CN101905975A - Preparation method of high wear-resistant eutectic ceramic - Google Patents
Preparation method of high wear-resistant eutectic ceramic Download PDFInfo
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- CN101905975A CN101905975A CN 201010215806 CN201010215806A CN101905975A CN 101905975 A CN101905975 A CN 101905975A CN 201010215806 CN201010215806 CN 201010215806 CN 201010215806 A CN201010215806 A CN 201010215806A CN 101905975 A CN101905975 A CN 101905975A
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- 230000005496 eutectics Effects 0.000 title claims abstract description 46
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000002791 soaking Methods 0.000 claims description 5
- 230000004927 fusion Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 14
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 229910016341 Al2O3 ZrO2 Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 9
- 238000007731 hot pressing Methods 0.000 description 7
- 239000008187 granular material Substances 0.000 description 6
- 230000002269 spontaneous effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000001272 pressureless sintering Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000010309 melting process Methods 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 2
- 239000011218 binary composite Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000009617 vacuum fusion Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002114 nanocomposite Substances 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
- 230000005501 phase interface Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 230000003245 working effect Effects 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 high wear-resistant eutectic ceramic, belonging to the technical field of new material preparation, wherein the eutectic ceramic comprises Al2O3-ZrO2(3Y). The preparation method of the eutectic ceramic comprises the following steps: firstly acquiring a ceramic sintered body with a certain shape as a blank for preparing the eutectic ceramic, and finally obtaining the high wear-resistant eutectic ceramic by a high-temperature melting method under the condition of vacuum. In the method, mol content of Al2O3 in the eutectic ceramic is 40%-49%, mol content of ZrO2(3Y) is 51%-60%, and average particle size of the original powder is less than 100 nanometers; and sintering temperature of the eutectic ceramic is 1400-1550 DEG C, melting temperature is 1850-1950 DEG C, and melting holding time is 30-60min. The effect and benefit of the invention is that the preparation method of the eutectic ceramic is simple. The preparation method of the invention has the advantages of low price of main equipment, easy implementation, simplicity and capability of producing large-sized materials; and the obtained eutectic ceramic has high-temperature resistance and high wear resistance.
Description
Technical field
The invention belongs to technical field of new material preparation, relate to a kind of preparation method of high wear-resistant eutectic ceramic.
Background technology
Along with science and technology development, some high-end devices are had higher requirement to the wear resistance of material, especially under severe environment, as the wear resistance of material under the environment such as high temperature, deep-etching, as the nozzle of aircraft engine, larynx lining, dividing plate, combustion chamber etc.The two component eutectic pottery has high rigidity, high-wearing feature, resistant to elevated temperatures characteristic, not only can satisfy the requirement of material mechanical performance aspect preferably, and its weave construction is stable under high temperature, strong corrosive environment, can be under high temperature, strong acid and strong base environment long service.
The two component eutectic pottery is a kind of synthetic material of excellent property, pass through melt growth owing to have the material of eutectic composition, become vermiform or fibrous three-dimensional network eutectic structure, so the spontaneous pottery of eutectic not only has following excellent characteristic: hang down voidage, interface in conjunction with good, and at high temperature show a kind of very excellent mechanical property.The spontaneous pottery of eutectic still has high tissue and stability near fusing point, have high-wearing feature, high rigidity, high specific strength, high creep resistance, high toughness and excellent oxidation-resistance and erosion resistance under room temperature and high temperature.The spontaneous pottery of two component eutectic can also have the wear resistance of superelevation having under the condition of excellent comprehensive mechanical properties.If under severe environment, use,, improve the market competitiveness because its stable chemical property reduces production costs the work-ing life that can improve high-abrasive material as high-abrasive material.
The method for preparing the spontaneous pottery of two component eutectic in the prior art has two kinds, and a kind of is to adopt conventional directional solidification method after the material melts; Another kind is to adopt laser beam or the molten directional freeze of area electron beam.Above-mentioned two kinds of methods all need special apparatus for directional solidification and electron-beam melting system or laser apparatus etc., all exist production efficiency low, to the equipment requirements height, be difficult to prepare the shortcomings such as material of large-size.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high abrasion two component eutectic pottery.The present invention adopts the binary composite granule with eutectic composition to prepare eutectic ceramic, and hot pressing and sintering technique is combined with the high-temperature vacuum fusion technology prepares eutectic ceramic, makes to have specified shape and larger-size high wear-resistant eutectic ceramic material.
