CN107500777B - PCBN cutter material and preparation method thereof - Google Patents
PCBN cutter material and preparation method thereof Download PDFInfo
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- CN107500777B CN107500777B CN201710709833.9A CN201710709833A CN107500777B CN 107500777 B CN107500777 B CN 107500777B CN 201710709833 A CN201710709833 A CN 201710709833A CN 107500777 B CN107500777 B CN 107500777B
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- 239000000463 material Substances 0.000 title claims abstract description 33
- GJNGXPDXRVXSEH-UHFFFAOYSA-N 4-chlorobenzonitrile Chemical compound ClC1=CC=C(C#N)C=C1 GJNGXPDXRVXSEH-UHFFFAOYSA-N 0.000 title claims abstract 6
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 63
- 229910052582 BN Inorganic materials 0.000 claims abstract description 44
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 38
- 239000002223 garnet Substances 0.000 claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 238000010298 pulverizing process Methods 0.000 claims abstract description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 6
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 36
- 238000002156 mixing Methods 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 17
- 239000007767 bonding agent Substances 0.000 claims description 15
- 229910033181 TiB2 Inorganic materials 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- -1 ytterbium aluminum Chemical compound 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 6
- 238000007580 dry-mixing Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 238000007731 hot pressing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 abstract description 6
- 229910003454 ytterbium oxide Inorganic materials 0.000 abstract description 6
- 229940075624 ytterbium oxide Drugs 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
- C04B35/5831—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride based on cubic boron nitrides or Wurtzitic boron nitrides, including crystal structure transformation of powder
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention belongs to the field of polycrystalline cubic boron nitride cutter materials, and discloses a novel PCBN cutter material and a preparation method thereof. The material is prepared from the following raw materials in percentage by weight: 25-95% of cubic boron nitride powder and 5-75% of a binding agent; the weight percentage of the binding agent is the following composition a or composition b; composition a: 0<Zirconia content not more than 20 percent and 0 percent<Ytterbium aluminum garnet or ytterbium oxide less than or equal to 5%, and TiB in balance2Pulverizing; composition b: 1-10% of metal powder and 0<Zirconia content not more than 20 percent and 0 percent<Ytterbium aluminum garnet or ytterbium oxide less than or equal to 5%, and TiB in balance2Pulverizing; wherein the metal powder is one or a mixture of two of Ti powder and Al powder. The PCBN prepared by the invention has high hardness and excellent high-temperature performance.
Description
Technical Field
The invention belongs to the field of polycrystalline cubic boron nitride cutter materials, and particularly relates to a PCBN cutter material and a preparation method thereof.
Background
The cubic boron nitride cutter material has high hardness and wear resistance, stable chemical property and high oxidation resistance temperature, is particularly suitable for processing iron-based alloy materials which cannot be processed by diamond cutters, and has great market potential. The recent introduction and use of high speed cutting and non-lube cutting has made higher demands on the high temperature performance of the tool material.
The cubic boron nitride cutter material produced in China has low performance and is difficult to meet the use requirement, and the high-performance cubic boron nitride cutter material mainly depends on import. Therefore, the development of the high-performance cubic boron nitride cutter material has important significance.
Disclosure of Invention
In order to improve the high-temperature stability and the mechanical property of the PCBN, the invention aims to provide a PCBN cutter material and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
PCBN (polycrystalline cubic boron nitride) cutter material is prepared from the following raw materials in percentage by weight:
25-95% of cubic boron nitride powder and 5-75% of a binding agent; the weight percentage of the binding agent is the following composition a or composition b;
composition a: 0<Zirconia content not more than 20 percent and 0 percent<Ytterbium aluminum garnet or ytterbium oxide less than or equal to 5%, and TiB in balance2Pulverizing;
composition b: 1-10% of metal powder and 0<Zirconia content not more than 20 percent and 0 percent<Ytterbium aluminum garnet or ytterbium oxide less than or equal to 5%, and TiB in balance2Pulverizing; wherein the metal powder is one or a mixture of two of Ti powder and Al powder.
