CN115745602A - Zirconia-based ceramic composite material and preparation method and application thereof - Google Patents
Zirconia-based ceramic composite material and preparation method and application thereof Download PDFInfo
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- CN115745602A CN115745602A CN202211590373.XA CN202211590373A CN115745602A CN 115745602 A CN115745602 A CN 115745602A CN 202211590373 A CN202211590373 A CN 202211590373A CN 115745602 A CN115745602 A CN 115745602A
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 239000000919 ceramic Substances 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 239000011812 mixed powder Substances 0.000 claims abstract description 14
- 239000011858 nanopowder Substances 0.000 claims abstract description 12
- 229910052582 BN Inorganic materials 0.000 claims abstract description 10
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 4
- 239000011159 matrix material Substances 0.000 claims description 9
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 5
- 238000000713 high-energy ball milling Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000005728 strengthening Methods 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
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- 238000005303 weighing Methods 0.000 description 2
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
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- 238000009792 diffusion process Methods 0.000 description 1
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- 239000008187 granular material Substances 0.000 description 1
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- 229940057995 liquid paraffin Drugs 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
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Abstract
The invention provides a preparation method of a zirconia-based ceramic composite material, which comprises the following steps: uniformly mixing zirconia powder and CBN nano powder to obtain mixed powder, and then carrying out plasma sintering treatment on the mixed powder, wherein the mass ratio of the zirconia powder to the CBN nano powder is (90-98.5) to (1.5-10) calculated by 100 parts by mass. The zirconia-based ceramic composite material prepared by the method realizes that a small amount of nano cubic boron nitride is added into a zirconia-based material to achieve the purpose of hard point dispersion strengthening, thereby improving the hardness and toughness of the zirconia ceramic. Meanwhile, in the spark plasma sintering process, CBN particles and zirconia powder are subjected to interface reaction to generate ZrN and ZrB 2 The bonding force of the crystal boundary is increased, the crystal boundary is strengthened, and the density and the strength of the material are improved. The invention also provides a zirconia-based ceramic composite material and application thereof.
Description
Technical Field
The invention belongs to the technical field of ceramic cutters, and particularly relates to a zirconia-based ceramic composite material and a preparation method and application thereof.
Background
The ceramic cutter material has high hardness and wear resistance, good high-temperature performance, small affinity effect with metal, difficult bonding with metal and good chemical stability, and has very wide application in the industries of machinery, electronics, petroleum, chemical engineering, precise instruments, medical instruments, bioengineering and the like. Zirconia ceramic materials have been made into ceramic cutting tools, artificial teeth, ball milling media, wear resistant components, medical cutting tool materials, and the like. Besides the advantages, the zirconia ceramic material also has the characteristics of no magnetism, no static electricity, long service life, high precision, good biocompatibility and the like. Therefore, the zirconia ceramic has unique physical properties and good mechanical properties, so that the zirconia ceramic has important research significance in the fields of functional ceramics and structural ceramics.
The chemical bonds of zirconia ceramics are mainly ionic bonds, unlike metallic bonds in metallic materials. When the zirconia material is under the action of a large impact force, the slippage of dislocation is difficult due to high ionic bond strength and difficult bond breakage, and the recombination is difficult after the ionic bond is broken; this contributes to the intrinsic brittleness of the zirconia ceramic. Therefore, zirconia ceramic materials often have the characteristics of high brittleness and poor toughness, so that the zirconia ceramic materials are difficult to deform, and the application of the zirconia ceramic materials in structural ceramic components is severely limited. Meanwhile, the zirconia ceramic material has a crystal structure different from that of a metal material, and once micro cracks are generated in the material, the cracks can be rapidly expanded, so that the material is subjected to brittle fracture, the use safety of the material is seriously influenced, and the application of zirconia devices such as wear-resistant cutters, wear-resistant zero devices and medical cutter materials is also influenced.
Disclosure of Invention
In view of the above, the present invention provides a zirconia-based ceramic composite material, a method for preparing the same and applications thereof, so as to solve the above problems.
