CN104003728A - Pressureless sintering preparation method of Ti2SC ceramic - Google Patents
Pressureless sintering preparation method of Ti2SC ceramic Download PDFInfo
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- CN104003728A CN104003728A CN201410209332.0A CN201410209332A CN104003728A CN 104003728 A CN104003728 A CN 104003728A CN 201410209332 A CN201410209332 A CN 201410209332A CN 104003728 A CN104003728 A CN 104003728A
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- ceramic
- ti2sc
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- pottery
- sintering
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Abstract
A pressureless sintering preparation method of Ti2SC ceramic is characterized by comprising the following steps: (1) evenly mixing Ti2SC ceramic powder with polyvinyl alcohol PVA, and then filling into a die for preforming; (2) performing cold isostatic pressing treatment on the preformed Ti2SC ceramic; (3) putting the cold isostatic pressing treated Ti2SC ceramic into a microwave sintering furnace filled with inert gas protective atmosphere for sintering for 20-60 minutes at 800-1100 DEG C to obtain the Ti2SC bulk ceramic; the preparation method not only improves the density of the ceramic material, realizes the controllable density of the Ti2SC ceramic material, can prepare Ti2SC ceramic materials with complex shapes, and has the advantages of low sintering temperature, short time, saving energy and the like.
Description
Technical field
The invention provides a kind of preparation method of ternary layered compound pottery, relate to specifically a kind of non-pressure sintering technology and prepare Ti
2sC ceramic block material.
Background technology
Ti
2sC is M
n+1aX
na member in (n=1,2,3) ternary layered compound in " 211 " phase family, it belongs to hexagonal system, and it has and is similar to the good high heat conductance of metal and high conductivity, and has good corrosion resistance nature.Ti simultaneously
2sC also has the high strength that pottery has concurrently, and good high-temperature oxidation resistance.Therefore, Ti
2sC has broad application prospects in aerospace, nuclear industry, communications and transportation, petrochemical complex and the field such as metallurgical as high-temperature oxidation resistant and corrosion-resistant ceramic member and supercoat.Ti in whole MAX phase family
2sC has the feature of lattice parameter c minimum, and this just makes Ti
2sC has a lot of special performances, as the highest Vickers' hardness (8GPa) and the highest room temperature thermal conductivity (60W/mK) etc.These cause more and more investigation of materials persons' concern.
But, the research of other MAX phase of comparing, Ti
2the research of SC is very few, particularly aspect the correlative study that utilizes simple substance element to prepare, is rarely having especially report, and this is because elemental sulfur is easy to distillation volatilization in heat-processed.At present, Ti
2sC block materials is mostly by hot pressed sintering Ti
2[J.Am.Ceram, 2007,90:3953～3958 that the method for SC powder obtains; J.Appl.Phys, 2008,104:033502; Scripta Mater, 2011,65:573～576].Recently, the people [J.Alloys Comp, 2013,566:191～195] such as Wen Bin Zhu are with metallic titanium powder, and sulfuration titanium valve and carbon dust are raw material, and adopting traditional hot-pressing sintering method is that Ti has been synthesized in 30MPa insulation for 2 hours at 1600 ° of C pressure
2sC block materials.2013, Chinese invention patent (CN103253667A) was reported and a kind of as 2～6GPa condition under has been synthesized Ti in temperature as 1600 ° of C pressure taking simple substance as prepared using high temperature and high pressure method
2sC material.As can be seen here, synthesize at present Ti
2the method of SC block materials is mainly the method for hot pressed sintering, this kind of method synthesis temperature high (high temperature of nearly 1600 ° of C), and generated time very long want several hours.And size and dimension has certain limitation.The present invention adopts the method for microwave sintering can just prepare in low temperature and very short time the Ti of high-compactness
2sC ceramic block material.
Summary of the invention
The object of the invention provides a kind of pressureless sintering to prepare Ti for existing weak point in above-mentioned prior art just
2the method of SC ceramic block.The present invention is by microwave sintering and pass into inert atmosphere, and rate of heating is fast, and sintering temperature is low, and sintering time is short, general heating several minutes that only need.
Object of the present invention can realize by following technique measures:
Microwave of the present invention synthesizes Ti
2preparation method's step of SC stupalith is as follows: by Ti
2sC ceramic powder mixes with PVAC polyvinylalcohol, then packs mould premolding into.Ti after premolding
2sC pottery carries out isostatic cool pressing processing.By the Ti after isostatic cool pressing
2sC pottery not with the protection of the rare gas element of raw material and reaction product generation chemical reaction under the synthetic high-purity Ti of microwave heating
2sC pottery.