The present invention realizes that the technical scheme that aforesaid method is taked is: with Al
2O
3And ZrO
2(3Y) two kinds of powders mix by the eutectic composition of specified proportion.Under 1400～1550 ℃ temperature, carry out hot pressed sintering, obtain the ceramic sintered bodies of specified shape (as cylindrical or plate-shaped); Perhaps with mixed composite granule at room temperature isostatic cool pressing become specified shape, pressureless sintering obtains ceramic sintered bodies under 1400～1550 ℃ temperature afterwards.Subsequently, the sintered compact that obtains is put into the melt temperature of 1850～1950 ℃ of graphite jig inherences and carried out vacuum melting, afterwards, at room temperature take out stupalith behind the furnace cooling, promptly obtain having the two component eutectic pottery of high-wearing feature.
The aforesaid method that the present invention prepares high wear-resistant eutectic ceramic is summarised as: powder preparing, processing---sintering, adopt vacuum heating-press sintering or cold isostatic compaction+pressureless sintering---fusion, and the fusion of employing high-temperature vacuum---stove is cold.
The main component that is used to prepare the two component eutectic pottery of high abrasion in the inventive method is: Al
2O
3+ ZrO
2(3Y), 3Y represents to adopt 3%Y
2O
3Stable ZrO
2Al wherein
2O
3Molar content be 40%～49%, ZrO
2Molar content (3Y) is 60%～51%.Its composition proportion realizes by three kinds of powders of initial weighing.
Two kinds of powders of the preceding original adoption of sintering are in the inventive method: Al
2O
3And ZrO
2(3Y).Two kinds of powders all should guarantee good dispersion, hard aggregation-free, and the median size of each powder is all less than 100 nanometers.
The hot pressed sintering temperature that adopts vacuum heating-press sintering to prepare sintered compact in the inventive method is 1400～1550 ℃, and the soaking time of hot pressed sintering is 30～45min, and hot pressing pressure is 〉=25MPa.If adopt isostatic cool pressing+pressureless sintering method to prepare sintered compact, then the pressure of isostatic cool pressing should be 〉=200MPa, and the dwell time is 〉=5min; The temperature of pressureless sintering subsequently is 1400～1550 ℃, the insulation 30～90min, in vacuum oven sintering or in antivacuum equipment sintering.
The temperature of vacuum fusion is 1850～1950 ℃ in the inventive method, and to guarantee that blank becomes molten state fully, the soaking time of vacuum melting is generally 30～60min, and liquid composition is fully spread, and avoids pore and cavity occurring in sample inside.The moulding stock that is adopted in the melting process should be resistant to elevated temperatures structured material, can be high-strength graphite or silicon carbide.
The present invention utilizes the microtexture of the uniqueness that the spontaneous pottery of two component eutectic has itself, and its eutectic structure is the three-dimensional net structure of a kind of aluminum oxide and zirconium oxide single crystal IPN.It at high temperature has favorable tissue and stability.And because each phase interface is in conjunction with good, pore-free and being mingled with at the interface, therefore, the spontaneous pottery of two component eutectic has high-wearing feature.
Effect of the present invention and benefit are:
Under this composition, aluminum oxide and zirconium white have formed eutectic, the staggered growth mutually of monocrystalline eutectic in melting process, and this has just determined eutectic ceramic, and high-temperature stability is good, good corrosion resistance except having, and also has high-wearing feature, high-intensity characteristic.Present method adopts sintering+high-temperature vacuum fused preparation technology, does not need expensive apparatus for directional solidification and laser apparatus and electron beam equipment, only needs a vacuum heating-press sintering stove to get final product.The shape of final in the method material or product is guaranteed by the shape of mould, is suitable for producing in batches the material of regular shape, as thin plate, bar-shaped, taper, tubulose etc.; And, just can obtain the specified shape material of large-size as long as the internal space of equipment and mold is enough big.
Description of drawings
Accompanying drawing is the present invention's melt-shaping mould structure synoptic diagram when preparing the regular shape eutectic ceramic.
Among the figure: 1 pressure head, 2 sleeves, 3 cushion blocks, 4 overcoats, 5 ceramic batchs.
Embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme and accompanying drawing.
