CN105369104B - Al2O3‑ZrO2/ Co Ni BN cermet mold materials and preparation method thereof - Google Patents

Al2O3‑ZrO2/ Co Ni BN cermet mold materials and preparation method thereof Download PDF

Info

Publication number
CN105369104B
CN105369104B CN201510864792.1A CN201510864792A CN105369104B CN 105369104 B CN105369104 B CN 105369104B CN 201510864792 A CN201510864792 A CN 201510864792A CN 105369104 B CN105369104 B CN 105369104B
Authority
CN
China
Prior art keywords
zro
content
preparation
mold materials
mass percentage
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201510864792.1A
Other languages
Chinese (zh)
Other versions
CN105369104A (en
Inventor
马伟民
***
马澜
张艳丽
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenyang University of Chemical Technology
Original Assignee
Shenyang University of Chemical Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenyang University of Chemical Technology filed Critical Shenyang University of Chemical Technology
Priority to CN201510864792.1A priority Critical patent/CN105369104B/en
Publication of CN105369104A publication Critical patent/CN105369104A/en
Application granted granted Critical
Publication of CN105369104B publication Critical patent/CN105369104B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

Al2O3‑ZrO2/ Co Ni BN cermet mold materials and preparation method thereof, are related to a kind of non-ferrous alloy mold materials and preparation method thereof, and material component includes matrix material and toughness reinforcing phase, matrix material Al2O3, its grain diameter is 60nm, and mass percentage content is 72.25% 82.45%, transformation toughening phase ZrO2For mass fraction 12.8% 14.6%, its particle diameter is 200nm；Stratiform toughness reinforcing phase BN is 1% 5%, and its particle diameter is 100nm；Ductility toughness reinforcing phase Co Ni are mass fraction 2% 10%, and its particle diameter is 100nm.Step of preparation process：The first step is the mixing and drying of raw material, and Part II is powder compacting and sintering.The bending strength of prepared cermet mold material is 1014 1423MPa, and fracture toughness is 7 ~ 14.7MPa.m1/2, hardness reaches 8.7 13.4GPa.The material is widely used as the hot worked wear-resisting extrusion die of non-ferrous metal.

