CN115745602B - 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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- CN115745602B CN115745602B CN202211590373.XA CN202211590373A CN115745602B CN 115745602 B CN115745602 B CN 115745602B CN 202211590373 A CN202211590373 A CN 202211590373A CN 115745602 B CN115745602 B CN 115745602B
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 239000000919 ceramic Substances 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000011812 mixed powder Substances 0.000 claims abstract description 14
- 239000011159 matrix material Substances 0.000 claims abstract description 12
- 239000011858 nanopowder Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000713 high-energy ball milling Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000002245 particle Substances 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 12
- 229910052582 BN Inorganic materials 0.000 abstract description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 abstract description 8
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000002490 spark plasma sintering Methods 0.000 abstract description 2
- 238000005728 strengthening Methods 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- 230000002159 abnormal effect 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
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 229940057995 liquid paraffin Drugs 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000012173 sealing wax Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- 238000005303 weighing Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 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) (1.5-10) calculated by 100 parts by mass. The method ensures that the prepared zirconia-based ceramic composite material realizes that a small amount of nano cubic boron nitride is added into a zirconia matrix material to achieve the purpose of hard particle dispersion strengthening, thereby improving the hardness and toughness of zirconia ceramics. Meanwhile, in the spark plasma sintering process, CBN particles and zirconia powder undergo interface reaction to generate ZrN and ZrB 2 The bonding force of the grain boundary is increased, the grain boundary is strengthened, and the compactness 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 with metal, difficult adhesion with metal and good chemical stability, so that the ceramic cutter material has very wide application in industries such as machinery, electronics, petroleum, chemical industry, precision instruments, medical instruments, bioengineering and the like. Zirconia ceramic materials have been made into ceramic cutters, artificial teeth, ball milling media, wear resistant components, medical cutter materials, and the like. Besides the advantages, the zirconia ceramic material has the characteristics of no magnetism, no static electricity, long service life, high precision, good biocompatibility and the like. Therefore, the zirconia ceramics have unique physical properties and good mechanical properties, so that the zirconia ceramics have important research significance in the fields of functional ceramics and structural ceramics.
The chemical bonds of zirconia ceramics are mainly ionic bonds, unlike the metal bonds in metallic materials. The zirconia material is subjected to a large impact force, and the dislocation is difficult to slip due to high strength of ionic bonds and difficult bond breaking, and the ionic bonds are difficult to recombine after being broken; this results in the intrinsic brittleness of the zirconia ceramic. Therefore, the zirconia ceramic material often has the characteristics of high brittleness and poor toughness, so that the zirconia ceramic material is difficult to deform in a molding way, and the application of the zirconia ceramic material in the aspect of structural ceramic members is severely limited. Meanwhile, the zirconia ceramic material has a crystal structure different from that of a metal material, and once micro cracks are initiated 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 parts and medical cutter materials is also influenced.
Disclosure of Invention
In view of the foregoing, it is desirable to provide a zirconia-based ceramic composite material, and a preparation method and application thereof, so as to solve the above-mentioned 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) (1.5-10) calculated by 100 parts by mass.
Based on the preparation method, the granularity of the zirconia powder is 1-5 mu m, and the zirconia powder with the granularity has small granularity, narrow distribution, good appearance, uniform distribution, uniform sintered ceramic microstructure and relatively good strength and toughness. The granularity of the CBN nano powder is less than or equal to 50 and nm, so that the CBN with the nano size has small size effect and disorder of interfaces, the brittleness of zirconia ceramic is reduced, and the smoothness of the surface of a cutter is improved.
Based on the preparation method, the step method for obtaining the mixed powder comprises the following steps: and carrying out high-energy ball milling treatment on the zirconia powder and the CBN nano powder to obtain the mixed powder which is uniformly mixed. Other conventional mixing methods can be adopted in the step, and only the zirconia powder and the CBN nano powder are uniformly mixed.
Based on the preparation method, the step of the plasma sintering treatment comprises the following steps: pre-pressing the mixed powder, and then sintering by 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 aim of the pre-pressing treatment in the step is to pre-form and improve the density of the powder, which is beneficial to the improvement of the forming and the density of the sintered body. In addition, the surface of the powder particles can be purified and activated by electric shock waves and electrons generated by discharge 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 non-contacted parts, 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 the sintered body with uniform microstructure, excellent mechanical property and high compactness 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 surface 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 density of the zirconia-based ceramic composite material is more 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 treating the mixed powder of the zirconia powder and the CBN nano powder through plasma sintering, so that the prepared zirconia-based ceramic composite material realizes the purpose of adding a small amount of nano cubic boron nitride into the zirconia matrix material to achieve hard particle dispersion strengthening, the abnormal growth of zirconia grains can be inhibited in the process of sintering the nano particle reinforced phase, the zirconia matrix material is refined in structure, the smaller the grains are, the denser the microstructure is, and the strength of the zirconia-based ceramic composite material is higher, because the smaller the grain size of the zirconia isThe microstructure is relatively denser, and defects such as air holes in the composite material are reduced, so that the hardness and toughness of the zirconia ceramic are improved. Meanwhile, in the spark plasma sintering process, CBN particles and zirconia powder undergo interface reaction to generate ZrN and ZrB 2 The bonding force of the grain boundary is further increased, the grain boundary is strengthened, and the compactness and the strength of the material are improved.
