CN1412150A - Self-lubricating ceramic composite material and its preparation process - Google Patents
Self-lubricating ceramic composite material and its preparation process Download PDFInfo
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- CN1412150A CN1412150A CN 02150057 CN02150057A CN1412150A CN 1412150 A CN1412150 A CN 1412150A CN 02150057 CN02150057 CN 02150057 CN 02150057 A CN02150057 A CN 02150057A CN 1412150 A CN1412150 A CN 1412150A
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Abstract
The present invention discloses a self-lubricating ceramic composite material and its preparation process. Said composite material is formed from yttrium oxide, zirconia and molybdenum disulfide, and its preparation process includes the following steps: adding the MoS2 powder body into the alcohol-water solution of yttrium nitrate and ZrOCl.8H2O, heating filtering, washing and calcining to prepare the composite powder body in which the yttrium oxide is stable tetragonal phase and molybdenum disulfide is covered with sirconia, making said composite powder body undergo the hot-pressing and sintering process so as to obtain the invented composite material.
Description
Technical field
The present invention relates to a kind of ceramic composite and preparation technology, specially refer to a kind of self-lubricating ceramic composite material and preparation technology.
Background technology
High technology ceramics is owing to have high-melting-point, high rigidity, wear-resistant, characteristics such as chemical property is stable, make it serve as high-abrasive material under the unlubricated medium in fields such as oil, chemical industry, automobile, mechanical industries, such as bearing, ball, liner, piston ring, wear ring etc., so the tribological property of stupalith is an importance that needs consideration.And find that under study for action though stupalith has high hardness and shear strength, when join pair with ceramic member, its frictional coefficient is generally 0.7～0.9, and generation heavy wear and losing efficacy, in application of practical project, be restricted.Therefore, the tribological property that improves stupalith makes it can be by one of critical prerequisite of successful Application.A kind of method of improving ceramic friction pair tribological property makes the material sliding surface have self-lubricating property exactly, promptly under DRY SLIDING, frictional coefficient and coefficient of wear is reduced in the desired scope.Another meaning that realizes the material self-lubricating is: save oiling system, can reduce weight, volume, improve equipment dependability and prolongs life (needn't consider replenishing of lubricant).Yttrium oxide (Y
2O
3) stablize tetragonal phase zirconium oxide (ZrO
2) pottery (Y-TZP) has very high intensity and fracture toughness property, thereby in engineering, used widely.Molybdenumdisulphide is the compound of a metalloid laminate structure, promptly at two-layer S atom therebetween one deck Mo atom, form sandwich sandwich structure, this flaggy is piled up up and down in crystal, make the S atomic shell of the S atomic shell of a flaggy and another flaggy adjacent, therebetween by weak Van der Waals force combination.6 the S atoms of arranging around the Mo atom in the laminate structure, between them with the strong covalent bond combination.Because molybdenumdisulphide (MoS
2) laminate structure of material uniqueness, and make it have good self-lubricating.Therefore, the compound available of molybdenumdisulphide and zirconium white can the complementary self-lubricating composite.
The mechanical property of material and tribological property and its microstructure and technological process have confidential relation; Simultaneously, in composition one timing of material, technological process has decisive action to the microstructure of material.And the technology of existing preparation self-lubricating ceramic composite material is with after ceramic powder and the direct mixing of lubricated powder mutually, by certain moulding and sintering process, prepares massive material.Above-mentioned technological process is difficult to guarantee the homodisperse of ceramic powder and lubricated powder mutually, thereby has determined the unhomogeneity of self-lubrication ceramic material on microstructure of preparation.Therefore, the ceramic composite that goes out of this prepared is difficult to guarantee the unification of oilness and mechanical property.So synthetic be uniformly dispersed, reunite less, active high ceramic composite powder is one of gordian technique of preparation high-performance self-lubricating ceramic composite material, could guarantee to prepare uniform microstructure and the good ceramic composite of macro property like this.
Summary of the invention
The object of the present invention is to provide a kind of self-lubricating composite ceramic material and preparation technology, this prepared composite ceramic material has excellent mechanical property and tribological property.
A kind of self-lubricating ceramic composite material, the parts by weight that it is characterized in that material be by 2～8 parts of yttrium oxide, 100 parts of zirconium whites, 50～100 parts of compositions of molybdenumdisulphide.
