CN101279840A - Preparation of aluminum oxide-tungsten carbide nanometer composite ceramic material - Google Patents
Preparation of aluminum oxide-tungsten carbide nanometer composite ceramic material Download PDFInfo
- Publication number
- CN101279840A CN101279840A CNA2008100162091A CN200810016209A CN101279840A CN 101279840 A CN101279840 A CN 101279840A CN A2008100162091 A CNA2008100162091 A CN A2008100162091A CN 200810016209 A CN200810016209 A CN 200810016209A CN 101279840 A CN101279840 A CN 101279840A
- Authority
- CN
- China
- Prior art keywords
- nanometer
- ceramic material
- composite ceramic
- aluminum oxide
- micron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention belongs to the material science technique field, in particular relates to a process for preparing an aluminum oxide-tungsten titanium carbide nano-composite ceramic material. The process is characterized in that: nanometer-sized alpha-Al2O3 and micron-sized (W, Ti) C powder are added to a matrix of submicron-sized alpha-Al2O3, MgO and NiO are taken as an inhibitor and a combustion improver, and the nano-composite ceramic material of Al2O3 matrix is prepared through the protection of a high purity N2 atmosphere and the hot pressing and sintering technique for even compression. The introduction of nano-Al2O3 particles can effectively inhibit the growth of micron aluminum oxide particles and thinning the crystal grains, and the material has advantages of even particle size distribution, high hardness, bending strength and fracture toughness, excellent wear resistance and high stability under high temperature. The nano-composite ceramic material is suitable for making metal cutting tools and nozzles with rather high requirements on high temperature and wear resistance.
Description
Technical field
The invention belongs to materials science field, particularly a kind of preparation method of aluminum oxide-tungsten carbide nanometer composite ceramic material.
Background technology
Composite ceramic material has advantages such as high-melting-point, good wear resistance, thermo-chemical stability, high rigidity, is suitable for making the cutter of difficult processing work material.The Ai Xing of Shandong University, Xiao Hong etc. use aluminium hydroxide thermolysis material and tungsten carbide solid-solution powder to be raw material, adopt the quick hot-press method of high temperature to prepare the aluminum oxide-tungsten carbide composite ceramic tool material, the bending strength of this material is that 850MPa, hardness are that HRA94.7-95.3, fracture toughness are 4.94MPam
1/2The semi-finishing and the precision work of difficult-to-machine material have been applied to, but relatively low fracture toughness property has limited its further range of application (Ai Xing, Deng Jianxin. the development of sintex and application. mechanic's (cold working) [J], 2000,9:4-6), the toughness that how further to improve this composite ceramic material is one of emphasis of research.Studies show that, in ceramic material, add bending strength that nano particle can the Effective Raise composite ceramic material and fracture toughness (M.Sternitzke.Review:Structural Ceramic Nanocomposites[J] .J.Eur.Ceram.Soc[J], 1997,17:1061-1082), obviously improve its high-temperature behavior (Li Guanghai, Jiang'an is complete, Zhang Lide. add nanometer Al
2O
3To Al
2O
3The impact of ceramic toughening and enhancing [J]. Acta Metallurgica Sinica, 1996,32 (12): 1285-1288).In addition, in the micron order matrix powder, add an amount of nano level matrix powder, mix with the wild phase powder, can obtain having composite ceramic material (the Z.J.L ü of favorable comprehensive mechanical property behind the sintering, X.Ai and J.Zhao.Preparation of Agglomerate-freeStarting Powders for TiCp-reinforced beta-Sialon Nanocomposites.Materials Science Forum.2004,471-472:282-286).But in the feedstock production process since particle diameter of nanometer powder little, specific surface area is big, chemically reactive is high, be easy to reunion and form larger-size coacervate, the reunion of nano-powder will have a strong impact on density, intensity, toughness, reliability and other performance of sintered compact.The dispersion effect of nano-powder is subjected to influence of various factors, the intensity of granularity, specific surface area, dispersion agent kind, add-on, dispersion medium, solid load, pH value and ultra-sonic dispersion and time etc. are all directly relevant with dispersion effect, need a large amount of contrast experiments with definite optimum dispersion processing parameter.The dispersion of existing nano aluminium oxide adopts polyoxyethylene glycol (PEG), Sodium hexametaphosphate 99 as dispersion agent more, the dispersion effect of PEG is general, though the dispersion effect of Sodium hexametaphosphate 99 is better, can introduce impurity such as sodium ion behind its sintering, for the performance of nanocomposite ceramic material certain influence is arranged.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, a kind of preparation method with aluminum oxide-tungsten carbide nanometer composite ceramic material of high strength, high rigidity, high tenacity and good high-temperature stability is provided.
