CN111362703B - Polycrystalline cubic boron nitride cutter sintered at low pressure and preparation method - Google Patents
Polycrystalline cubic boron nitride cutter sintered at low pressure and preparation method Download PDFInfo
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- CN111362703B CN111362703B CN202010233513.2A CN202010233513A CN111362703B CN 111362703 B CN111362703 B CN 111362703B CN 202010233513 A CN202010233513 A CN 202010233513A CN 111362703 B CN111362703 B CN 111362703B
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 61
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 65
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- 229910002804 graphite Inorganic materials 0.000 claims description 20
- 239000010439 graphite Substances 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention discloses a polycrystalline cubic boron nitride cutter sintered at low pressure and a preparation method thereof, wherein the polycrystalline cubic boron nitride cutter takes cBN micro powder, hBN micro powder and lithium tetraborate as raw materials and adopts a spark plasma sintering process to prepare a polycrystalline cubic boron nitride sintered body; and processing the polycrystalline cubic boron nitride sintered body into a polycrystalline cubic boron nitride cutter. The invention has simple process, convenient manufacture, energy saving and environmental protection; by adopting a spark plasma sintering process, the polycrystalline cubic boron nitride cutter material can be prepared at low pressure; the sintered polycrystalline cubic boron nitride material prepared by the invention has the unique properties of two BN phases, and is superior to the existing polycrystalline cubic boron nitride cutter material with ceramic binder and metal binder; the polycrystalline cubic boron nitride cutter obtained by processing the polycrystalline cubic boron nitride powder disclosed by the invention has the density of 95-98% and the microhardness of 36.5-51.5 GPa.
Description
Technical Field
The invention relates to the technical field of superhard cutting tools, in particular to a low-pressure sintered polycrystalline cubic boron nitride cutter and a preparation method thereof.
Background
Polycrystalline cubic boron nitride (PcBN) has characteristics of high hardness, high wear resistance, high thermal conductivity, high chemical stability, excellent impact toughness, and the like, and has received great attention. As a superhard tool material, the PcBN is more and more widely applied to modern cutting processing, can better meet the requirements of severe processing conditions during hard cutting, high-speed cutting and dry cutting on the tool material, is suitable for application to automatic production lines and numerical control processing equipment, and obviously improves the production efficiency. Different from a diamond cutter, the cubic boron nitride cutter has better high-temperature resistance, shows good chemical stability to iron group metal elements at high temperature, has strong anti-bonding capability, and is suitable for cutting and processing various iron-based materials (such as tool steel, high-speed steel, bearing steel, powder metallurgy metal, high-strength steel and the like), cobalt-based materials and nickel-based materials.
The traditional preparation method of the polycrystalline cubic boron nitride cutter is a high-temperature and high-pressure method (the pressure is 3-8Gpa, and the temperature is 1300-. The Spark Plasma Sintering (SPS) process is a rapid sintering preparation technology developed in recent years, has the characteristics of high temperature rise speed, short sintering time, rapid cooling, energy conservation, environmental protection and the like, and is widely applied to the preparation of superhard materials. For example, CN1817434A, takes binder and 40-90% cBN as raw materials, utilizes the spark plasma sintering process to prepare the polycrystalline cubic boron nitride sintered body at lower pressure and relatively lower temperature, the method overcomes the defects of the traditional method, does not need a top hammer or a die of a high-pressure cavity of hard alloy, greatly reduces working pressure and die consumption, and greatly improves the size and the shape of the product.
However, the existing method for preparing the polycrystalline cubic boron nitride cutter by using the spark plasma sintering process also has the problems of high sintering temperature, easy conversion of cBN into hBN and the like, so that the density of the polycrystalline cubic boron nitride prepared by using the spark plasma sintering process is smaller, and the application of the cutter is limited.
Disclosure of Invention
The polycrystalline cubic boron nitride sintered body material with high density and high strength is prepared by taking cBN micro powder, hBN micro powder and lithium tetraborate as raw materials and utilizing a spark plasma sintering process at lower pressure and temperature, and the sintered body material is used for processing a corresponding cutter. In order to achieve the purpose, the invention is implemented according to the following technical scheme:
a preparation method of a low-pressure sintered polycrystalline cubic boron nitride cutter is characterized in that the polycrystalline cubic boron nitride cutter takes cBN micro powder, hBN micro powder and lithium tetraborate as raw materials, and a polycrystalline cubic boron nitride sintered body is prepared by adopting a spark plasma sintering process; and processing the polycrystalline cubic boron nitride sintered body into a polycrystalline cubic boron nitride cutter.
