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 PDFInfo
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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
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.
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| 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 |
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