CN105369104A - Al2O3-ZrO2/Co-Ni-BN metal ceramic die material and preparation method thereof - Google Patents

Al2O3-ZrO2/Co-Ni-BN metal ceramic die material and preparation method thereof Download PDF

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CN105369104A
CN105369104A CN201510864792.1A CN201510864792A CN105369104A CN 105369104 A CN105369104 A CN 105369104A CN 201510864792 A CN201510864792 A CN 201510864792A CN 105369104 A CN105369104 A CN 105369104A
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powder
ball
sintering
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CN105369104B (en
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马伟民
聂力
马澜
张艳丽
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Shenyang University of Chemical Technology
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Shenyang University of Chemical Technology
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Abstract

An Al2O3-ZrO2/Co-Ni-BN metal ceramic die material and a preparation method thereof relate to a non-ferrous alloy die material and a preparation method thereof. The components of the material include a base material and toughening phases, wherein the base material is Al2O3, is 60 nm in particle diameter and is 72.25%-82.45% in mass percent content; a phase transformation toughening phase ZrO2 is 12.8%-14.6% in mass fraction and 200 nm in particle diameter; a lamellar toughening phase BN is 1%-5% in mass fraction and 100 nm in particle diameter; and a ductile toughening phase Co-Ni is 2%-10% in mass fraction and 100 nm in particle diameter. The preparation process steps are as follows: 1, mixing and drying of raw materials; and 2, powder forming and sintering. The prepared metal ceramic die material prepared has the bending strength of 1,014-1,423 MPa, the fracture toughness of 7-14.7 MPa.m<l/2> and the hardness of 8.7-13.4 GPa. The material is widely applied to abrasion-resistant extrusion dies for non-ferrous metal processing.

Description

Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material and preparation method thereof
Technical field
The present invention relates to a kind of non-ferrous alloy moulding stock and preparation method thereof, particularly relate to a kind of Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material and preparation method thereof.
Background technology
Along with the fast development of materials industry, mould becomes irreplaceable equipment in development of modern industry, has established the basis of extensive development to industrial development.Due to mould in the work environment, being often oxidized, mucous membrane, even there is the phenomenons such as seam in corrosion, and traditional material is as hard in height just, Wimet, traditional ceramics can not meet industrial actual production demand.The ceramic die material that industrial circle is commonly used at present is mostly TZP/Al 2o 3, PSZ, Si 3n 4, Sialon, 3Y-TZP/Al 2o 3, Al 2o 3/ Ni etc.Because the poor performance opposite sex is comparatively large, the moulding stock of different ceramic systems is subject to the limitation of environment for use.
Have high temperature resistant as heterogeneous composite cermet, the excellent properties such as wear-resistant, anti-oxidant, anti-thermal shock, its cermet mold has become the best materials that the hot extrusion manufacture fields such as copper alloy, aluminium alloy and titanium alloy substitute Wimet, die steel, ceramic die.
Summary of the invention
The object of the present invention is to provide a kind of Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material and preparation method thereof, the present invention prepares high performance cermet mold material, can better for the mal-condition such as easy to wear, perishable, high temperature, high pressure, cutting down finished cost in production, there is marked improvement the aspect such as to enhance productivity.
The object of the invention is to be achieved through the following technical solutions:
Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material, the batching of described material comprises raw material A l 2o 3powder, ZrO 2bN, Co, Ni powder of powder, equal proportion quality, Al 2o 3the content of nano particle is 72.25-82.45%, ZrO by mass percentage 2the content of micron particle be by mass percentage 12.75-14.55%, BN, Co, Ni in mass ratio 1:1:1 weighing content by total mass per-cent 3-15%; Material bending strength is 1014 ~ 1423Mpa, and fracture toughness property is 7-14.7MPa.m 1/2, hardness reaches 8.7-13.4Gpa.
Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material preparation method, described method adopts following processing step one-stop operation:
1. prepare burden: by raw material A l 2o 3powder, ZrO 2bN, Co, Ni powder of powder, equal proportion quality is raw material, Al 2o 3the content of nano particle is 72.25-82.45%, ZrO by mass percentage 2the content of micron particle be by mass percentage 12.75-14.55%, BN, Co, Ni in mass ratio 1:1:1 weighing content by total mass per-cent 3-15%;
2. ball mill mixing, adds in ball mill by the material prepared, and ball milling 24 hours, puts into loft drier, and 60 DEG C of dryings 24 hours, prepare Al 2o 3-ZrO 2/ Co-Ni-BN composite granule;
3. powder compacting and sintering: the composite granule after step 2. being processed joins in vacuum sintering funace graphite jig, under vacuum, sintering temperature is 1450 DEG C ~ 1650 DEG C, and pressure is 30Mpa, and vacuum tightness is 6 × 10 -2,hot pressing 30 minutes.
Described Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material preparation method, described step 2. middle ball-milling medium selects dehydrated alcohol, and abrading-ball is high purity aluminium oxide ball, and mixed composite granule is dry in loft drier.
Described Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material preparation method, the described method steps 3. middle method of vacuum heating-press sintering that adopts sinters, and sintering temperature is 1450 DEG C ~ 1650 DEG C, and pressure is 30Mpa, and vacuum tightness is 6 × 10 -2, hot pressing 30 minutes.
Advantage of the present invention and effect are:
Al of the present invention 2o 3-ZrO 2/ Co-Ni-BN cermet mold material performance perameter is: bending strength 1014-1423MPa, and fracture toughness property is 7-14.7MPa.m 1/2, hardness reaches 8.7-13.4Pa.When Co-Ni-BN content is 4%, the bending strength of sample, fracture toughness property and hardness reach maximum value.The inventive method prepares high performance cermet mold material, can better for the mal-condition such as easy to wear, perishable, high temperature, high pressure, cutting down finished cost in production, and there is marked improvement the aspect such as to enhance productivity.
Accompanying drawing explanation
Fig. 1 is metal ceramic surface first node back scattering idea picture;
Fig. 2 is the energy spectrum analysis collection of illustrative plates of Fig. 1;
Fig. 3 is metal ceramic surface Section Point back scattering idea picture;
Fig. 4 is the energy spectrum analysis collection of illustrative plates of Fig. 3;
Fig. 5 is BN-Co-Ni alloy content when being 3% at 1500 DEG C, is incubated the sample fracture apperance after 30min under 30PMPa pressure condition;
Fig. 6 is BN-Co-Ni alloy content when being 6% at 1500 DEG C, is incubated the sample fracture apperance after 30min under 30PMPa pressure condition;
Fig. 7 is BN-Co-Ni alloy content when being 9% at 1500 DEG C, is incubated the sample fracture apperance after 30min under 30PMPa pressure condition;
Fig. 8 is BN-Co-Ni alloy content when being 12% at 1500 DEG C, is incubated the sample fracture apperance after 30min under 30PMPa pressure condition;
Fig. 9 is BN-Co-Ni alloy content when being 15% at 1500 DEG C, is incubated the sample fracture apperance after 30min under 30PMPa pressure condition;
Figure 10 is the bending strength curve of sample;
Figure 11 is the fracture toughness property curve of sample;
Figure 12 is the hardness curve of sample.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Material component of the present invention comprises body material and toughness reinforcing phase, and body material is Al 2o 3, its grain diameter is 60nm mass percentage content is 72%-82%, transformation toughening phase ZrO 2for massfraction 12.8-14.6%, its particle diameter is 200nm; The toughness reinforcing phase BN of stratiform is 1%-5%, and its particle diameter is 100nm; The toughness reinforcing phase Co-Ni of ductility is its particle diameter of massfraction 2%-10% is 100nm.Step of preparation process: the first step is mixing and the drying of raw material, and second section is powder compacting and sintering.The bending strength of prepared cermet mold material is 1014-1423, MPa, and fracture toughness property is 7-14.7MPa.m 1/2, hardness reaches 8.7-13.4GPa.