Preferably, the preparation method of the polycrystalline cubic boron nitride sintered body comprises the following steps:
(1) mixing materials: uniformly grinding and mixing the cBN micro powder, the hBN micro powder and the lithium tetraborate, and filling the mixture into a graphite die;
(2) and (3) heat treatment: placing the filled graphite mold in a nitrogen atmosphere furnace, carrying out heat treatment at 750 ℃ for 2-4 h, and transferring to a 150 ℃ oven for drying for 6-8 h;
(3) spark plasma sintering: placing the dried graphite mold in a discharge plasma sintering cavity, vacuumizing to below 6Pa, heating to 1000-1400 ℃ at a heating rate of 150 ℃/min, sintering under the pressure condition of 30-100 MPa, and keeping the temperature for 5-20 min;
(4) and (3) cooling: and after sintering, cooling the graphite mold along with the furnace, releasing pressure and demolding to obtain the high-density high-strength polycrystalline cubic boron nitride sintered body.
Preferably, the cBN micro powder, hBN micro powder and lithium tetraborate have the following composition: the volume percentage content of the cBN micro powder is 60-90%, the volume percentage content of the hBN micro powder is 10-30%, and the volume percentage content of the lithium tetraborate is 0-10%.
Preferably, the cBN micro powder is a mixture of cBN micro powder with the particle size of 2-10 mu m and cBN micro powder with the particle size of 30-100 mu m; the volume ratio of cBN micro powder with the granularity of 2-10 mu m to cBN micro powder with the granularity of 30-100 mu m is V2~10μm:V30~100μm=1:4。
Preferably, the particle size of the hBN micro powder is 30-50 microns.
The invention has the following function principle:
according to the invention, the BN micropowder with a proper particle size is selected and mixed according to a certain proportion, so that an ideal stacking structure can be obtained; the more appropriate cBN grain size range and 750 ℃ heat treatment both help to prevent cBN to hBN transformation; the good lubricating property of hBN is beneficial to mutual contact of cBN particles in the sintering process; after sintering processing by the SPS process, the polycrystalline cubic boron nitride cutter with high density and high strength can be obtained, the density is 96-98%, and the microhardness of the cutter is as high as 36.5-51.5 GPa.
The invention has simple process and easily obtained equipment, and can prepare the polycrystalline cubic boron nitride sintered body material with wide application and high compactness under lower pressure and temperature, and the material is used for processing the polycrystalline cubic boron nitride cutter. The cutter material prepared by the invention has the unique properties of two BN phases, and is superior to the polycrystalline cubic boron nitride cutter material of the existing ceramic binder and metal binder. The hBN binder imparts self-lubricating properties to the polycrystalline cubic boron nitride (PcBN) of the present invention. Compared with the PcBN cutter material of the metal binder, the low-pressure sintered polycrystalline cubic boron nitride material avoids polluting processed metal devices in the process of grinding or polishing the metal devices, thereby having wide application.
Compared with the prior art, the invention has the beneficial effects that:
the invention has simple process, convenient manufacture, energy saving and environmental protection; by adopting a spark plasma sintering process, the polycrystalline cubic boron nitride cutter material can be prepared at low pressure; the sintered polycrystalline cubic boron nitride material prepared by the invention has the unique properties of two BN phases, and is superior to the existing polycrystalline cubic boron nitride cutter material with ceramic binder and metal binder; the polycrystalline cubic boron nitride cutter obtained by processing the polycrystalline cubic boron nitride powder disclosed by the invention has the density of 95-98% and the microhardness of 36.5-51.5 GPa.