Description

Al2O3-ZrO2/ Co-Ni-BN cermet mold materials and preparation method thereof
Technical field
The present invention relates to a kind of non-ferrous alloy mold materials and preparation method thereof, more particularly to a kind of Al2O3-ZrO2 / Co-Ni-BN cermet mold materials and preparation method thereof.
Background technology
With the fast development of materials industry, mould turns into irreplaceable equipment in development of modern industry, to industry The basis of extensive development has been established in development.Due to mould in the work environment, often aoxidize, mucous membrane, corrosion even goes out Phenomena such as existing soldering, and traditional material can not meet industrial actual production need such as high hard firm, hard alloy, traditional ceramics Ask.The currently used ceramic die material of industrial circle is mostly TZP/Al2O3、PSZ、Si3N4、Sialon、3Y-TZP/Al2O3、 Al2O3/ Ni etc..Because the poor performance opposite sex is larger, the mold materials of different ceramic systems are limited to by use environment.
There is high temperature resistant, the excellent properties such as wear-resistant, anti-oxidant, anti-thermal shock, its metal as multiphase composite cermet Ceramic die has turned into the hot extrusion manufacture fields such as copper alloy, aluminium alloy and titanium alloy and has substituted hard alloy, mould steel, ceramic die The optimal material of tool.
The content of the invention
It is an object of the invention to provide a kind of Al2O3-ZrO2/ Co-Ni-BN cermet mold materials and its preparation side Method, the present invention prepare high performance cermet mold material, can preferably be used for easy to wear, perishable, high temperature, height The mal-conditions such as pressure, to reducing processing cost in production, improving production efficiency etc. has marked improvement.
The purpose of the present invention is achieved through the following technical solutions：
Al2O3-ZrO2/ Co-Ni-BN cermet mold materials, the dispensing of the material include raw material A l2O3Powder, ZrO2BN, Co, Ni powder of powder, equal proportion quality, Al2O3The content of nano particle is 72.25- by mass percentage 82.45%, ZrO2The content of micron particles is 12.75-14.55%, BN, Co, Ni in mass ratio 1 by mass percentage：1：1 weighing Content presses gross mass percentage 3-15%；Material bending strength is 1014 ~ 1423Mpa, fracture toughness 7-14.7MPa.m1/2, firmly Degree reaches 8.7-13.4Gpa.
Al2O3-ZrO2/ Co-Ni-BN cermet mold material preparation methods, methods described use following processing step One-stop operation：
1. dispensing：By raw material A l2O3Powder, ZrO2Powder, BN, Co, Ni powder of equal proportion quality are raw material, Al2O3Receive The content of rice grain is 72.25-82.45%, ZrO by mass percentage2The content of micron particles is 12.75- by mass percentage 14.55%, BN, Co, Ni in mass ratio 1：1：1 weighing content presses gross mass percentage 3-15%；
2. ball mill mixing, the material prepared is added in ball mill, ball milling 24 hours, is put into drying box, 60 DEG C of dryings 24 hours, prepare Al2O3-ZrO2/ Co-Ni-BN composite granules；
3. powder compacting and sintering：Composite granule 2. step is handled after is added to vacuum sintering funace graphite mo(u)ld In tool, under vacuum, sintering temperature is 1450 DEG C ~ 1650 DEG C, pressure 30Mpa, and vacuum is 6 × 10- 2,Hot pressing 30 divides Clock.
Described Al2O3-ZrO2/ Co-Ni-BN cermet mold material preparation methods, 2. middle ball milling is situated between the step Matter selects absolute ethyl alcohol, and abrading-ball is high purity aluminium oxide ball, and mixed composite granule is dried in drying box.
Described Al2O3-ZrO2/ Co-Ni-BN cermet mold material preparation methods, methods described step 3. in adopt Be sintered with the method for vacuum heating-press sintering, sintering temperature be 1450 DEG C ~ 1650 DEG C, pressure 30Mpa, vacuum be 6 × 10-2, hot pressing 30 minutes.
Advantages of the present invention is with effect：
The Al of the present invention2O3-ZrO2/ Co-Ni-BN cermet mold material performance parameters are：Bending strength 1014- 1423MPa, fracture toughness 7-14.7MPa.m1/2, hardness reaches 8.7-13.4Pa.When Co-Ni-BN contents are 4%, sample Bending strength, fracture toughness and hardness reach maximum.The inventive method prepares high performance cermet mold material, The mal-condition such as easy to wear, perishable, high temperature, high pressure can be preferably used for, to reducing processing cost in production, improving life Production efficiency etc. has marked improvement.
Brief description of the drawings
Fig. 1 is metal ceramic surface first node back scattering idea picture；
Fig. 2 is Fig. 1 energy spectrum analysis collection of illustrative plates；
Fig. 3 is metal ceramic surface section point back scattering idea picture；
Fig. 4 is Fig. 3 energy spectrum analysis collection of illustrative plates；