Ti described in the present invention
2the mass ratio of SC ceramic powder and PVAC polyvinylalcohol is 100:0.5 ~ 5; Ti
2the premolding pressure 1 ~ 10MPa of SC ceramic powder and PVAC polyvinylalcohol, pressurize 2 ~ 5 releases; The pressure of isostatic cool pressing is 100 ~ 280PMa, and microwave heating time is 5 ~ 20 minutes, and Heating temperature is 800 ~ 1100 ° of C; Described rare gas element is argon gas.
With existing preparation Ti
2the method of SC material is compared, and beneficial effect of the present invention is as follows:
(1) the present invention is first by Ti
2sC ceramic powder and PVAC polyvinylalcohol are mixed with Ti
2sC stupalith, by
A kind of water soluble adhesive in PVA, to Ti
2sC pottery has good bonding effect, and the present invention has simultaneously carried out innovative design to preparation technology, carries out Ti by techniques such as pre-compacted, isostatic cool pressing processing, pressureless sinterings
2the preparation of SC stupalith, this preparation method has not only improved Ti greatly
2the density of SC stupalith, isostatic cool pressing sample density after treatment is theoretical density 40 ~ 60%, and can prepare large-size and complicated shape ~ stupalith.
(2) the present invention is easy to operate, and technique is simple.The present invention adopts non-pressure sintering technology to carry out Ti
2the preparation of SC stupalith, does not need pressure when sintering, overcome for example limit intensification limit pressurization of traditional heat pressing process moulding, can not prepare the shortcoming such as stupalith of size large and complex-shaped (can only be cylinder, the regular shape such as square).In addition, can pass through according to actual needs the mould of the different complicated shapes of design, thereby prepare the pottery of various complicated shapes.
(3) preparation time is short, and cost is low.The present invention makes full use of the feature of microwave fast heating sintering, at short notice the Ti of Fast Sintering densification
2sC block materials.Compared with traditional preparation method (as hot-pressing sintering technique), efficiency has improved decades of times, has energy-conservation, efficient feature.Adopt microwave sintering legal system with no pressure for Ti
2sC material, has greatly shortened the reaction times and has reduced densification temperature, just can prepare Ti under 800 ~ 1100 ° of C and 20 ~ 60min condition
2sC block materials, has saved the energy greatly, has improved production efficiency.
embodiment:
Embodiment 1:
By Ti
2sC ceramic powder mixes with the mass ratio of 100:0.5 with PVAC polyvinylalcohol, then packs mould into 1MPa premolding, pressurize 2 minutes.Ti after premolding
2sC pottery packs rubber mold into and adopts 100MPa pressure to carry out isostatic cool pressing processing.By the Ti after isostatic cool pressing
2sC pottery microwave heating to 800 ° C sintering under the protection of rare gas element obtains Ti for 20 minutes
2sC ceramic block.
Utilizing above-mentioned technique finally to obtain density is 75% Ti
2sC ceramic block.
Embodiment 2:
By Ti
2sC ceramic powder mixes with the mass ratio of 100:2 with PVAC polyvinylalcohol, then packs mould into 5MPa premolding, pressurize 5 minutes.Ti after premolding
2sC pottery packs rubber mold into and adopts 150MPa pressure to carry out isostatic cool pressing processing.By the Ti after isostatic cool pressing
2sC pottery microwave heating to 900 ° C sintering under the protection of rare gas element obtains Ti for 40 minutes
2sC ceramic block.
Utilizing above-mentioned technique finally to obtain density is 88% Ti
2sC ceramic block.
Embodiment 3:
By Ti
2sC ceramic powder mixes with the mass ratio of 100:5 with PVAC polyvinylalcohol, then packs mould into 6MPa premolding, pressurize 5 minutes.Ti after premolding
2sC pottery packs rubber mold into and adopts 280MPa pressure to carry out isostatic cool pressing processing.By the Ti after isostatic cool pressing
2sC pottery microwave heating to 1100 ° C sintering under the protection of rare gas element obtains Ti for 60 minutes
2sC ceramic block.
Utilizing above-mentioned technique finally to obtain density is 98% Ti
2sC ceramic block.
Claims (8)
1. a microwave sintering Ti with no pressure
2the preparation method of SC stupalith, is characterized in that: by Ti
2sC ceramic powder mixes with PVAC polyvinylalcohol, then packs mould premolding into.
2. the Ti after premolding
2sC pottery carries out isostatic cool pressing processing.
3. by the Ti after isostatic cool pressing
2sC pottery not with the protection of the rare gas element of raw material and reaction product generation chemical reaction under microwave fire standby high fine and close Ti
2sC ceramic block material.
4. the microwave heating time described in the present invention is 20 ~ 60 minutes, and Heating temperature is 800 ~ 1100 ° of C; Described rare gas element is argon gas.