The present invention realizes in the following manner:
A kind of preparation method of aluminum oxide-tungsten carbide nanometer composite ceramic material, its feature may further comprise the steps:
(1) dispersion of nano particle
With nanometer α-Al
2O
3Slowly add in the deionized water, stir while adding, the configuration volume fraction is 2% suspension, and ultrasonic agitation is even; With polymethylacrylic acid ammonia (PMAA-NH
4) be dispersant, its consumption is the nanometer α that will disperse-Al
2O
31.2% of quality splashes into the nanometer α that mixed-Al with dispersant
2O
3Suspension, adjusting the Ph value is 9.5-10; Ultrasonic agitation is even, obtains the α-Al of good dispersion property
2O
3Suspension;
(2) batch mixing
Percentage nanometer α-Al by volume
2O
3Be 5～54%, submicron alpha-Al
2O
3Be 5～49%, micron (W, a Ti) C is 45%, MgO is 0.5%, NiO 0.5% prepares burden; With submicron alpha-Al
2O
3, the nanometer α for preparing of micron (W, Ti) C and additive MgO and NiO and (1)-Al
2O
3Suspension mixes, and the ultrasonic agitation ball milling bucket of packing into after evenly mixed 48～72 hours at ball mill again, through vacuum drying, sieve the material powder that obtains mixing;
(3) hot pressed sintering
The mixed raw materials powder is packed in the high-strength graphite mould, adopt nitrogen protection, the even hot-pressing sintering technique of pressurization; During in room temperature～1700 ℃, heat-up rate is 75～85 ℃/minute, and pressure steadily adds to 30Mpa equably; Under 1700 ℃, pressure 30MPa condition, be incubated 10 minutes, outage naturally cools to room temperature then.
The preparation method of above-mentioned a kind of aluminum oxide-tungsten carbide nanometer composite ceramic material is characterized in that the time of twice ultrasonic agitation in the step (1) is 20 minutes.
By above step, can make even particle size distribution, hardness height, have the aluminum oxide-tungsten carbide nanometer composite ceramic material of high-flexural strength, fracture toughness property and high temperature resistance.
This preparation method passes through at micron-sized α-Al
2O
3Add nanometer alpha-Al in the matrix
2O
3(W, Ti) C solid-solution powder, and control nanometer α-Al
2O
3The volume fraction of particle take MgO, NiO as inhibitor with sintering agent, adopts N
2Atmosphere protection, the evenly hot pressing and sintering technique of pressurization.Nanometer α-Al
2O
3The introducing of particle has suppressed growing up of micrometer alumina particle effectively, refinement crystal grain; Nanometer (W, Ti) C particle and matrix α-Al in the raw material
2O
3Formed typical intracrystalline type/intergranular type structure; Al
2O
3Matrix is tight with the combination of (W, Ti) C wild phase interface, interts mutually and parcel, has formed typical skeleton structure.This composite ceramic material have granularity tiny and be evenly distributed, characteristics such as high rigidity, high-flexural strength, high-fracture toughness, good high-temperature stability.This nanocomposite ceramic material is suitable for making metal cutting tool that high temperature and wear resistance have relatively high expectations, nozzle etc.
Embodiment
Provide most preferred embodiment of the present invention below.
Embodiment 1
Submicron alpha-Al
2O
3(0.5 μ m)+nanometer α-Al
2O
3(80nm)+and micron (W, Ti) C (1 μ m), the content of each component (percent by volume) is in the nano composite material: 43% submicron alpha-Al
2O
3, 11% nanometer α-Al
2O
3, 45% micron (W, Ti) C, 0.5%MgO, 0.5%NiO.With the nanometer α after weighing-Al
2O
3Slowly add in the deionized water, stir while adding, the configuration volume fraction is 2% suspension, ultrasonic agitation 20 minutes; With polymethylacrylic acid ammonia (PMAA-NH
4) be dispersant, its consumption is the nanometer α that will disperse-Al
2O
31.2% of quality splashes into dispersant the α-Al that has mixed
2O
3The aqueous solution, adjusting the Ph value is 9.5-10; Ultrasonic agitation 20 minutes obtains the suspension of good dispersion property.α-Al with sub-micron
2O
3, micron (W, the Ti) C behind the ball milling and additive MgO and NiO and the nanometer α that prepared-Al
2O
3Suspension mixes, and ultrasonic agitation was mixed 72 hours at planetary ball mill after 30 minutes, passes through vacuum drying again, sieves, and obtains finely disseminated composite powder material.Adopt the high-purity nitrogen gas shiled, evenly the hot-pressing sintering technique of pressurization; During in room temperature～1700 ℃, heat-up rate is 75 ℃/minute, and pressure steadily adds to 30MPa equably, is incubated 10 minutes, and the holding stage temperature is 1700 ℃, and pressure 30MPa naturally cools to room temperature after the outage.