The invention relates to a preparation method of a zirconia-based ceramic composite material, which comprises the following steps: uniformly mixing zirconia powder and CBN nano powder to obtain mixed powder, and then carrying out plasma sintering treatment on the mixed powder, wherein the mass ratio of the zirconia powder to the CBN nano powder is (90-98.5) to (1.5-10) calculated by 100 parts by mass.
Based on the preparation method, the zirconia powder has the granularity of 1-5 mu m, small grain size, narrow distribution, good appearance, uniform distribution, uniform microstructure of sintered ceramics and relatively good strength and toughness. The granularity of the CBN nano powder is less than or equal to 50 nm, so that the nano CBN has small size effect and interface disorder, the brittleness of the zirconia ceramic is reduced, and the surface smoothness of the cutter is improved.
Based on the preparation method, the method for obtaining the mixed powder comprises the following steps: and carrying out high-energy ball milling treatment on the zirconium oxide powder and the CBN nano powder to obtain the uniformly mixed powder. Other conventional mixing methods can be adopted in the step, and the zirconium oxide powder and the CBN nano powder can be uniformly mixed.
Based on the preparation method, the plasma sintering treatment comprises the following steps: the mixed powder is pre-pressed and then sintered by the discharge plasma, wherein the sintering pressure is 50-80 MPa, the sintering temperature is 1300-1500 ℃, and the heat preservation time is 30-50 min. The purpose of performing pre-pressing treatment in the step is to perform and improve the density of the powder, which is beneficial to the forming of a sintered body and the improvement of the density. In addition, the surface of the powder particles can be purified and activated by electric shock waves and electrons generated by discharge in the step of spark plasma sintering, a large amount of joule heat is generated by high-frequency discontinuous current when the powder particles are contacted, and discharge heat can be generated in the non-contacted part, so that the diffusion of the particles is promoted, the rapid sintering of the powder is realized, the sintering time is shortened, the efficiency is improved, the energy is saved, and a sintered body with uniform microstructure, excellent mechanical property and high density can be obtained.
The invention also provides a zirconia-based ceramic composite material prepared by the method, which comprises the following components: zirconia matrix, cubic boron nitride particles uniformly dispersed in the zirconia matrix, and ZrN and ZrB coated on the surfaces of the cubic boron nitride particles 2 。
Based on the above, the zirconia matrix accounts for 90-98.5% of the zirconia-based ceramic composite material by mass.
Based on the above, the compactness of the zirconia-based ceramic composite material is greater than or equal to 95%. Preferably 95%, 95.5%, 96%, 96.5%, 97%, 97.5%, 98%, 98.5%, 99%, 99.5%.
The invention also provides application of the zirconia-based ceramic composite material in the fields of wear-resistant cutters, wear-resistant parts, medical cutter materials and the like.
Therefore, the preparation method provided by the invention is mainly prepared by processing mixed powder of zirconia powder and CBN nano powder through plasma sintering, so that the prepared zirconia-based ceramic composite material is added with a small amount of nano cubic boron nitride in the zirconia-based material to achieve the purpose of hard point dispersion strengthening, and the abnormal growth of zirconia grains can be inhibited in the sintering process of the nano particle reinforced phase, so that the structure of the zirconia-based material is refined, the grains are smaller, the microstructure is denser, the strength of the zirconia-based ceramic composite material is higher, because the smaller the grain size of zirconia is, the denser the microstructure is relatively, and the defects such as pores in the composite material are reduced, thereby improving the hardness and toughness of the zirconia ceramic. Meanwhile, in the spark plasma sintering process, CBN particles and zirconia powder are subjected to interface reaction to generate ZrN and ZrB 2 The bonding force of the crystal boundary is further increased, the crystal boundary is strengthened, and the density and the strength of the material are improved.