Preferably, the cubic boron nitride powder has a particle size of 0.1 to 100. mu.m, more preferably 0.5 to 15 μm.
Optimally, the feed is prepared from the following raw materials in percentage by weight:
80% of cubic boron nitride powder and 20% of a bonding agent; the cubic boron nitride powder has the particle size of 1-8 mu m; the weight percentage of the binding agent is the following composition a or composition b;
composition a: zirconium oxide 10%, ytterbium aluminum garnet or ytterbium oxide 0.5%, and the balance TiB2Pulverizing;
composition b: 3% of metal powder, 7% of zirconium oxide, 0.5% of ytterbium aluminum garnet or ytterbium oxide, and the balance of TiB2Pulverizing; wherein the metal powder is Ti powder.
The preparation method of the PCBN cutter material comprises the following steps:
firstly, processing cubic boron nitride powder: carrying out acid pickling on cubic boron nitride powder for 2-4 h by using 10-20 mol/L hydrofluoric acid, centrifugally separating the acid-pickled cubic boron nitride powder, washing with water, then washing with absolute ethyl alcohol, and then drying in vacuum;
mixing materials: mixing a bonding agent with the cubic boron nitride powder treated in the step I by adopting a dry mixing method or a wet mixing method, and drying after wet mixing;
thirdly, adopting one of the following three sintering methods to prepare the PCBN cutter material:
high temperature and high pressure method: putting the mixed powder in the step two into a pyrophyllite mould, and then carrying out vacuum drying for 20-40 min at the temperature of 200-400 ℃; then placing the pyrophyllite mould into a cubic press, and sintering for 10-30 min under the conditions that the temperature is 1200-1700 ℃ and the pressure is 4.5-7.5 GPa;
high temperature low pressure process: putting the mixed powder in the step two into a graphite mold, then putting the graphite mold into a hot pressing furnace, and sintering for 10-50 min under the conditions that the temperature is 1200-1600 ℃ and the pressure is 15-50 MPa in an inert atmosphere;
discharge plasma fast sintering method: and (4) putting the mixed powder in the step two into a graphite die, and sintering for 1-30 min at 1200-1500 ℃ under the vacuum or inert atmosphere by adopting a discharge plasma rapid sintering method.
Preferably, in the step I, the vacuum drying is drying for 8-12 hours at 40-80 ℃ in a vacuum drying oven.
Preferably, in step c, the vacuum pressure is less than 10 Pa.
Preferably, the step two is: uniformly mixing a bonding agent and the cubic boron nitride powder treated in the step I in a two-dimensional ball mill by adopting a wet mixing method, or uniformly mixing in a three-dimensional mixer by adopting a dry mixing method or a wet mixing method; adding alcohol or deionized water during wet mixing, and drying after wet mixing.
Preferably, when the mixture is carried out in a two-dimensional ball mill, the weight ratio of the total weight of the bonding agent and the cubic boron nitride powder to the weight of the grinding balls is 1 to (1-3), and the mixing time is 4-8 h.
Preferably, in the second step, after wet mixing, the mixture is placed in a drying oven for drying for 4-24 hours at the temperature of 100-140 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the PCBN prepared by the invention has high hardness and excellent high-temperature performance;
2. the controllability of the sintering process is strong: PCBN prepared by adopting a high-temperature high-pressure method has higher hardness; when the PCBN is prepared by adopting a high-temperature low-pressure method and a discharge plasma rapid sintering method, the production efficiency is high, and the PCBN has certain hardness;
3. the final performance of the PCBN cutter material can be conveniently controlled by adjusting the granularity of the raw material cubic boron nitride powder and the proportion of the cubic boron nitride powder and the binder.
Detailed Description
The technical solution of the present invention is further explained with reference to the following specific examples, but the scope of the present invention is not limited thereto.