Fig. 5 is to be incubated the sample after 30min when BN-Co-Ni alloy contents are 3% under 1500 DEG C, 30PMPa pressure conditions Fracture apperance；
Fig. 6 is to be incubated the sample after 30min when BN-Co-Ni alloy contents are 6% under 1500 DEG C, 30PMPa pressure conditions Fracture apperance；
Fig. 7 is to be incubated the sample after 30min when BN-Co-Ni alloy contents are 9% under 1500 DEG C, 30PMPa pressure conditions Fracture apperance；
Fig. 8 is to be incubated the sample after 30min when BN-Co-Ni alloy contents are 12% under 1500 DEG C, 30PMPa pressure conditions Product fracture apperance；
Fig. 9 is to be incubated the sample after 30min when BN-Co-Ni alloy contents are 15% under 1500 DEG C, 30PMPa pressure conditions Product fracture apperance；
Figure 10 is the bending strength curve of sample；
Figure 11 is the fracture toughness curve of sample；
Figure 12 is the hardness curve of sample.
Embodiment
With reference to embodiment, the present invention is described in detail.
Material component of the present invention includes matrix material and toughness reinforcing phase, matrix material Al2O3, its grain diameter is 60nm matter Amount degree is 72%-82%, transformation toughening phase ZrO2For mass fraction 12.8-14.6%, its particle diameter is 200nm；Stratiform increases Tough phase BN is 1%-5%, and its particle diameter is 100nm;Ductility toughness reinforcing phase Co-Ni is that mass fraction 2%-10% its particle diameter is 100nm.Prepare Processing step：The first step is the mixing and drying of raw material, and Part II is powder compacting and sintering.Prepared cermet mold The bending strength for having material is 1014-1423, MPa, fracture toughness 7-14.7MPa.m1/2, hardness reaches 8.7-13.4GPa.
The Al of the present invention2O3-ZrO2/ Co-Ni-BN cermet mold materials preparation technology uses following steps：
1）Dispensing：With Al2O3Powder, ZrO2Powder, BN powder, metal Co, Ni powder are raw material, Al2O3Nano particle Content is 72-82%, ZrO by mass percentage2For mass fraction 12.8-14.6%, BN, Co, Ni in mass ratio 1：1：1 weighing contains Measure 3-15% by mass percentage；
2）Ball mill mixing：The material prepared is added in planetary ball mill, ball milling 24 hours, is put into vacuum drying chamber, 60 DEG C of dryings 24 hours, ball milling prepares Al2O3-ZrO2/ Co-Ni-BN composite granules；
3）Powder compacting and sintering：Composite granule after step 2 is handled is added in vacuum sintering funace, in vacuum Under the conditions of, temperature is 1450 DEG C ~ 1650 DEG C, and pressure is 30MPa vacuum hotpressing 30min, prepares Al2O3-ZrO2/Co-Ni-BN Cermet mold material.
The raw material that the present invention uses：Al2O3Powder：Particle diameter is 60nm, purity Al2O3Content>99.9%；ZrO2Powder：Particle diameter For 0.2 μm of content>99.7%；BN particle diameters are 0.1 μm, content>99.7%；Co powder and Ni powder：Particle diameter is 0.1 μm of content>99.9%.
Embodiment 1
With Al2O3Nano particle, ZrO2It is raw material with BN, Co, Ni micron particles, Al2O3The content of nano particle presses quality Percentage is 82.45%, ZrO2The content of particle is 14.55% by mass percentage, BN, Co, Ni micron of equal quality ratio Grain content is respectively 1% by mass percentage；Then the composite granule prepared is added in planetary ball mill, ball-milling medium is nothing Water-ethanol, high purity aluminium oxide ball are abrading-ball, ball milling 24h, 24h are then dried in drying box, prepares Al2O3-ZrO2/Co- Ni-BN composite granules, composite granule is subjected to hot pressed sintering in vacuum sintering funace, vacuum heating-press sintering temperature is 1550 DEG C, hot pressing pressure 30MPa, hot pressing time 30min, vacuum be 6 × 10-2MPa, prepare Al2O3-ZrO2/ Co-Ni-BN gold Belong to ceramic die material.Using unilateral three-point bending strength testing inspection material bending strength；Using SENB methods detection material Fracture toughness；Using the Vickers hardness of Vickers identation hardnesses method measure material（Hv）；Using ESEM（SEM）It has detected The microscopic structure and fracture apperance of material.
Prepared Al2O3-ZrO2The performance test results of/Co-Ni-BN cermet mold materials are：Bending strength is 1014MPa, fracture toughness 7MPa.m1/2, hardness reaches 8.7Gpa（Fracture apperance is as shown in Figure 5）.
Embodiment 2
With Al2O3Nano particle, ZrO2It is raw material with BN, Co, Ni micron particles, Al2O3The content of nano particle presses quality Percentage is 79.9%, ZrO2The content of particle is 14.1% by mass percentage, BN, Co, Ni micron particles of equal quality ratio Content is respectively 2% by mass percentage；Then the composite granule prepared is added in planetary ball mill, ball-milling medium is anhydrous Ethanol, high purity aluminium oxide ball are abrading-ball, ball milling 24h, 24h are then dried in drying box, prepares Al2O3-ZrO2/Co-Ni- BN composite granules, composite granule is subjected to hot pressed sintering in vacuum sintering funace, vacuum heating-press sintering temperature is 1550 DEG C, Hot pressing pressure is 30MPa, and hot pressing time 30min, vacuum is 6 × 10-2MPa, prepare Al2O3-ZrO2/ Co-Ni-BN metals Ceramic die material.Using unilateral three-point bending strength testing inspection material bending strength；Using the disconnected of SENB methods detection material Split toughness；Using the Vickers hardness of Vickers identation hardnesses method measure material（Hv）；Using ESEM（SEM）It has detected material The microscopic structure and fracture apperance of material.