Because yttrium oxide (Y
2O
3) stablize tetragonal phase zirconium oxide (ZrO
2) pottery (Y-TZP) has very high intensity and fracture toughness property, and molybdenumdisulphide (MoS
2) material has good self-lubricating, therefore, by special process means, preparation Y-TZP parcel MoS
2Composite granule, have special microstructural composite ceramic material by high temperature hot pressed sintering preparation.The micro-structural feature of this material is: Y-TZP is an external phase, MoS
2Self-lubricating is dispersed among the Y-TZP mutually.This microstructure can Y-TZP is high intensity and fracture toughness property and MoS
2The organic combination of good self-lubricating property is so this matrix material has good mechanical property and tribological property.Simultaneously, MoS
2Wrapped up by Y-TZP, help stoping MoS
2High temperature oxidation, thereby improved this matrix material use temperature.
The alcohol-water solution heating method is that a kind of preparation reunion is few, active high ZrO
2The method of powder, its ultimate principle is: work as ZrOCl
28H
2When O heated in alcohol-water solution, the specific inductivity of solution descended rapidly, caused the solvation energy decline of solution, the solvency power of solvent to descend, and solution reaches capacity state and produces precipitation.Utilize this principle, can prepare the good ZrO of sintering character
2Powder.And the present invention utilizes above-mentioned principle, at Yttrium trinitrate and ZrOCl
28H
2Add MoS in the alcohol-water solution of O
2Powder, and heating make ZrOCl
28H
2The Zr (OH) that O forms
4At MoS
2The particle surface heterogeneous nucleation; When the pH value of regulator solution to greater than 9 the time, Yttrium trinitrate is transformed into Y (OH)
3And from solution, separate out, finally form Y (OH)
3And Zr (OH)
4Parcel MoS
2Powder granule is calcined under nitrogen protection then, makes Y (OH)
3And Zr (OH)
4Decompose and formation Y-TZP, can prepare the good Y-TZP parcel MoS of sintering character by above-mentioned technological process
2Powder granule.Sintering under certain temperature, pressure finally makes the stabilized with yttrium oxide tetragonal phase zirconium oxide and the molybdenumdisulphide matrix material of tribology and good mechanical performance.
The used raw material of the present invention is an industrial raw material, Yttrium trinitrate, ZrOCl
28H
2O, MoS
2Purity greater than 99%, MoS wherein
2Granularity be 1～5 μ m, the alcoholic acid water content is less than 1%, water is distilled water.The raw material of stabilized with yttrium oxide tetragonal phase zirconium oxide and molybdenumdisulphide matrix material consists of: Yttrium trinitrate is 6～15 parts, ZrOCl
28H
2O is 100 parts, MoS
2It is 50～100 parts.
The preparation method of stabilized with yttrium oxide tetragonal phase zirconium oxide and molybdenumdisulphide matrix material step in the following order carries out:
(1) 6～15 part Yttrium trinitrate and 100 parts of ZrOCl
28H
2O joins in the mixing solutions of second alcohol and water, under agitation condition, with 50～100 parts MoS
2Powder granule joins in the above-mentioned solution, up to MoS
2In solution, be uniformly dispersed;
(2) under agitation condition, mixing solutions is heated to 70～80 ℃, be incubated 4～8 hours, cool to room temperature, the pH value of regulator solution is greater than 9;
(3) mixed solution is filtered, and filtration product is washed, dry and calcining;
(4) with the powder of preparation, use compression molding, behind pressure 100～200MPa, the base substrate after the moulding is put into hot pressing furnace and is carried out sintering.
Among the preparation method of the present invention, Yttrium trinitrate, ZrOCl
28H
2O, MoS
2Purity greater than 99%, MoS wherein
2Granularity be 1～5 μ m.
In the mixing solutions of second alcohol and water, the alcoholic acid volumetric concentration is 20～95% among the preparation method of the present invention.
ZrOCl among the preparation method of the present invention
28H
2Concentration 0.1～0.5 mol of O in the mixed solution of second alcohol and water.
Desciccate is calcined under nitrogen protection among the preparation method of the present invention, temperature is 700～900 ℃, is incubated 1～5 hour.
Among the preparation method of the present invention, the sintering temperature of matrix material is 1200～1400 ℃, and pressure is 20～40MPa, and soaking time is 0.5～2 hour.