Detailed Description
The present invention will be further described with reference to specific examples, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
A preparation method of a low-pressure sintered polycrystalline cubic boron nitride cutter comprises the following steps:
(1) mixing materials: uniformly grinding and mixing the cBN micro powder, the hBN micro powder and the lithium tetraborate, and filling the mixture into a graphite die; the volume percentage contents of the cBN micro powder, the hBN micro powder and the lithium tetraborate are as follows: 70% of cBN micro powder, 25% of hBN micro powder and 5% of lithium tetraborate; the cBN micro powder is a mixture of cBN micro powder with the particle size of 2-4 mu m and cBN micro powder with the particle size of 30-40 mu m, and the volume ratio of the cBN micro powder to the cBN micro powder is V2~4μm:V30~40μm=1: 4; the particle size of the hBN micro powder is 40-50 mu m;
(2) and (3) heat treatment: placing the filled graphite mold in a nitrogen atmosphere furnace, carrying out heat treatment at 750 ℃ for 3h, and transferring to a 150 ℃ oven for drying for 7 h;
(3) spark plasma sintering: placing the dried graphite mold in a discharge plasma sintering chamber, vacuumizing to below 6Pa, heating to 1050 ℃ at a heating rate of 150 ℃/min, keeping the pressure at 50MPa, and keeping the temperature for 15 min;
(4) and (3) cooling: after sintering, cooling the graphite mold along with the furnace, releasing pressure and demolding to obtain a high-density high-strength polycrystalline cubic boron nitride sintered body;
(5) processing a cutter: and processing the polycrystalline cubic boron nitride sintered body to obtain the polycrystalline cubic boron nitride cutter.
The polycrystalline cubic boron nitride cutter processed and obtained in the embodiment is detected to have the density of 96%, the microhardness of 40 +/-3.5 GPa and the bending strength of 375 +/-23 MPa.
Example 2
A preparation method of a low-pressure sintered polycrystalline cubic boron nitride cutter comprises the following steps:
(1) mixing materials: uniformly grinding and mixing the cBN micro powder, the hBN micro powder and the lithium tetraborate, and filling the mixture into a graphite die; the volume percentage contents of the cBN micro powder, the hBN micro powder and the lithium tetraborate are as follows: 75% of cBN micro powder, 20% of hBN micro powder and 5% of lithium tetraborate; cBN micropowder is a mixture of cBN micropowder having a particle size of 4 to 8 μm and cBN micropowder having a particle size of 40 to 50 μm in a volume ratio of V4~8μm:V40~50μm=1: 4; the particle size of the hBN micro powder is 30-40 mu m;
(2) and (3) heat treatment: placing the filled graphite mold in a nitrogen atmosphere furnace, carrying out heat treatment at 750 ℃ for 3h, and transferring to a 150 ℃ oven for drying for 7 h;
(3) spark plasma sintering: placing the dried graphite mold in a discharge plasma sintering chamber, vacuumizing to below 6Pa, heating to 1200 ℃ at a heating rate of 150 ℃/min, keeping the pressure at 80MPa, and keeping the temperature for 10 min;
(4) and (3) cooling: after sintering, cooling the graphite mold along with the furnace, releasing pressure and demolding to obtain a high-density high-strength polycrystalline cubic boron nitride sintered body;
(5) processing a cutter: and processing the polycrystalline cubic boron nitride sintered body to obtain the polycrystalline cubic boron nitride cutter.
The detection shows that the density of the polycrystalline cubic boron nitride cutter obtained by processing in the embodiment reaches 97%, the microhardness of the cutter is 43 +/-2.5 GPa, and the bending strength is 390 +/-18 MPa.
Example 3
A preparation method of a low-pressure sintered polycrystalline cubic boron nitride cutter comprises the following steps:
(1) mixing materials: uniformly grinding and mixing the cBN micro powder, the hBN micro powder and the lithium tetraborate, and filling the mixture into a graphite die; the volume percentage contents of the cBN micro powder, the hBN micro powder and the lithium tetraborate are as follows: 78% of cBN micro powder, 15% of hBN micro powder and 7% of lithium tetraborate; the cBN micro powder is a mixture of cBN micro powder with the particle size of 2-4 mu m and cBN micro powder with the particle size of 30-40 mu m, and the volume ratio of the cBN micro powder to the cBN micro powder is V2~4μm:V30~40μm=1: 4; the particle size of the hBN micro powder is 40-50 mu m;
(2) and (3) heat treatment: placing the filled graphite mold in a nitrogen atmosphere furnace, carrying out heat treatment at 750 ℃ for 3h, and transferring to a 150 ℃ oven for drying for 7 h;
(3) spark plasma sintering: placing the dried graphite mold in a discharge plasma sintering chamber, vacuumizing to below 6Pa, heating to 1300 ℃ at a heating rate of 150 ℃/min, keeping the pressure at 100MPa, and keeping the temperature for 10 min;
(4) and (3) cooling: after sintering, cooling the graphite mold along with the furnace, releasing pressure and demolding to obtain a high-density high-strength polycrystalline cubic boron nitride sintered body;
(5) processing a cutter: and processing the polycrystalline cubic boron nitride sintered body to obtain the polycrystalline cubic boron nitride cutter.
