃ to 1500 ℃ at the heating rate of 3 ℃/min, and the temperature is kept for 30min at constant temperature.
The sintering is a vacuum sintering method. The forming agent is fully refined paraffin with the melting point of 58 ℃. The tungsten carbide has a fischer-tropsch average particle size of 3 um.
Example two
A method of increasing the toughness of cemented carbide comprising the steps of:
wet milling to prepare powder, taking 80 parts of tungsten carbide, 20 parts of hydrofluoric acid, 7 parts of Co, 10 parts of titanium carbide and 7 parts of nickel according to parts by weight, mixing, adding into a wet mill, and ball-milling for 65 hours; and then, sieving the mixed slurry with a 350-mesh sieve, discharging and precipitating, and separating a supernatant medium.
Drying, adding low-melting-point paraffin into the mixed slurry, stirring to dry the mixed slurry, then sieving with a 400-mesh sieve, and filtering to remove impurities.
And (3) forming, namely adding the dried material into a mixer, adding a forming agent, uniformly stirring, and then performing compression forming to obtain the blank hard alloy.
And sintering the blank hard alloy, and cooling after sintering to obtain the finished hard alloy.
The tungsten carbide comprises particles of two particle size sizes with an average particle size of 3 μm and 6 μm.
And when the wet milling is carried out to prepare powder, adding solvent oil, wherein the amount of the added solvent oil is 25% of the total amount of tungsten carbide, hydrofluoric acid, Co, titanium carbide and nickel.
During sintering, a three-section heating mode is adopted under the argon atmosphere condition;
in the first stage, under the pressure condition of 12MPa, the temperature is raised from room temperature to 500 ℃ at the temperature raising speed of 4 ℃/min, and the temperature is kept for 50min at constant temperature.
In the second stage, the temperature is raised from 500 ℃ to 1050 ℃ at the temperature raising speed of 9 ℃/min, and the temperature is kept for 40min at constant temperature.
And in the third stage, the temperature is increased from 1050 ℃ to 1520 ℃ at the heating rate of 4 ℃/min, and the constant temperature is kept for 40 min.
The sintering is a low pressure sintering process. The forming agent is fully refined paraffin with the melting point of 58 ℃.
EXAMPLE III
A method of increasing the toughness of cemented carbide comprising the steps of:
wet milling to prepare powder, taking 85 parts of tungsten carbide, 25 parts of hydrofluoric acid, 11 parts of Co, 15 parts of titanium carbide and 8 parts of nickel according to parts by weight, mixing, adding into a wet mill, and ball-milling for 70 hours; and then, sieving the mixed slurry with a 350-mesh sieve, discharging and precipitating, and separating a supernatant medium.
Drying, adding low-melting-point paraffin into the mixed slurry, stirring to dry the mixed slurry, then sieving with a 400-mesh sieve, and filtering to remove impurities.
And (3) forming, namely adding the dried material into a mixer, adding a forming agent, uniformly stirring, and then performing compression forming to obtain the blank hard alloy.
And sintering the blank hard alloy, and cooling after sintering to obtain the finished hard alloy.
The tungsten carbide comprises particles of two particle size sizes with an average particle size of 3 μm and 6 μm.
When the wet milling is carried out to prepare powder, solvent oil is added, and the amount of the added solvent oil is 30% of the total amount of tungsten carbide, hydrofluoric acid, Co, titanium carbide and nickel.
During sintering, a three-section heating mode is adopted under the argon atmosphere condition;
in the first stage, under the pressure condition of 15MPa, the temperature is raised from room temperature to 500 ℃ at the temperature raising speed of 5 ℃/min, and the temperature is kept for 60min at constant temperature.
In the second stage, the temperature is raised from 500 ℃ to 1100 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 60min at constant temperature.
And in the third stage, the temperature is increased from 1100 ℃ to 1550 ℃ at the temperature increase speed of 5 ℃/min, and the temperature is kept for 45min at constant temperature.
The sintering is a plasma sintering method. The forming agent is fully refined paraffin with the melting point of 58 ℃.
Although the present invention has been described in detail with reference to the embodiments, it will be apparent to those skilled in the art that modifications, equivalents, improvements, and the like can be made in the technical solutions of the foregoing embodiments or in some of the technical features of the foregoing embodiments, but those modifications, equivalents, improvements, and the like are all within the spirit and principle of the present invention.