Prepared Al2O3-ZrO2The performance test results of/Co-Ni-BN cermet mold materials are：Bending strength is 1106MPa, fracture toughness 8.2MPa.m1/2, hardness reaches 10.4Gpa（Fracture apperance is as shown in Figure 5）.
Embodiment 3
With Al2O3Nano particle, ZrO2It is raw material with BN, Co, Ni micron particles, Al2O3The content of nano particle presses quality Percentage is 77.35%, ZrO2The content of particle is 13.66% by mass percentage, BN, Co, Ni micron of equal quality ratio Grain content is respectively 3% by mass percentage；Then the composite granule prepared is added in planetary ball mill, ball-milling medium is nothing Water-ethanol, high purity aluminium oxide ball are abrading-ball, ball milling 24h, 24h are then dried in drying box, prepares Al2O3-ZrO2/Co- Ni-BN composite granules, composite granule is subjected to hot pressed sintering in vacuum sintering funace, vacuum heating-press sintering temperature is 1550 DEG C, hot pressing pressure 30MPa, hot pressing time 30min, vacuum be 6 × 10-2MPa, prepare Al2O3-ZrO2/ Co-Ni-BN gold Belong to ceramic die material.Using unilateral three-point bending strength testing inspection material bending strength；Using SENB methods detection material Fracture toughness；Using the Vickers hardness of Vickers identation hardnesses method measure material（Hv）；Using ESEM（SEM）It has detected The microscopic structure and fracture apperance of material.
Prepared Al2O3-ZrO2The performance test results of/Co-Ni-BN cermet mold materials are：Bending strength is 1372MPa, fracture toughness 12.6MPa.m1/2, hardness reaches 11.32Gpa（Fracture apperance is as shown in Figure 5）.
Embodiment 4
With Al2O3Nano particle, ZrO2It is raw material with BN, Co, Ni micron particles, Al2O3The content of nano particle presses quality Percentage is 74.8%, ZrO2The content of particle is 13.2% by mass percentage, BN, Co, Ni micron particles of equal quality ratio Content is respectively 4% by mass percentage；Then the composite granule prepared is added in planetary ball mill, ball-milling medium is anhydrous Ethanol, high purity aluminium oxide ball are abrading-ball, ball milling 24h, 24h are then dried in drying box, prepares Al2O3-ZrO2/Co-Ni- BN composite granules, composite granule is subjected to hot pressed sintering in vacuum sintering funace, vacuum heating-press sintering temperature is 1550 DEG C, Hot pressing pressure is 30MPa, and hot pressing time 30min, vacuum is 6 × 10-2MPa, prepare Al2O3-ZrO2/ Co-Ni-BN metals Ceramic die material.Using unilateral three-point bending strength testing inspection material bending strength；Using the disconnected of SENB methods detection material Split toughness；Using the Vickers hardness of Vickers identation hardnesses method measure material（Hv）；Using ESEM（SEM）It has detected material The microscopic structure and fracture apperance of material.
Prepared Al2O3-ZrO2The performance test results of/Co-Ni-BN cermet mold materials are：Bending strength is 1423MPa, fracture toughness 14.7MPa.m1/2, hardness reaches 13.4Gpa（Fracture apperance is as shown in Figure 5）.
Embodiment 5
With Al2O3Nano particle, ZrO2It is raw material with BN, Co, Ni micron particles, Al2O3The content of nano particle presses quality Percentage is 72.25%, ZrO2The content of particle is 12.75% by mass percentage, BN, Co, Ni micron of equal quality ratio Grain content is respectively 5% by mass percentage；Then the composite granule prepared is added in planetary ball mill, ball-milling medium is nothing Water-ethanol, high purity aluminium oxide ball are abrading-ball, ball milling 24h, 24h are then dried in drying box, prepares Al2O3-ZrO2/Co- Ni-BN composite granules, composite granule is subjected to hot pressed sintering in vacuum sintering funace, vacuum heating-press sintering temperature is 1550 DEG C, hot pressing pressure 30MPa, hot pressing time 30min, vacuum be 6 × 10-2MPa, prepare Al2O3-ZrO2/ Co-Ni-BN gold Belong to ceramic die material.Using unilateral three-point bending strength testing inspection material bending strength；Using SENB methods detection material Fracture toughness；Using the Vickers hardness of Vickers identation hardnesses method measure material（Hv）；Using ESEM（SEM）It has detected The microscopic structure and fracture apperance of material.
Prepared Al2O3-ZrO2The performance test results of/Co-Ni-BN cermet mold materials are：Bending strength is 1408Mpa, fracture toughness 13.4MPa.m1/2, hardness reaches 12.52Gpa（Fracture apperance is as shown in Figure 5）.