5. microwave sintering Ti with no pressure according to claim 1
2the preparation method of SC pottery, is characterized in that: Ti
2the mass ratio of SC ceramic powder and PVAC polyvinylalcohol is 100:0.5 ~ 5.
6. microwave sintering Ti with no pressure according to claim 1
2the preparation method of SC pottery, is characterized in that: Ti
2the premolding pressure 1 ~ 10MPa of SC ceramic powder and PVAC polyvinylalcohol, pressurize 2 ~ 5 releases;
Microwave sintering Ti with no pressure according to claim 1
2the preparation method of SC pottery, is characterized in that: the pressure of isostatic cool pressing is 100 ~ 280PMa.
7. microwave sintering Ti with no pressure according to claim 1
2the preparation method of SC pottery, is characterized in that: microwave sintering Heating temperature is 800 ~ 1100 ° of C, and the time is 20 ~ 60 minutes.
8. microwave synthesizes Ti according to claim 1
2the preparation method of SC pottery, is characterized in that: described rare gas element is argon gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410209332.0A CN104003728B (en) | 2014-05-19 | 2014-05-19 | A kind of pressureless sintering prepares Ti2The method of SC ceramics |
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| CN201410209332.0A CN104003728B (en) | 2014-05-19 | 2014-05-19 | A kind of pressureless sintering prepares Ti2The method of SC ceramics |
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| CN104003728B CN104003728B (en) | 2018-04-27 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083030A (en) * | 2016-06-22 | 2016-11-09 | 成都锦钛精工科技有限公司 | Ti3o5compact block material and preparation method thereof |
| CN115849925A (en) * | 2022-12-30 | 2023-03-28 | 江苏材睿科技有限公司 | Preparation method of pressureless sintering refractory material |
| CN115925432A (en) * | 2022-12-30 | 2023-04-07 | 江苏材睿科技有限公司 | Preparation method of high-conductivity refractory material |
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| US5942455A (en) * | 1995-11-14 | 1999-08-24 | Drexel University | Synthesis of 312 phases and composites thereof |
| CN101037201A (en) * | 2007-04-27 | 2007-09-19 | 武汉理工大学 | High-purity Ti2AlC powder material and preparing method thereof |
| CN101448760A (en) * | 2006-05-30 | 2009-06-03 | 原子能委员会 | MAX-phase powders and method for making same |
| CN102633505A (en) * | 2012-03-14 | 2012-08-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-purity MAX-phase ceramic powder |
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2014
- 2014-05-19 CN CN201410209332.0A patent/CN104003728B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5942455A (en) * | 1995-11-14 | 1999-08-24 | Drexel University | Synthesis of 312 phases and composites thereof |
| CN101448760A (en) * | 2006-05-30 | 2009-06-03 | 原子能委员会 | MAX-phase powders and method for making same |
| CN101037201A (en) * | 2007-04-27 | 2007-09-19 | 武汉理工大学 | High-purity Ti2AlC powder material and preparing method thereof |
| CN102633505A (en) * | 2012-03-14 | 2012-08-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-purity MAX-phase ceramic powder |
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| QIAN WANG ET AL.: "Synthesis of High-Purity Ti3SiC2 by Microwave Sintering", 《INTERNATIONAL JOURNAL OF APPLIED CERAMIC TECHNOLOGY》 * |
| SHAHRAM AMINI ET AL.: "Synthesis and Mechanical Properties of Fully Dense Ti2SC", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
| 林宗寿等: "《无机非金属材料工学 第4版》", 31 December 2013, 武汉理工大学出版社 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083030A (en) * | 2016-06-22 | 2016-11-09 | 成都锦钛精工科技有限公司 | Ti3o5compact block material and preparation method thereof |
| CN106083030B (en) * | 2016-06-22 | 2019-11-12 | 成都锦钛精工科技有限公司 | Ti3O5Compact block material and preparation method thereof |
| CN115849925A (en) * | 2022-12-30 | 2023-03-28 | 江苏材睿科技有限公司 | Preparation method of pressureless sintering refractory material |
| CN115925432A (en) * | 2022-12-30 | 2023-04-07 | 江苏材睿科技有限公司 | Preparation method of high-conductivity refractory material |
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Inventor after: Guan Chunlong Inventor after: Wang Shun Inventor after: Lu Xinpo Inventor after: Tian Ye Inventor after: Li Jinling Inventor after: Qin Yue Inventor after: Sun Nana Inventor after: Li Wenfeng Inventor after: Zhao Zhiwei Inventor before: Guan Chunlong Inventor before: Lu Xinpo Inventor before: Ma Qiuhua Inventor before: Li Jinling Inventor before: Bi Yu Inventor before: Wang Haikuo Inventor before: He Weichun Inventor before: Chen Yan |
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