Material described in the embodiment of the invention is the two component eutectic complex phase ceramic, and starting material are Al
2O
3Aluminum oxide and ZrO
2(3Y) Zirconium powder, the median size of each powder are all less than 100 nanometers.At first with Al
2O
3And ZrO
2(3Y) two kinds of initial nano-powder uniform mixing by sintering process, obtain fine and close columned sinter blank.The blank that sintering is obtained is put into mould then, again mould is put into vacuum hotpressing stove, is heated to 1850～1950 ℃, is incubated 30 minutes, applies less power in insulating process, makes the easier eliminating of molten mass gas inside.Sintering process required for the present invention and melting process all can be realized in common vacuum hotpressing stove.
Embodiment 1:
Present embodiment provides a kind of preparation method of high wear-resistant eutectic ceramic.Adopt commercially available Al
2O
3And ZrO
2(3Y) nano-powder, the median size of each powder are all less than 100 nanometers.It is Al that its proportioning satisfies the sintered compact composition that obtains behind the sintering
2O
3: ZrO
2(3Y)=40: 60, proportioning is a mol ratio; Two kinds of powders are mixed in proportion, obtain the binary composite granule.In ZRY-100 type vacuum heating-press sintering stove the gained composite granule is carried out vacuum heating-press sintering, sintering process adopts high-strength graphite as moulding stock, and sintering temperature is 1500 ℃, and sintering pressure is 30MPa, and the hot pressing soaking time is 30min.Promptly obtain a columniform nano heterogeneous ceramic sintered compact, as next step ceramic batch 5.
The melt-shaping technological process that present embodiment provides is: sintered compact ceramic batch 5 is put into sleeve 2, assemble entire die as shown in drawings.Subsequently, entire die is put into the vacuum heating-press sintering stove, is warming up to 1860 ℃, insulation 60min so that liquid phase fully spreads, during pressure head 1 pressurization and pressurize 10MPa, avoid in molten mass, occurring cavity and pore.Subsequently, close heating power supply, after hot pressing furnace is cooled to room temperature with stove, take out the high abrasion ceramic objects after being shaped.Adopt this mould can prepare the high wear-resistant eutectic ceramic of regular shape.
Embodiment 2:
Present embodiment provides a kind of method for preparing the two component eutectic complex phase ceramic.Adopt commercially available Al
2O
3And ZrO
2(3Y) nano-powder, the median size of each powder are all less than 100 nanometers, and the sintered compact composition that its proportioning satisfies behind the sintering is Al
2O
3: ZrO
2(3Y)=49: 51, proportioning is a mol ratio.Two kinds of powders are mixed in proportion, and back drying, grinding obtain the bielement nano composite granule.In cold isostatic press the gained composite granule is carried out isostatic cool pressing and handle, the pressure that waits static pressure to handle is 200MPa, and the dwell time is 5min; Pressureless sintering in chamber type electric resistance furnace subsequently, sintering temperature are 1550 ℃, soaking time 60min.Promptly obtain a thickness and be 3 millimeters, diameter and be 30 millimeters sheet complex phase ceramic sintered compact, as the blank of preparation fused ceramic.
The preparation process that present embodiment provides is: sintered compact ceramic batch 5 is put into fusion mould sleeve 2.Assemble entire die as shown in drawings.Subsequently, entire die is put into the vacuum heating-press sintering stove, subsequently, entire die is put into the vacuum heating-press sintering stove, be warming up to 1900 ℃, insulation 30min.Pressure head 1 is descending during this time, pressurization 5MPa, pressurize 30min.Subsequently, the hot pressing furnace cooling is cooled to room temperature, takes out the ceramic objects after being shaped.Mould can be designed to other shapes as required, adopts the part with definite shape that this smelting process can make to be needed.
Claims (1)
1. the preparation method of a high wear-resistant eutectic ceramic, the preparation process of described method be at first obtaining ceramic sintered bodies, fusion at high temperature then, and back furnace cooling obtains high wear-resistant eutectic ceramic, it is characterized in that:
A. described eutectic ceramic is to adopt the fused method preparation again of first sintering;
B. Al in the described eutectic ceramic material
2O
3Molar content be 40%～49%, ZrO
2Molar content (3Y) is 51%～60%; The median size of described two kinds of original powders is all less than 100 nanometers;