Al of the present invention 2o 3-ZrO 2/ Co-Ni-BN cermet mold material preparation technology adopts following steps:
1) prepare burden: with Al 2o 3powder, ZrO 2powder, BN powder, metal Co, Ni powder are raw material, Al 2o 3the content of nano particle is 72-82%, ZrO by mass percentage 2for massfraction 12.8-14.6%, BN, Co, Ni be 1:1:1 weighing content 3-15% by mass percentage in mass ratio;
2) ball mill mixing: add in planetary ball mill by the material prepared, ball milling 24 hours, puts into vacuum drying oven, and 60 DEG C of dryings 24 hours, ball milling prepares Al 2o 3-ZrO 2/ Co-Ni-BN composite granule;
3) powder compacting and sintering: the composite granule after step 2 being processed joins in vacuum sintering funace, under vacuum, temperature is 1450 DEG C ~ 1650 DEG C, and pressure is 30MPa vacuum hotpressing 30min, prepares Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material.
The raw material that the present invention adopts: Al 2o 3powder: particle diameter is 60nm, purity Al 2o 3content >99.9%; ZrO 2powder: particle diameter is 0.2 μm of content >99.7%; BN particle diameter is 0.1 μm, content >99.7%; Co powder and Ni powder: particle diameter is 0.1 μm of content >99.9%.
Embodiment 1
With Al 2o 3nano particle, ZrO 2be raw material with BN, Co, Ni micron particle, Al 2o 3the content of nano particle is 82.45%, ZrO by mass percentage 2the content of particle is 14.55% by mass percentage, waits BN, Co, Ni micron particle content of mass ratio to be respectively 1% by mass percentage; Then add in planetary ball mill by the composite granule prepared, ball-milling medium is dehydrated alcohol, and high purity aluminium oxide ball is abrading-ball, ball milling 24h, then at loft drier inner drying 24h, prepares Al 2o 3-ZrO 2/ Co-Ni-BN composite granule, carries out hot pressed sintering by composite granule in vacuum sintering funace, and vacuum heating-press sintering temperature is 1550 DEG C, hot pressing pressure is 30MPa, hot pressing time 30min, and vacuum tightness is 6 × 10 -2mPa, prepares Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material.Adopt monolateral three-point bending strength testing inspection material bending strength; Adopt the fracture toughness property of SENB method test material; Vickers penetration hardness method is adopted to measure the Vickers' hardness (Hv) of material; Scanning electron microscope (SEM) is adopted to have detected microstructure and the fracture apperance of material.
Prepared Al 2o 3-ZrO 2the performance test results of/Co-Ni-BN cermet mold material is: bending strength is 1014MPa, and fracture toughness property is 7MPa.m 1/2, hardness reaches 8.7Gpa(fracture apperance as shown in Figure 5).
Embodiment 2
With Al 2o 3nano particle, ZrO 2be raw material with BN, Co, Ni micron particle, Al 2o 3the content of nano particle is 79.9%, ZrO by mass percentage 2the content of particle is 14.1% by mass percentage, waits BN, Co, Ni micron particle content of mass ratio to be respectively 2% by mass percentage; Then add in planetary ball mill by the composite granule prepared, ball-milling medium is dehydrated alcohol, and high purity aluminium oxide ball is abrading-ball, ball milling 24h, then at loft drier inner drying 24h, prepares Al 2o 3-ZrO 2/ Co-Ni-BN composite granule, carries out hot pressed sintering by composite granule in vacuum sintering funace, and vacuum heating-press sintering temperature is 1550 DEG C, hot pressing pressure is 30MPa, hot pressing time 30min, and vacuum tightness is 6 × 10 -2mPa, prepares Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material.Adopt monolateral three-point bending strength testing inspection material bending strength; Adopt the fracture toughness property of SENB method test material; Vickers penetration hardness method is adopted to measure the Vickers' hardness (Hv) of material; Scanning electron microscope (SEM) is adopted to have detected microstructure and the fracture apperance of material.