The polycrystalline cubic boron nitride cutter obtained by processing in the embodiment is detected to have the density of 98%, the microhardness of 47 +/-4.5 GPa and the bending strength of 430 +/-25 MPa.
The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.
Claims (2)
1. A preparation method of a low-pressure sintered polycrystalline cubic boron nitride cutter is characterized by comprising the following steps: the polycrystalline cubic boron nitride cutter is prepared by taking cBN micro powder, hBN micro powder and lithium tetraborate as raw materials and adopting a discharge plasma sintering process to obtain a polycrystalline cubic boron nitride sintered body; processing the polycrystalline cubic boron nitride sintered body into a polycrystalline cubic boron nitride cutter;
the preparation method of the polycrystalline cubic boron nitride sintered body comprises the following steps:
(1) mixing materials: uniformly grinding and mixing the cBN micro powder, the hBN micro powder and the lithium tetraborate, and filling the mixture into a graphite die;
(2) and (3) heat treatment: placing the filled graphite mold in a nitrogen atmosphere furnace, carrying out heat treatment at 750 ℃ for 2-4 h, and transferring to a 150 ℃ oven for drying for 6-8 h;
(3) spark plasma sintering: placing the dried graphite mold in a discharge plasma sintering cavity, vacuumizing to below 6Pa, heating to 1000-1400 ℃ at a heating rate of 150 ℃/min, sintering under the pressure condition of 30-100 MPa, and keeping the temperature for 5-20 min;
(4) and (3) cooling: after sintering, cooling the graphite mold along with the furnace, releasing pressure and demolding to obtain a high-density high-strength polycrystalline cubic boron nitride sintered body;
the components of the cBN micro powder, the hBN micro powder and the lithium tetraborate are as follows: the volume percentage content of the cBN micro powder is 60-90%, the volume percentage content of the hBN micro powder is 10-30%, and the volume percentage content of the lithium tetraborate is 0-10%;
the cBN micro powder is a mixture of cBN micro powder with the particle size of 2-10 mu m and cBN micro powder with the particle size of 30-100 mu m; the volume ratio of cBN micro powder with the granularity of 2-10 mu m to cBN micro powder with the granularity of 30-100 mu m is V2~10μm:V30~100μm=1:4；
The particle size of the hBN micro powder is 30-50 mu m.
2. A polycrystalline cubic boron nitride cutting tool prepared by the method of claim 1.
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| CN1817434A (en) * | 2006-01-11 | 2006-08-16 | 燕山大学 | Method for sintering polycrystal cubic boron nitride by plasma discharge |
| CN101058507A (en) * | 2006-04-20 | 2007-10-24 | 宁波密克斯新材料科技有限公司 | Silicon carbide-boron nitride ceramics composite material |
| CN101230454A (en) * | 2007-12-28 | 2008-07-30 | 北京工业大学 | Method for preparing cubic boron nitride thin film |
| CN110885250A (en) * | 2019-11-20 | 2020-03-17 | 天津大学 | Low-cost high-performance polycrystalline cubic boron nitride cutter material |
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| JP6447197B2 (en) * | 2015-02-04 | 2019-01-09 | 住友電気工業株式会社 | Cubic boron nitride polycrystal, cutting tool, wear-resistant tool, grinding tool, and method for producing cubic boron nitride polycrystal |
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| CN1817434A (en) * | 2006-01-11 | 2006-08-16 | 燕山大学 | Method for sintering polycrystal cubic boron nitride by plasma discharge |
| CN101058507A (en) * | 2006-04-20 | 2007-10-24 | 宁波密克斯新材料科技有限公司 | Silicon carbide-boron nitride ceramics composite material |
| CN101230454A (en) * | 2007-12-28 | 2008-07-30 | 北京工业大学 | Method for preparing cubic boron nitride thin film |
| CN110885250A (en) * | 2019-11-20 | 2020-03-17 | 天津大学 | Low-cost high-performance polycrystalline cubic boron nitride cutter material |
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