C. the sintering temperature of described eutectic ceramic is 1400～1550 ℃;
D. the melt temperature of described eutectic ceramic is 1850～1950 ℃, and the fusion soaking time is 30～60min.
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|---|---|---|---|
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| Publication Number | Publication Date |
|---|---|
| CN101905975A true CN101905975A (en) | 2010-12-08 |
Family
ID=43261590
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|---|---|---|---|
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503380A (en) * | 2011-10-20 | 2012-06-20 | 西北工业大学 | Method for preparing alumina-base eutectic ceramics in laser surface atmosphere heating furnace |
| CN102531553A (en) * | 2012-01-05 | 2012-07-04 | 西北工业大学 | Method for preparing alumina-based eutectic ceramic |
| CN102557595A (en) * | 2012-01-05 | 2012-07-11 | 西北工业大学 | Method for performing laser solid forming on aluminum oxide-based eutectic authigenic composite ceramic |
| CN102795842A (en) * | 2012-08-09 | 2012-11-28 | 广东潮流集团有限公司 | Ceramic material and preparation method thereof |
| CN103586296A (en) * | 2013-10-23 | 2014-02-19 | 大连理工大学 | Mosaic ceramic drawing die and making method thereof |
| CN105294085A (en) * | 2015-12-07 | 2016-02-03 | 哈尔滨工业大学 | Method for preparing aluminum oxide-based binary eutectic in-situ composite ceramic by pulsed discharge plasma-assisted melting treatment |
| CN108516808A (en) * | 2018-07-10 | 2018-09-11 | 哈尔滨工业大学 | The method that high-temperature fusant aeroponics prepare alumina-based nano eutectic composite micro-powder |
| CN108546122A (en) * | 2018-07-10 | 2018-09-18 | 哈尔滨工业大学 | A kind of method that alumina conbustion synthesis aerosol method prepares alumina-based nano eutectic composite ceramics micro mist |
-
2010
- 2010-06-26 CN CN 201010215806 patent/CN101905975A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 20091015 杜巍 共晶成分Al2O3-ZrO2复相陶瓷的制备与超塑成形 1-61 1 , 第10期 * |
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| CN102503380A (en) * | 2011-10-20 | 2012-06-20 | 西北工业大学 | Method for preparing alumina-base eutectic ceramics in laser surface atmosphere heating furnace |
| CN102531553A (en) * | 2012-01-05 | 2012-07-04 | 西北工业大学 | Method for preparing alumina-based eutectic ceramic |
| CN102557595A (en) * | 2012-01-05 | 2012-07-11 | 西北工业大学 | Method for performing laser solid forming on aluminum oxide-based eutectic authigenic composite ceramic |
| CN102557595B (en) * | 2012-01-05 | 2013-07-17 | 西北工业大学 | Method for performing laser solid forming on aluminum oxide-based eutectic authigenic composite ceramic |
| CN102531553B (en) * | 2012-01-05 | 2013-07-17 | 西北工业大学 | Method for preparing alumina-based eutectic ceramic |
| CN102795842A (en) * | 2012-08-09 | 2012-11-28 | 广东潮流集团有限公司 | Ceramic material and preparation method thereof |
| CN103586296A (en) * | 2013-10-23 | 2014-02-19 | 大连理工大学 | Mosaic ceramic drawing die and making method thereof |
| CN103586296B (en) * | 2013-10-23 | 2017-01-11 | 大连理工大学 | Mosaic ceramic drawing die and making method thereof |
| CN105294085A (en) * | 2015-12-07 | 2016-02-03 | 哈尔滨工业大学 | Method for preparing aluminum oxide-based binary eutectic in-situ composite ceramic by pulsed discharge plasma-assisted melting treatment |
| CN105294085B (en) * | 2015-12-07 | 2018-07-06 | 哈尔滨工业大学 | A kind of method that pulsed discharge plasma auxiliary remelting prepares the spontaneous composite ceramics of alumina base binary eutectic |
| CN108516808A (en) * | 2018-07-10 | 2018-09-11 | 哈尔滨工业大学 | The method that high-temperature fusant aeroponics prepare alumina-based nano eutectic composite micro-powder |
| CN108546122A (en) * | 2018-07-10 | 2018-09-18 | 哈尔滨工业大学 | A kind of method that alumina conbustion synthesis aerosol method prepares alumina-based nano eutectic composite ceramics micro mist |
| CN108516808B (en) * | 2018-07-10 | 2021-03-02 | 哈尔滨工业大学 | Method for preparing aluminum oxide-based nano eutectic composite micro powder by high-temperature melt aerosol method |
| CN108546122B (en) * | 2018-07-10 | 2021-10-15 | 哈尔滨工业大学 | Method for preparing alumina-based nano eutectic composite ceramic micro powder by using alumina combustion synthesis aerosol method |
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Application publication date: 20101208 |