Claims (1)

1.Al2O3-ZrO2/ Co-Ni-BN cermet mold materials, it is characterised in that the dispensing of the material includes raw material Al2O3Powder, ZrO2BN, Co, Ni powder of powder, equal proportion quality, Al2O3The content of nano particle is by mass percentage 72.25-82.45%, ZrO2The content of micron particles is 12.75-14.55%, BN, Co, Ni in mass ratio 1 by mass percentage： 1：1 weighing content presses gross mass percentage 3-15%, and material bending strength is 1014 ~ 1423MPa, fracture toughness 7- 14.7MPa.m1/2, hardness reaches 8.7-13.4GPa.
CN201510864792.1A 2015-12-01 2015-12-01 Al2O3‑ZrO2/ Co Ni BN cermet mold materials and preparation method thereof Expired - Fee Related CN105369104B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510864792.1A CN105369104B (en) 2015-12-01 2015-12-01 Al2O3‑ZrO2/ Co Ni BN cermet mold materials and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510864792.1A CN105369104B (en) 2015-12-01 2015-12-01 Al2O3‑ZrO2/ Co Ni BN cermet mold materials and preparation method thereof

Publications (2)

Publication Number Publication Date
CN105369104A CN105369104A (en) 2016-03-02
CN105369104B true CN105369104B (en) 2018-01-30

Family

ID=55371727

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510864792.1A Expired - Fee Related CN105369104B (en) 2015-12-01 2015-12-01 Al2O3‑ZrO2/ Co Ni BN cermet mold materials and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105369104B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108101520B (en) * 2017-12-23 2021-01-29 邹平宏发铝业科技有限公司 Aluminum oxide-silicon carbide composite material and preparation method thereof
CN113186441B (en) * 2021-04-27 2022-02-22 湖北中烟工业有限责任公司 Nickel-zirconia cermets and uses thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101486564B (en) * 2009-02-16 2011-08-10 山东大学 Preparation of boron nitride nano tube enhanced alumina ceramic
CN104480364A (en) * 2014-11-10 2015-04-01 沈阳理工大学 Al2O3-TiCN/Co-Ni metal ceramic die material and preparation method thereof

Also Published As

Publication number Publication date
CN105369104A (en) 2016-03-02

Similar Documents

Publication Publication Date Title
CN110483085B (en) Whisker reinforced alumina composite ceramic and preparation method and application thereof
CN103833363B (en) Silicon carbide graphite composite material and preparation method thereof
GB2506287B (en) Tungsten Carbide Composite Containing Alumina Grains and Silicon Nitride Whiskers and the Preparation Method Thereof
CN110468320B (en) High-hardness and high-toughness metal ceramic and preparation method and application thereof
CN105272260B (en) A kind of soap-free emulsion polymeization phase tungsten carbide composite and preparation method thereof
CN102701773B (en) Authigenic silicon nitride crystal whisker toughening tungsten carbide composite material and preparation method thereof
CN103866165A (en) Isotropical high-strength high-toughness particle reinforced aluminium-based composite material and preparation method thereof
CN101913876B (en) Method for preparing zirconium boride-tungsten titanium carbide self-lubricating composite ceramic material
CN106216687B (en) A kind of gradient tungsten carbide-base micro-nano complex cutter material and preparation method thereof
CN106735249B (en) A kind of niobium based composites and preparation method
CN104451324B (en) Preparation process of WCoB-based metal ceramic
JPWO2014208447A1 (en) Cermet, manufacturing method thereof and cutting tool
CN109439991A (en) A kind of TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method
CN105369104B (en) Al2O3‑ZrO2/ Co Ni BN cermet mold materials and preparation method thereof
CN104480364A (en) Al2O3-TiCN/Co-Ni metal ceramic die material and preparation method thereof
CN109320249B (en) Tungsten carbide composite material containing boron oxide and preparation method thereof
CN109518057A (en) A kind of tungsten carbide material and its preparation method and application by high-entropy alloy cobalt ferronickel aluminum bronze bonding
CN100391898C (en) Plasma discharging and sintering process of synthesizing aluminum-titanium nitride-titanium nitride composite block material
CN104232961A (en) High-strength high-hardness Cu-Cr composite material as well as preparation method and application thereof
CN111778436A (en) Method for preparing WC-Y2O3 binderless hard alloy by cold pressing-hot pressing sintering
CN109824365A (en) A kind of preparation method of fabricated in situ titanium silicon-carbon/alumina composite material
CN106591747B (en) A kind of β-Si3N4Whisker and Ni3The WC composite material and preparation methods of Al Binder Phase coordination plasticizings
CN112080678B (en) Ternary boride alloy screw material and production process thereof
CN108085526A (en) A kind of low-density niobium based composites and preparation method
CN102321837A (en) High-hardness composite material for cutter and preparation method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20180130

Termination date: 20201201

CF01 Termination of patent right due to non-payment of annual fee