The mechanical property of material is: hardness HV19～21GPa, and bending strength 820～840MPa, fracture toughness property is 6～6.89MPa.m
1/2
Embodiment 2
Submicron alpha-Al
2O
3(0.5 μ m)+nanometer α-Al
2O
3(80nm)+and micron (W, Ti) C (1 μ m), the content of each component (percent by volume) is in the nano composite material: 36% submicron alpha-Al
2O
3, 18% nanometer α-Al
2O
3, 45% micron (W, Ti) C, 0.5%MgO, 0.5%NiO.With the nanometer α after weighing-Al
2O
3Slowly add in the deionized water, stir while adding, the configuration volume fraction is 2% suspension, ultrasonic agitation 20 minutes; With polymethylacrylic acid ammonia (PMAA-NH
4) be dispersant, its consumption is the nanometer α that will disperse-Al
2O
31.2% of quality splashes into dispersant the α-Al that has mixed
2O
3The aqueous solution, adjusting the Ph value is 9.5-10; Ultrasonic agitation 20 minutes obtains the suspension of good dispersion property.With sub-micron and α-Al
2O
3, micron (W, the Ti) C behind the ball milling and additive MgO and NiO and the nanometer α that prepared-Al
2O
3Suspension mixes, and ultrasonic agitation was mixed 72 hours at planetary ball mill after 30 minutes, passes through vacuum drying again, sieves, and obtains finely disseminated composite powder material.Adopt the high-purity nitrogen gas shiled, evenly the hot-pressing sintering technique of pressurization; During in room temperature～1700 ℃, heat-up rate is 85 ℃/minute, and pressure steadily adds to 30MPa equably, is incubated 10 minutes, and the holding stage temperature is 1700 ℃, and pressure 30MPa naturally cools to room temperature after the outage.
The mechanical property of material is: hardness HV17～19GPa, and bending strength 790～810MPa, fracture toughness property is 6.5～7.15MPa.m
1/2
Embodiment 3
Submicron alpha-Al
2O
3(0.5 μ m)+nanometer α-Al
2O
3(30nm)+and micron (W, Ti) C (1 μ m), the content of each component (percent by volume) is in the nano composite material: 27% submicron alpha-Al
2O
3, 27% nanometer α-Al
2O
3, 45% micron (W, Ti) C, 0.5%MgO, 0.5%NiO.With the nanometer α after weighing-Al
2O
3Slowly add in the deionized water, stir while adding, the configuration volume fraction is 2% suspension, ultrasonic agitation 20 minutes; With polymethylacrylic acid ammonia (PMAA-NH
4) be dispersant, its consumption is the nanometer α that will disperse-Al
2O
31.2% of quality splashes into dispersant the α-Al that has mixed
2O
3The aqueous solution, adjusting the Ph value is 9.5-10; Ultrasonic agitation 20 minutes obtains the suspension of good dispersion property.With sub-micron and α-Al
2O
3, micron (W, the Ti) C behind the ball milling and additive MgO and NiO and the nanometer α that prepared-Al
2O
3Suspension mixes, and ultrasonic agitation was mixed 48 hours at planetary ball mill after 30 minutes, passes through vacuum drying again, sieves, and obtains finely disseminated composite powder material.Adopt the high-purity nitrogen gas shiled, evenly the hot-pressing sintering technique of pressurization; During in room temperature～1700 ℃, heat-up rate is 85 ℃/minute, and pressure steadily adds to 30MPa equably, is incubated 10 minutes, and the holding stage temperature is 1700 ℃, and pressure 30MPa naturally cools to room temperature after the outage.