The stabilized with yttrium oxide tetragonal phase zirconium oxide and the molybdenumdisulphide performance of composites parameter of embodiment 1 preparation:
| Relative theory density | 90～99％ |
| | 2～5GPa |
| Frictional coefficient (friction pair is a zirconium white) | Be not more than 0.25 |
| Coefficient of wear (friction pair is a zirconium white) | Less than 1 * 10 -6mm 3/Nm |
The stabilized with yttrium oxide tetragonal phase zirconium oxide and the molybdenumdisulphide matrix material of the present invention's preparation have following characteristics:
(1) the stabilized with yttrium oxide tetragonal phase zirconium oxide parcel molybdenumdisulphide powder particle of preparing has reunion and lacks, the sintering activity height, and good uniformity is etc. characteristics;
(2) the particle coated outside stabilized with yttrium oxide tetragonal phase zirconium oxide of molybdenumdisulphide, the oxidation of molybdenumdisulphide under the favourable prevention high temperature, thus improved the high temperature oxidation temperature of molybdenumdisulphide;
(3) particle surface of molybdenumdisulphide parcel stabilized with yttrium oxide tetragonal phase zirconium oxide makes the stabilized with yttrium oxide tetragonal phase zirconium oxide form external phase by high temperature sintering, and the stupalith of final preparation has the good mechanical performance;
(4) there is molybdenumdisulphide self-lubricating phase in the matrix material, makes it have little frictional coefficient and coefficient of wear, can reach the requirement of solid lubricant.
Description of drawings
Fig. 1 is among the embodiment 1, under nitrogen protection, and the X-ray diffractogram of calcining back powder.From the X-ray diffractogram of powder, the composite granule by the present invention's preparation only contains tetragonal zircite (t-ZrO as can be seen
2) and MoS
2Two-phase.
Fig. 2 is embodiment 1, the profile scanning electromicroscopic photograph of stabilized with yttrium oxide tetragonal phase zirconium oxide and molybdenumdisulphide matrix material.Can observe from the profile scanning electromicroscopic photograph of matrix material, the stabilized with yttrium oxide tetragonal phase zirconium oxide is an external phase, is wrapped in around the flaky molybdenum disulfide particulate, and molybdenumdisulphide aligns owing to be under pressure, and its slip plane is perpendicular to pressure direction.
Embodiment
Embodiment 1
Yttrium trinitrate and 26 gram ZrOCl with 2 grams
28H
2It is in 10～6: 1 the mixing solutions that O joins ethanol and water volume ratio, ZrOCl
28H
2The strength of solution of O is 0.1～0.3 mol, stirs.Under agitation condition, with the MoS of 11.82 grams
2Powder granule joins in the above-mentioned solution, up to MoS
2In solution, be uniformly dispersed.Under agitation condition, mixing solutions is heated to 70～80 ℃, be incubated 2～4 hours, naturally cool to room temperature, the pH value of regulator solution arrives greater than 9.Mixed solution filters, washs, drying.With desciccate under nitrogen protection, calcine, temperature is 700～900 ℃, is incubated 1～4 hour, naturally cooling.With the powder of preparation, use compression molding, behind the pressure 200MPa, put into hot pressing furnace and carry out sintering.Sintering temperature is 1200～1300 ℃, and soaking time is 1 hour.
Yttrium trinitrate and 52 gram ZrOCl with 3 grams
28H
2O joins the mixing solutions of second alcohol and water, under agitation condition, with the MoS of 20 grams
2In the powder granule mixing solutions, prepare stabilized with yttrium oxide tetragonal phase zirconium oxide and molybdenumdisulphide matrix material by the technological process of embodiment 1.
Claims (8)
1. self-lubricating ceramic composite material, the parts by weight that it is characterized in that material be by 2～8 parts of yttrium oxide, 100 parts of zirconium whites, 50～100 parts of compositions of molybdenumdisulphide.
2. self-lubricating ceramic composite material, it is characterized in that the microstructure of material: the stabilized with yttrium oxide tetragonal phase zirconium oxide is an external phase, and the molybdenumdisulphide self-lubricating is dispersed in the stabilized with yttrium oxide tetragonal phase zirconium oxide mutually.