Claims (7)

1. A method of increasing the toughness of cemented carbide comprising the steps of:
wet milling to prepare powder, taking 70-85 parts of tungsten carbide, 10-25 parts of hydrofluoric acid, 5-11 parts of Co, 3-15 parts of titanium carbide and 6-8 parts of nickel according to parts by weight, mixing, adding into a wet mill, and ball-milling for 55-70 hours; then, sieving the mixed slurry with a 350-mesh sieve, discharging and precipitating, and separating a supernatant medium;
drying, adding low-melting-point paraffin into the mixed slurry, stirring to dry the mixed slurry, then sieving with a 400-mesh sieve, and filtering to remove impurities;
forming, namely adding the dried material into a mixer, adding a forming agent, uniformly stirring, and then performing compression forming to obtain blank hard alloy;
and sintering the blank hard alloy, and cooling after sintering to obtain the finished hard alloy.
2. The method of increasing the toughness of cemented carbide according to claim 1, wherein the tungsten carbide comprises particles of two particle size sizes with an average particle size of 3 μ ι η and 6 μ ι η.
3. The method for improving the toughness of the hard alloy according to claim 2, wherein when the wet grinding is carried out, the solvent oil is added, and the amount of the solvent oil added is 20-30% of the total amount of the tungsten carbide, the hydrofluoric acid, the Co, the titanium carbide and the nickel.
4. The method for improving the toughness of the hard alloy according to claim 3, wherein during sintering, a three-stage heating mode is adopted, and the temperature is increased under the condition of argon atmosphere;
in the first stage, under the pressure condition of 10-15 MPa, the temperature is raised from room temperature to 500 ℃ at the temperature raising speed of 3-5 ℃/min, and the temperature is kept constant for 30-60 min;
in the second stage, the temperature is increased from 500 ℃ to 1000-1100 ℃ at the temperature increase speed of 8-10 ℃/min, and the temperature is kept for 30-60 min at constant temperature;
and in the third stage, the temperature is increased from 1000-1100 ℃ to 1500-1550 ℃ at the temperature increase speed of 3-5 ℃/min, and the temperature is kept for 30-45 min at constant temperature.
5. The method for improving the toughness of a hard alloy according to claim 4, wherein the sintering is a vacuum sintering method, a low pressure sintering method or a plasma sintering method.
6. The method for improving the toughness of the hard alloy according to claim 5, wherein the forming agent is fully refined paraffin with a melting point of 58 ℃.
7. The method of increasing the toughness of a cemented carbide according to claim 6, wherein the titanium carbide has a Fisher average grain size of 1.5 um.
CN202010701404.9A 2020-07-21 2020-07-21 Method for improving toughness of hard alloy Pending CN111705251A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5831059A (en) * 1981-08-18 1983-02-23 Tatsuro Kuratomi Hard carbide-base tool material and its manufacture
JPH03281752A (en) * 1990-03-29 1991-12-12 Kobe Steel Ltd High toughness cermet
WO2004065645A1 (en) * 2003-01-13 2004-08-05 Genius Metal, Inc. Compositions and fabrication methods for hardmetals
CN106048360A (en) * 2016-07-11 2016-10-26 中南大学 Hard alloy with double-layer gradient structure on surface and making method for hard alloy
CN109763053A (en) * 2019-03-05 2019-05-17 常熟中材钨业科技有限公司 A kind of mold high temperature toughness cemented carbide material and preparation method thereof
CN109809818A (en) * 2017-11-20 2019-05-28 赵超峰 A kind of high-quality high-intensitive toughness cemented carbide material
CN111386355A (en) * 2018-11-01 2020-07-07 住友电气工业株式会社 Cemented carbide, cutting tool, and method for producing cemented carbide
CN111566241A (en) * 2018-01-09 2020-08-21 住友电工硬质合金株式会社 Cemented carbide and cutting tool

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5831059A (en) * 1981-08-18 1983-02-23 Tatsuro Kuratomi Hard carbide-base tool material and its manufacture
JPH03281752A (en) * 1990-03-29 1991-12-12 Kobe Steel Ltd High toughness cermet
WO2004065645A1 (en) * 2003-01-13 2004-08-05 Genius Metal, Inc. Compositions and fabrication methods for hardmetals
CN106048360A (en) * 2016-07-11 2016-10-26 中南大学 Hard alloy with double-layer gradient structure on surface and making method for hard alloy
CN109809818A (en) * 2017-11-20 2019-05-28 赵超峰 A kind of high-quality high-intensitive toughness cemented carbide material
CN111566241A (en) * 2018-01-09 2020-08-21 住友电工硬质合金株式会社 Cemented carbide and cutting tool
CN111386355A (en) * 2018-11-01 2020-07-07 住友电气工业株式会社 Cemented carbide, cutting tool, and method for producing cemented carbide
CN109763053A (en) * 2019-03-05 2019-05-17 常熟中材钨业科技有限公司 A kind of mold high temperature toughness cemented carbide material and preparation method thereof

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Application publication date: 20200925

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