The mechanical property of material is: hardness HV17～18GPa, and bending strength 765～800MPa, fracture toughness property is 6～6.72MPa.m
1/2
Claims (2)
1. the preparation method of an aluminum oxide-tungsten carbide nanometer composite ceramic material, its feature may further comprise the steps:
(1) dispersion of nano particle
With nanometer α-Al
2O
3Slowly add in the deionized water, stir while adding, the configuration volume fraction is 2% suspension, and ultrasonic agitation is even; With polymethylacrylic acid ammonia (PMAA-NH
4) be dispersant, its consumption is the nanometer α that will disperse-Al
2O
31.2% of quality splashes into the nanometer α that mixed-Al with dispersant
2O
3Suspension, adjusting the Ph value is 9.5-10; Ultrasonic agitation is even, obtains the α-Al of good dispersion property
2O
3Suspension;
(2) batch mixing
Percentage nanometer α-Al by volume
2O
3Be 5～54%, submicron alpha-Al
2O
3Be 5～49%, micron (W, a Ti) C is 45%, MgO is 0.5%, NiO 0.5% prepares burden; With submicron alpha-Al
2O
3, the nanometer α for preparing of micron (W, Ti) C and additive MgO and NiO and (1)-Al
2O
3Suspension mixes, and the ultrasonic agitation ball milling bucket of packing into after evenly mixed 48～72 hours at ball mill again, through vacuum drying, sieve the material powder that obtains mixing;
(3) hot pressed sintering
The mixed raw materials powder is packed in the high-strength graphite mould, adopt nitrogen protection, the even hot-pressing sintering technique of pressurization; During in room temperature～1700 ℃, heat-up rate is 75～85 ℃/minute, and pressure steadily adds to 30Mpa equably; Under 1700 ℃, pressure 30MPa condition, be incubated 10 minutes, outage naturally cools to room temperature then.
2. the preparation method of a kind of aluminum oxide-tungsten carbide nanometer composite ceramic material according to claim 1 is characterized in that the time of twice ultrasonic agitation in the step (1) is 20 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100162091A CN101279840A (en) | 2008-05-13 | 2008-05-13 | Preparation of aluminum oxide-tungsten carbide nanometer composite ceramic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100162091A CN101279840A (en) | 2008-05-13 | 2008-05-13 | Preparation of aluminum oxide-tungsten carbide nanometer composite ceramic material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101279840A true CN101279840A (en) | 2008-10-08 |
Family
ID=40012540
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100162091A Pending CN101279840A (en) | 2008-05-13 | 2008-05-13 | Preparation of aluminum oxide-tungsten carbide nanometer composite ceramic material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101279840A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913876A (en) * | 2010-07-01 | 2010-12-15 | 山东大学 | Method for preparing zirconium boride-tungsten titanium carbide self-lubricating composite ceramic material |
| CN101486578B (en) * | 2009-02-27 | 2011-08-17 | 山东大学 | Silicon nitride based nano complex gradient function ceramic tool material and preparation thereof |
| CN101654366B (en) * | 2009-09-10 | 2012-10-24 | 中国矿业大学(北京) | Composite sintering agent and method for preparing nano crystalline ceramics at low temperature |
| CN102815929A (en) * | 2012-09-10 | 2012-12-12 | 山东轻工业学院 | Multivariate gradient self-lubricating ceramic cutting tool material with surface having residual compressive stress and preparation method of multivariate gradient self-lubricating ceramic cutting tool material |
| CN103360074A (en) * | 2013-07-11 | 2013-10-23 | 东华大学 | Preparation method for WC-Al2O3 nanometer composite material |
| CN106316398A (en) * | 2016-08-17 | 2017-01-11 | 齐鲁工业大学 | Tungsten titanium carbide-based ceramic tool material added with cubic boron nitride and preparation method of material |
| CN108424161A (en) * | 2018-04-13 | 2018-08-21 | 山东大学 | A kind of preparation method of the diphase ceramic material of graphene Strengthening and Toughening |
| CN111087247A (en) * | 2020-01-03 | 2020-05-01 | 神华新能源有限责任公司 | Method for inhibiting grain growth of ceramic material and application thereof |
| CN112760544A (en) * | 2020-12-25 | 2021-05-07 | 湖南天益高技术材料制造有限公司 | Formula and preparation process of high-temperature-resistant vapor chamber for 3D glass hot bending machine |
-
2008
- 2008-05-13 CN CNA2008100162091A patent/CN101279840A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486578B (en) * | 2009-02-27 | 2011-08-17 | 山东大学 | Silicon nitride based nano complex gradient function ceramic tool material and preparation thereof |
| CN101654366B (en) * | 2009-09-10 | 2012-10-24 | 中国矿业大学(北京) | Composite sintering agent and method for preparing nano crystalline ceramics at low temperature |