Tests prove that the density of the zirconia-based ceramic composite material is more than or equal to 95 percent, the Vickers hardness is 13.9-15.5 Gpa, and the fracture toughness is 8.83-10.56 MPa.m 1/2 . Therefore, the zirconia-based ceramic composite material provided by the invention has higher density, toughness and strength, and can be used as a material for wear-resistant tools, wear-resistant parts and medical tools, so that the tools are not easy to crack in the processing process, the safety and wear resistance of tool processing are improved, the service life is prolonged, and the processing efficiency is improved.
Drawings
Fig. 1 is a schematic structural diagram of a zirconia-based ceramic composite provided in an embodiment of the present invention.
FIGS. 2 to 6 are SEM photographs of zirconia-based ceramic composites provided in examples 1 to 5 of the present invention.
Wherein, the reference numbers in the upper drawing: 1. a zirconia matrix; 2. cubic boron nitride particles; 3. ZrN and ZrB 2 And (3) granules.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
Examples 1 to 5
zirconium oxide ZrO 2 Uniformly mixing the powder and the nano cubic boron nitride powder by high-energy ball milling according to the mass ratio shown in the table 1 to obtain mixed powder; placing the mixed powder in a tool steel mold, performing prepressing treatment by using a press to form a material rod, and performing discharge plasma sintering treatment on the material rod by using the sintering parameters shown in Table 1 to obtain ZrO shown in figures 1-6 2 A base ceramic composite material. The ZrO 2 The base ceramic composite material comprises a zirconia matrix 1, cubic boron nitride particles 2 uniformly dispersed in the zirconia matrix 1, and ZrN and ZrB coated on the surfaces of the cubic boron nitride particles 2 2 And (3) particles.
TABLE 1 Process parameters involved in the preparation Process
Comparative examples 1 to 3
Comparative examples 1 to 3 each provide 3Y-ZrO 2 The preparation method of the ceramic composite material is basically the same as that provided in the embodiment, and the main difference is that: comparative examples 1 to 3 all with zirconium oxide ZrO 2 And yttrium oxide Y 2 O 3 The raw materials were used, and the mass ratios of the two were the same as in examples 1 to 3, respectively.
Performance testing
Hardness, toughness and compactness of the ceramic composite materials provided in examples 1 to 5 and comparative examples 1 to 3 were measured, respectively, and the results are shown in table 2. Wherein, the hardness and the toughness are measured by adopting the current industry standard; the method of measuring the density is as follows.
The density measurement method comprises the following steps: based on the Archimedes drainage principle, the dry weight m of the sample at room temperature is weighed by placing the sample on an analytical balance 1 Putting the sample into molten paraffin to ensure that the sample is completely immersed in the liquid paraffin; taking out the sample, placing the sample on weighing paper, scraping off excessive paraffin on the surface of the sample, cooling the sample to room temperature, and measuring the sealing wax weight m of the sample on an analytical balance 2 Weighing the floating weight m of the wax sealing sample in the water medium 3 The experiment was repeated 3 times, and the results were averaged to calculate the actual density ρ and the density (i.e., relative density) W of the sintered sample. In the formula:
ρ=m 1 ρ water (I) /(m 2 -m 3 )
W=ρ/ρ 0 ×100%
ρ Water (W) Representing the density of water at room temperature, taking the density value of water at 20 ℃, rho Water (W) =0.998203g/cm 3 ；ρ 0 Representing the theoretical density of the zirconia-based bulk material.
TABLE 2 ZrO 2 Performance parameter table of base ceramic composite material
Applications of
The zirconia-based ceramic composite materials provided by the examples 2-4 and the comparative examples 2-3 are respectively made into a standard cutter CNMN120716S05020 marketed by a cost company, and then the abrasion ratio detection is carried out according to the current national industry standard (JB 3235-83), wherein a standard grinding wheel TL80# Z2AP 100X 16X 20 is used for carrying out the abrasion ratio detection on a JS71-A type abrasion ratio tester, the linear speed of the grinding wheel is 25 m/S, the abrasion amount of the grinding wheel is not less than g, and the abrasion amount of the sample is not less than 0.2 mg.