Example 1
PCBN cutter material is prepared from the following raw materials in percentage by weight:
80% of cubic boron nitride powder and 20% of a bonding agent; the cubic boron nitride powder has the particle size of 1-8 mu m; the weight percentage of the binding agent is the following composition a or composition b;
composition a: zirconia 10%, ytterbium aluminium garnet 0.5%, balance TiB2Pulverizing;
composition b: 3% of metal powder, 7% of zirconium oxide, 0.5% of ytterbium aluminum garnet and the balance of TiB2Pulverizing; wherein all the metal powder is Ti powder.
The preparation method comprises the following steps:
firstly, processing cubic boron nitride powder: carrying out acid cleaning treatment on cubic boron nitride powder for 4 hours by using 15 mol/L hydrofluoric acid, centrifugally separating the acid cleaned cubic boron nitride powder, firstly washing with water and then washing with absolute ethyl alcohol, and then drying for 8 hours at 80 ℃ in a vacuum drying oven;
mixing materials: adding deionized water into the bonding agent and the cubic boron nitride powder treated in the step I in a two-dimensional ball mill, uniformly mixing by a wet mixing method, wherein the weight ratio of the total weight of the bonding agent and the cubic boron nitride powder to the weight of a grinding ball is 1: 1, the mixing time is 6 hours, and drying for 8 hours at 120 ℃ in a drying oven after wet mixing;
preparing PCBN cutter material by adopting the following high-temperature high-pressure method:
putting the mixed powder in the step two into a pyrophyllite mould, and then carrying out vacuum drying for 30min at the temperature of 300 ℃; then the pyrophyllite mould is placed into a cubic press and sintered for 15 min under the conditions that the temperature is 1400 ℃ and the pressure is 5 GPa.
Example 2
PCBN cutter material is prepared from the following raw materials in percentage by weight:
70% of cubic boron nitride powder and 30% of a bonding agent; the cubic boron nitride powder has the particle size of 8-15 mu m; the weight percentage of the binding agent is the following composition a or composition b;
composition a: 5% of zirconium oxide, 1% of ytterbium aluminum garnet and the balance of TiB2Pulverizing;
composition b: 1% of metal powder, 15% of zirconium oxide, 1% of ytterbium aluminum garnet and the balance of TiB2Pulverizing; wherein the metal powder is Ti powder and Al powder, and the weight ratio of the Ti powder to the Al powder is 1: 1.
The preparation method is the same as example 1.
Example 3
PCBN cutter material is prepared from the following raw materials in percentage by weight:
90% of cubic boron nitride powder and 10% of a bonding agent; the particle size of the cubic boron nitride powder is 4-10 mu m; the weight percentage of the binding agent is the following composition a or composition b;
composition a: 20% of zirconium oxide, 5% of ytterbium aluminum garnet and the balance of TiB2Pulverizing;
composition b: 10% of metal powder, 10% of zirconium oxide, 5% of ytterbium aluminum garnet and the balance of TiB2Pulverizing; wherein all the metal powder is Al powder.
The preparation method is the same as example 1.
Example 4
PCBN cutter material, the weight percentage composition of raw materials is the same as that of example 1.
The preparation method comprises the following steps:
firstly, processing cubic boron nitride powder: carrying out acid cleaning treatment on cubic boron nitride powder for 4 hours by using 15 mol/L hydrofluoric acid, centrifugally separating the acid cleaned cubic boron nitride powder, firstly washing with water and then washing with absolute ethyl alcohol, and then drying for 8 hours at 80 ℃ in a vacuum drying oven;
mixing materials: adding water into a bonding agent and the cubic boron nitride powder treated in the step I in a two-dimensional ball mill, uniformly mixing by a wet mixing method, wherein the weight ratio of the total weight of the bonding agent and the cubic boron nitride powder to a grinding ball is 1: 1, the mixing time is 6 hours, and drying for 8 hours at 120 ℃ in a drying oven after wet mixing;
thirdly, adopting the following discharge plasma rapid sintering method to prepare the PCBN cutter material:
and (4) filling the mixed powder in the step two into a graphite die, and sintering for 20 min at 1400 ℃ under a vacuum condition (the pressure is less than 10 Pa) by adopting a discharge plasma rapid sintering method.