| CN101913876A (en) * | 2010-07-01 | 2010-12-15 | 山东大学 | Method for preparing zirconium boride-tungsten titanium carbide self-lubricating composite ceramic material |
| CN101913876B (en) * | 2010-07-01 | 2012-10-31 | 山东大学 | Method for preparing zirconium boride-tungsten titanium carbide self-lubricating composite ceramic material |
| CN102815929A (en) * | 2012-09-10 | 2012-12-12 | 山东轻工业学院 | Multivariate gradient self-lubricating ceramic cutting tool material with surface having residual compressive stress and preparation method of multivariate gradient self-lubricating ceramic cutting tool material |
| CN102815929B (en) * | 2012-09-10 | 2014-02-26 | 山东轻工业学院 | Multivariate gradient self-lubricating ceramic cutting tool material with surface having residual compressive stress and preparation method of multivariate gradient self-lubricating ceramic cutting tool material |
| CN103360074A (en) * | 2013-07-11 | 2013-10-23 | 东华大学 | Preparation method for WC-Al2O3 nanometer composite material |
| CN106316398A (en) * | 2016-08-17 | 2017-01-11 | 齐鲁工业大学 | Tungsten titanium carbide-based ceramic tool material added with cubic boron nitride and preparation method of material |
| CN108424161A (en) * | 2018-04-13 | 2018-08-21 | 山东大学 | A kind of preparation method of the diphase ceramic material of graphene Strengthening and Toughening |
| CN111087247A (en) * | 2020-01-03 | 2020-05-01 | 神华新能源有限责任公司 | Method for inhibiting grain growth of ceramic material and application thereof |
| CN112760544A (en) * | 2020-12-25 | 2021-05-07 | 湖南天益高技术材料制造有限公司 | Formula and preparation process of high-temperature-resistant vapor chamber for 3D glass hot bending machine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101279840A (en) | Preparation of aluminum oxide-tungsten carbide nanometer composite ceramic material | |
| CN107475548B (en) | A kind of preparation method of nanometer of toughening superfine WC-Co cemented carbide | |
| CN104313380B (en) | A kind of step sintering prepares the method for high-compactness Nanograin Cemented Carbide | |
| CN102211925B (en) | Method for preparing micro and nano composite ceramic material | |
| CN102390998B (en) | Tungsten carbide composite material containing aluminum oxide particles and silicon nitride whiskers, and preparation method thereof | |
| CN110042280B (en) | In-situ endogenous multiphase particle reinforced aluminum matrix composite material and preparation method thereof | |
| CN109943739B (en) | Method for preparing ultrafine-grained WC-Co hard alloy by plasma ball milling | |
| CN101857438A (en) | Method for preparing aluminum oxide-titanium carbide-zirconium oxide nanocomposite ceramic material | |
| CN103739292A (en) | Method for preparing silicon nitride-tungsten carbide titanium nano-composite ceramic cutting tool material | |
| CN104876598A (en) | Max phase-boron nitride composite ceramic side seal plate for thin-strip casting and manufacturing method of Max phase-boron nitride composite ceramic side seal plate | |
| CN104446396A (en) | Preparation method of micro-nano composite aluminum oxide-titanium nitride-zirconium oxide-nickel-molybdenum ceramic material | |
| CN104911381A (en) | Ti2AlC/TiAl-based composite and preparation method thereof | |
| CN110257681A (en) | A kind of polycrystalline cubic boron nitride compound sheets and preparation method thereof | |
| CN113699406A (en) | High-strength and high-toughness extra-coarse-grain WC hard alloy with average grain size larger than 8 microns and preparation method thereof | |
| CN103938023B (en) | A kind of in-situ autogenic titanium aluminium carbon highly malleablized TiAl 3intermetallic compound and preparation method thereof | |
| CN100347124C (en) | Preparation process of conducting aluminium oxide base nano ceramic material | |
| Ni et al. | Effects of metal binder on the microstructure and mechanical properties of Al 2 O 3-based micro-nanocomposite ceramic tool material | |
| CN102021473A (en) | Method for preparing Fe3Al-Al2O3 composite material | |
| CN107267836A (en) | A kind of twin crystal hard alloy and preparation method thereof | |
| CN107043260A (en) | A kind of novel tertiary osmium rhenium diboride (Os1 xRexB2) hard material and preparation method thereof | |
| EP2146943A2 (en) | Boron suboxide composite materials | |
| CN106316398A (en) | Tungsten titanium carbide-based ceramic tool material added with cubic boron nitride and preparation method of material | |
| CN107299238B (en) | A kind of preparation method of Ti nano-particle reinforcement TiC-Ni system cermet | |
| CN107287464A (en) | A kind of composite porous preparation method of titanium-based of the ceramics containing nano TiN | |
| Wang et al. | Effects of nano-ZrO2 on the microstructure and mechanical properties of Ti (C, N)-based cermet die materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20081008 |