TABLE 3 wear ratio test results for cutting tools
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.
Claims (8)
1. A method for preparing a zirconia-based ceramic composite material, comprising the steps of: uniformly mixing zirconia powder and CBN nano powder to obtain mixed powder, and then carrying out plasma sintering treatment on the mixed powder, wherein the mass ratio of the zirconia powder to the CBN nano powder is (90-98.5) to (1.5-10) calculated by 100 parts by mass.
2. The method of claim 1, wherein: the granularity of the zirconia powder is 1-5 mu m, and the granularity of the CBN nano powder is less than or equal to 50 nm.
3. The method of claim 2, wherein: the step of obtaining the mixed powder comprises the step of carrying out high-energy ball milling treatment on the zirconium oxide powder and the CBN nano powder.
4. The production method according to claim 1, 2 or 3, characterized in that: the plasma sintering treatment comprises the following steps: the mixed powder is pre-pressed and then spark plasma sintering is carried out, wherein the sintering pressure is 50-80 MPa, the sintering temperature is 1300-1500 ℃, and the heat preservation time is 30-50 min.
5. A zirconia-based ceramic composite comprising: zirconia matrix, cubic boron nitride uniformly dispersed in the zirconia matrix and ZrN and ZrB coated on the surface of the cubic boron nitride 2 。
6. The ceramic composite of claim 5, wherein: the zirconia matrix accounts for 90-98.5% of the zirconia-based ceramic composite material by mass.
7. The ceramic composite of claim 6, wherein: the compactness of the zirconia-based ceramic composite material is greater than or equal to 95%.
8. Use of the zirconia-based ceramic composite of claim 5 or 6 or 7 in a wear resistant tool, wear resistant component or medical tool material.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05246760A (en) * | 1991-05-30 | 1993-09-24 | Matsushita Electric Works Ltd | Zirconia-based composite ceramic sintered compact and its production |
| US20070049484A1 (en) * | 2005-02-24 | 2007-03-01 | Kear Bernard H | Nanocomposite ceramics and process for making the same |
| CN106687426A (en) * | 2015-04-20 | 2017-05-17 | 住友电气工业株式会社 | Sintered body and cutting tool including same |
| CN106892660A (en) * | 2017-01-16 | 2017-06-27 | 广东百工新材料科技有限公司 | A kind of ceramic mobile phone bonnet and preparation method thereof |
| CN113754431A (en) * | 2021-09-09 | 2021-12-07 | 浙江大学 | Method for preparing nano polycrystalline composite phase zirconia by ultrahigh pressure/high temperature phase change method |
| CN114351026A (en) * | 2022-01-12 | 2022-04-15 | 富耐克超硬材料股份有限公司 | Polycrystalline cubic boron nitride composite material |
-
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- 2022-12-12 CN CN202211590373.XA patent/CN115745602B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05246760A (en) * | 1991-05-30 | 1993-09-24 | Matsushita Electric Works Ltd | Zirconia-based composite ceramic sintered compact and its production |
| US20070049484A1 (en) * | 2005-02-24 | 2007-03-01 | Kear Bernard H | Nanocomposite ceramics and process for making the same |
| CN106687426A (en) * | 2015-04-20 | 2017-05-17 | 住友电气工业株式会社 | Sintered body and cutting tool including same |
| CN106892660A (en) * | 2017-01-16 | 2017-06-27 | 广东百工新材料科技有限公司 | A kind of ceramic mobile phone bonnet and preparation method thereof |
| CN113754431A (en) * | 2021-09-09 | 2021-12-07 | 浙江大学 | Method for preparing nano polycrystalline composite phase zirconia by ultrahigh pressure/high temperature phase change method |
| CN114351026A (en) * | 2022-01-12 | 2022-04-15 | 富耐克超硬材料股份有限公司 | Polycrystalline cubic boron nitride composite material |
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