Comparative example 1
The difference from example 1 is that: the compositions a and b were the same as example 1 except that ytterbium aluminum garnet was not included.
Examples 1-3 and comparative example 1 the performance data for the PCBN cutter material prepared are given in the table below.
From the table, it can be seen that: the preparation method and the composition of the raw materials directly influence the performance of the finally prepared PCBN cutter material, but the PCBN cutter material prepared by adopting the high-temperature high-pressure method has the best performance under the raw material composition of the example 1.
Claims (7)
- PCBN cutter material is characterized by being prepared from the following raw materials in percentage by weight:80% of cubic boron nitride powder and 20% of a bonding agent; the cubic boron nitride powder has the particle size of 1-8 mu m; the weight percentage of the binding agent is the following composition a or composition b;composition a: zirconia 10%, ytterbium aluminium garnet 0.5%, balance TiB2Pulverizing;composition b: 3% of metal powder, 7% of zirconium oxide, 0.5% of ytterbium aluminum garnet and the balance of TiB2Pulverizing; wherein the metal powder is Ti powder.
- 2. A method of making PCBN cutter material as claimed in claim 1, in which: the method comprises the following steps:firstly, processing cubic boron nitride powder: carrying out acid pickling on cubic boron nitride powder for 2-4 h by using 10-20 mol/L hydrofluoric acid, carrying out centrifugal separation on the acid-pickled cubic boron nitride powder, washing with water and then absolute ethyl alcohol, and then carrying out vacuum drying;mixing materials: mixing a bonding agent with the cubic boron nitride powder treated in the step I by adopting a dry mixing method or a wet mixing method, and drying after wet mixing;thirdly, adopting one of the following three sintering methods to prepare the PCBN cutter material:a. high temperature and high pressure method:putting the mixed powder in the step two into a pyrophyllite mould, and then carrying out vacuum drying for 20-40 min at the temperature of 200-400 ℃; then placing the pyrophyllite mould into a cubic press, and sintering for 10-30 min under the conditions that the temperature is 1200-1700 ℃ and the pressure is 4.5-7.5 GPa;b. high temperature low pressure process:putting the mixed powder in the step two into a graphite mold, then putting the graphite mold into a hot pressing furnace, and sintering for 10-50 min under the conditions that the temperature is 1200-1600 ℃ and the pressure is 15-50 MPa in an inert atmosphere;c. discharge plasma fast sintering method:and (4) putting the mixed powder in the step two into a graphite die, and sintering for 1-30 min at 1200-1500 ℃ under the vacuum or inert atmosphere by adopting a discharge plasma rapid sintering method.
- 3. The method of claim 2, wherein: in the step I, the vacuum drying is drying for 8-12 hours at 40-80 ℃ in a vacuum drying oven.
- 4. The method of claim 2, wherein: in step c, the vacuum pressure is less than 10 Pa.
- 5. The method of claim 2, wherein step (ii) is: uniformly mixing a bonding agent and the cubic boron nitride powder treated in the step I in a two-dimensional ball mill by adopting a wet mixing method, or uniformly mixing in a three-dimensional mixer by adopting a dry mixing method or a wet mixing method; adding alcohol or deionized water during wet mixing, and drying after wet mixing.
- 6. The method of claim 5, wherein: when the mixture is mixed in a two-dimensional ball mill, the weight ratio of the total weight of the bonding agent and the cubic boron nitride powder to the weight of the grinding balls is 1: 1-3, and the mixing time is 4-8 h.
- 7. The method of claim 2, 5 or 6, wherein: and step two, after wet mixing, drying the mixture in a drying oven at 100-140 ℃ for 4-24 hours.
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| "ZrO2(Y2O3)增韧的Si3N4中介结合的聚晶立方氮化硼";臧建兵等;《材料研究学报》;20001231;第14卷(第6期);第1节和表1 * |
| "聚晶立方氮化硼刀具及其制造技术综述";刘一波等;《地质与勘探》;19960731;第32卷(第4期);第2.1.2节 * |
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