Prepared Al 2o 3-ZrO 2the performance test results of/Co-Ni-BN cermet mold material is: bending strength is 1106MPa, and fracture toughness property is 8.2MPa.m 1/2, hardness reaches 10.4Gpa(fracture apperance as shown in Figure 5).
Embodiment 3
With Al 2o 3nano particle, ZrO 2be raw material with BN, Co, Ni micron particle, Al 2o 3the content of nano particle is 77.35%, ZrO by mass percentage 2the content of particle is 13.66% by mass percentage, waits BN, Co, Ni micron particle content of mass ratio to be respectively 3% by mass percentage; Then add in planetary ball mill by the composite granule prepared, ball-milling medium is dehydrated alcohol, and high purity aluminium oxide ball is abrading-ball, ball milling 24h, then at loft drier inner drying 24h, prepares Al 2o 3-ZrO 2/ Co-Ni-BN composite granule, carries out hot pressed sintering by composite granule in vacuum sintering funace, and vacuum heating-press sintering temperature is 1550 DEG C, hot pressing pressure is 30MPa, hot pressing time 30min, and vacuum tightness is 6 × 10 -2mPa, prepares Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material.Adopt monolateral three-point bending strength testing inspection material bending strength; Adopt the fracture toughness property of SENB method test material; Vickers penetration hardness method is adopted to measure the Vickers' hardness (Hv) of material; Scanning electron microscope (SEM) is adopted to have detected microstructure and the fracture apperance of material.
Prepared Al 2o 3-ZrO 2the performance test results of/Co-Ni-BN cermet mold material is: bending strength is 1372MPa, and fracture toughness property is 12.6MPa.m 1/2, hardness reaches 11.32Gpa(fracture apperance as shown in Figure 5).
Embodiment 4
With Al 2o 3nano particle, ZrO 2be raw material with BN, Co, Ni micron particle, Al 2o 3the content of nano particle is 74.8%, ZrO by mass percentage 2the content of particle is 13.2% by mass percentage, waits BN, Co, Ni micron particle content of mass ratio to be respectively 4% by mass percentage; Then add in planetary ball mill by the composite granule prepared, ball-milling medium is dehydrated alcohol, and high purity aluminium oxide ball is abrading-ball, ball milling 24h, then at loft drier inner drying 24h, prepares Al 2o 3-ZrO 2/ Co-Ni-BN composite granule, carries out hot pressed sintering by composite granule in vacuum sintering funace, and vacuum heating-press sintering temperature is 1550 DEG C, hot pressing pressure is 30MPa, hot pressing time 30min, and vacuum tightness is 6 × 10 -2mPa, prepares Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material.Adopt monolateral three-point bending strength testing inspection material bending strength; Adopt the fracture toughness property of SENB method test material; Vickers penetration hardness method is adopted to measure the Vickers' hardness (Hv) of material; Scanning electron microscope (SEM) is adopted to have detected microstructure and the fracture apperance of material.
Prepared Al 2o 3-ZrO 2the performance test results of/Co-Ni-BN cermet mold material is: bending strength is 1423MPa, and fracture toughness property is 14.7MPa.m 1/2, hardness reaches 13.4Gpa(fracture apperance as shown in Figure 5).