Experiments prove that the density of the zirconia-based ceramic composite material provided by the invention is more than or equal to 95%, 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 wear-resistant cutter, a wear-resistant part and a medical cutter material, so that the cutter is not easy to crack in the processing process, the safety and wear resistance of cutter 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 material according to an embodiment of the present invention.
Fig. 2 to 6 are SEM photographs of the zirconia-based ceramic composites provided in examples 1 to 5 of the present invention.
Wherein, the reference numerals in the above figures: 1. a zirconia matrix; 2. cubic boron nitride particles; 3. ZrN and ZrB 2 And (3) particles.
Detailed Description
The technical scheme of the invention is further described in detail through the following specific embodiments.
Examples 1 to 5
The present embodiments 1 to 5 provide a method for preparing a zirconia-based ceramic composite material, comprising the steps of:
zirconium oxide ZrO 2 The powder and the nano cubic boron nitride powder are subjected to high-energy ball milling and uniform mixing according to the mass ratio shown in the table 1, and mixed powder is obtained; the mixed powder is placed in a tool steel die, prepressed by a press and is pre-pressed into a material rod, and then the material rod is sintered by spark plasma with sintering parameters shown in table 1 to obtain the powder shown in figures 1-6ZrO of (2) 2 A base ceramic composite. 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 Particles 3.
Table 1 process parameters relating to the preparation method
Comparative examples 1 to 3
Comparative examples 1 to 3 each provide a 3Y-ZrO 2 The preparation method of the ceramic composite material is basically the same as that provided in the examples, and is mainly different in that: comparative examples 1 to 3 were each based on zirconia ZrO 2 And yttrium oxide Y 2 O 3 The raw materials were the same as examples 1 to 3, respectively.
Performance testing
The hardness, toughness and density of the ceramic composites 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 toughness are measured by adopting the current industry standard; the method of measuring the density is as follows.
The density measuring method comprises the following steps: based on archimedes' drainage principle, the dry weight m of the sample at room temperature is weighed by placing on an analytical balance 1 The sample is put into the melted paraffin to ensure that the sample is totally free of the liquid paraffin; taking out the sample, placing on a weighing paper, scraping off superfluous paraffin on the surface of the sample, cooling to room temperature, and measuring the sealing wax weight m on an analytical balance 2 The float weight m of the wax sealing sample in the water medium is weighed 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. Wherein:
ρ=m 1 ρ water and its preparation method /(m 2 -m 3 )
W=ρ/ρ 0 ×100%
ρ Water and its preparation method Representing the density of water at room temperature, taking 20 DEG CDensity value ρ of time water Water and its preparation method =0.998203g/cm 3 ；ρ 0 Represents the theoretical density of the zirconia-based bulk material.
TABLE 2 ZrO 2 Performance parameter table for base ceramic composite material
Application of
The zirconia-based ceramic composite materials provided in examples 2 to 4 and comparative examples 2 to 3 were manufactured into a standard tool CNMN120716S05020 cutting tool on the market by the company, and then abrasion ratio detection was performed according to the national current industry standard (JB 3235-83) specification, wherein abrasion ratio measurement was performed on a JS71-a type abrasion ratio meter with a standard grinding wheel TL80#z2ap100×16×20, the grinding wheel linear speed was 25 m/S, the grinding wheel abrasion amount was not less than 25 g, and the sample abrasion amount was not less than 0.2 mg.
Table 3 results of wear ratio test of cutting tool
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same; while the invention has been described in detail with reference to the preferred embodiments, those skilled in the art will appreciate that: modifications may be made to the specific embodiments of the present invention or equivalents may be substituted for part of the technical features thereof; without departing from the spirit of the invention, it is intended to cover the scope of the invention as claimed.
Claims (6)
1. A preparation method of a zirconia-based ceramic composite material comprises the following steps: uniformly mixing zirconia powder with the granularity of 1-5 mu m and CBN nano powder with the granularity of less than or equal to 50 nm to obtain mixed powder, and then carrying out plasma sintering treatment on the mixed powder to obtain the zirconia-based ceramic composite material, wherein the mass ratio of the zirconia powder to the CBN nano powder is (90-98.5) (1.5-10) calculated by 100 parts by mass;
the step of the plasma sintering treatment comprises the following steps: pre-pressing the mixed powder, and then sintering by 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 zirconia-based ceramic composite material comprises a zirconia matrix, CBN uniformly dispersed in the zirconia matrix, and ZrN and ZrB coated on the surface of the CBN 2 。
2. The method of manufacturing according to claim 1, characterized in that: the step of obtaining the mixed powder comprises the step of performing high-energy ball milling treatment on the zirconia powder and the CBN nano powder.
3. A zirconia-based ceramic composite material produced by the production method according to any one of claims 1 to 2.
4. A ceramic composite according to claim 3, wherein: the zirconia matrix accounts for 90-98.5% of the zirconia-based ceramic composite material by mass percent.
5. The ceramic composite of claim 4, wherein: the density of the zirconia-based ceramic composite material is more than or equal to 95 percent.
6. Use of the zirconia-based ceramic composite material of claim 3 or 4 or 5 in wear resistant cutters, wear resistant parts or medical cutter materials.
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Citations (5)
| 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006091613A2 (en) * | 2005-02-24 | 2006-08-31 | Rutgers, The State University Of New Jersey | Nanocomposite ceramics and process for making the same |
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- 2022-12-12 CN CN202211590373.XA patent/CN115745602B/en active Active
Patent Citations (5)
| 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 |
| 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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