Embodiment 5
With Al 2o 3nano particle, ZrO 2be raw material with BN, Co, Ni micron particle, Al 2o 3the content of nano particle is 72.25%, ZrO by mass percentage 2the content of particle is 12.75% by mass percentage, waits BN, Co, Ni micron particle content of mass ratio to be respectively 5% by mass percentage; Then add in planetary ball mill by the composite granule prepared, ball-milling medium is dehydrated alcohol, and high purity aluminium oxide ball is abrading-ball, ball milling 24h, then at loft drier inner drying 24h, prepares Al 2o 3-ZrO 2/ Co-Ni-BN composite granule, carries out hot pressed sintering by composite granule in vacuum sintering funace, and vacuum heating-press sintering temperature is 1550 DEG C, hot pressing pressure is 30MPa, hot pressing time 30min, and vacuum tightness is 6 × 10 -2mPa, prepares Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material.Adopt monolateral three-point bending strength testing inspection material bending strength; Adopt the fracture toughness property of SENB method test material; Vickers penetration hardness method is adopted to measure the Vickers' hardness (Hv) of material; Scanning electron microscope (SEM) is adopted to have detected microstructure and the fracture apperance of material.
Prepared Al 2o 3-ZrO 2the performance test results of/Co-Ni-BN cermet mold material is: bending strength is 1408Mpa, and fracture toughness property is 13.4MPa.m 1/2, hardness reaches 12.52Gpa(fracture apperance as shown in Figure 5).

Claims (4)

1.Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material, is characterized in that, the batching of described material comprises raw material A l 2o 3powder, ZrO 2bN, Co, Ni powder of powder, equal proportion quality, Al 2o 3the content of nano particle is 72.25-82.45%, ZrO by mass percentage 2the content of micron particle be by mass percentage 12.75-14.55%, BN, Co, Ni in mass ratio 1:1:1 weighing content by total mass per-cent 3-15%; Material bending strength is 1014 ~ 1423Mpa, and fracture toughness property is 7-14.7MPa.m 1/2, hardness reaches 8.7-13.4Gpa.
2.Al 2o 3-ZrO 2/ Co-Ni-BN cermet mold material preparation method, is characterized in that, described method adopts following processing step one-stop operation:
1. prepare burden: by raw material A l 2o 3powder, ZrO 2bN, Co, Ni powder of powder, equal proportion quality is raw material, Al 2o 3the content of nano particle is 72.25-82.45%, ZrO by mass percentage 2the content of micron particle be by mass percentage 12.75-14.55%, BN, Co, Ni in mass ratio 1:1:1 weighing content by total mass per-cent 3-15%;
2. ball mill mixing, adds in ball mill by the material prepared, and ball milling 24 hours, puts into loft drier, and 60 DEG C of dryings 24 hours, prepare Al 2o 3-ZrO 2/ Co-Ni-BN composite granule;
3. powder compacting and sintering: the composite granule after step 2. being processed joins in vacuum sintering funace graphite jig, under vacuum, sintering temperature is 1450 DEG C ~ 1650 DEG C, and pressure is 30Mpa, and vacuum tightness is 6 × 10 -2,hot pressing 30 minutes.
3. Al according to claim 2 2o 3-ZrO 2/ Co-Ni-BN cermet mold material preparation method, is characterized in that, described step 2. middle ball-milling medium selects dehydrated alcohol, and abrading-ball is high purity aluminium oxide ball, and mixed composite granule is dry in loft drier.
4. Al according to claim 2 2o 3-ZrO 2/ Co-Ni-BN cermet mold material preparation method, is characterized in that, the described method steps 3. middle method of vacuum heating-press sintering that adopts sinters, and sintering temperature is 1450 DEG C ~ 1650 DEG C, and pressure is 30Mpa, and vacuum tightness is 6 × 10 -2, hot pressing 30 minutes.
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)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108101520A (en) * 2017-12-23 2018-06-01 深圳万佳互动科技有限公司 Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof
CN113186441A (en) * 2021-04-27 2021-07-30 湖北中烟工业有限责任公司 Nickel-zirconia cermets and uses thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108101520A (en) * 2017-12-23 2018-06-01 深圳万佳互动科技有限公司 Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof
CN113186441A (en) * 2021-04-27 2021-07-30 湖北中烟工业有限责任公司 Nickel-zirconia cermets and uses 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

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