3. the preparation technology of material according to claim 1, this technology step is in the following order carried out:
(1) with Yttrium trinitrate and 100 parts of ZrOCl of 6～15 parts
28H
2O joins in the mixing solutions of second alcohol and water, under agitation condition, with 50～100 parts MoS
2Powder granule joins in the above-mentioned solution, up to MoS
2In solution, be uniformly dispersed;
(2) under agitation condition, mixing solutions is heated to 70～80 ℃, be incubated 4～8 hours, cool to room temperature, the pH value of regulator solution is greater than 9;
(3) mixed solution is filtered, and filtration product is washed, dry and calcining;
(4) with the powder of preparation, use compression molding, behind pressure 100～200MPa, the base substrate after the moulding is put into hot pressing furnace and is carried out sintering.
4. preparation technology as claimed in claim 3 is characterized in that Yttrium trinitrate, ZrOCl
28H
2O, MoS
2Purity greater than 99%, MoS wherein
2Granularity be 1～5 μ m.
5. preparation technology as claimed in claim 3 is characterized in that in the mixing solutions of second alcohol and water that the alcoholic acid volumetric concentration is 20～95%.
6. preparation technology as claimed in claim 3 is characterized in that ZrOCl
28H
2Concentration 0.1～0.5 mol of O in the mixed solution of second alcohol and water.
7. preparation technology as claimed in claim 3 is characterized in that desciccate is calcined, temperature is 700～900 ℃ under nitrogen protection, be incubated 1～5 hour.
8. preparation technology as claimed in claim 3, the sintering temperature that it is characterized in that matrix material is 1200～1400 ℃, and pressure is 20～40MPa, and soaking time is 0.5～2 hour.
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|---|---|---|---|
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|---|---|---|---|
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|---|---|---|---|---|
| CN103102157A (en) * | 2007-04-27 | 2013-05-15 | 应用材料公司 | Apparatus and method which reduce the erosion rate of surfaces exposed to halogen-containing plasmas |
| CN101293771B (en) * | 2007-04-27 | 2013-06-26 | 应用材料公司 | Apparatus and method which reduce the erosion rate of surfaces exposed to halogen-containing plasmas |
| CN105294099A (en) * | 2014-07-22 | 2016-02-03 | 中国科学院兰州化学物理研究所 | ZrO2-MoS2-CaF2 high-temperature self-lubricating wear-resistant material |
| CN107082639A (en) * | 2017-04-23 | 2017-08-22 | 南京云启金锐新材料有限公司 | High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof |
| CN108395246A (en) * | 2018-05-15 | 2018-08-14 | 钱兴 | A kind of preparation method of high tenacity oral cavity Nano ceramic powder material |
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| US10840113B2 (en) | 2007-04-27 | 2020-11-17 | Applied Materials, Inc. | Method of forming a coated article and semiconductor chamber apparatus from yttrium oxide and zirconium oxide |
| US11014853B2 (en) | 2018-03-07 | 2021-05-25 | Applied Materials, Inc. | Y2O3—ZrO2 erosion resistant material for chamber components in plasma environments |
| CN115677385A (en) * | 2022-10-25 | 2023-02-03 | 哈尔滨工业大学 | Preparation method of abradable composite coating with ceramic matrix composite surface capable of resisting temperature up to 1300 DEG C |
-
2002
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| US10847386B2 (en) | 2007-04-27 | 2020-11-24 | Applied Materials, Inc. | Method of forming a bulk article and semiconductor chamber apparatus from yttrium oxide and zirconium oxide |
| CN101293771B (en) * | 2007-04-27 | 2013-06-26 | 应用材料公司 | Apparatus and method which reduce the erosion rate of surfaces exposed to halogen-containing plasmas |
| CN103102157A (en) * | 2007-04-27 | 2013-05-15 | 应用材料公司 | Apparatus and method which reduce the erosion rate of surfaces exposed to halogen-containing plasmas |
| US11373882B2 (en) | 2007-04-27 | 2022-06-28 | Applied Materials, Inc. | Coated article and semiconductor chamber apparatus formed from yttrium oxide and zirconium oxide |
| US10622194B2 (en) | 2007-04-27 | 2020-04-14 | Applied Materials, Inc. | Bulk sintered solid solution ceramic which exhibits fracture toughness and halogen plasma resistance |
| US10840113B2 (en) | 2007-04-27 | 2020-11-17 | Applied Materials, Inc. | Method of forming a coated article and semiconductor chamber apparatus from yttrium oxide and zirconium oxide |
| US10840112B2 (en) | 2007-04-27 | 2020-11-17 | Applied Materials, Inc. | Coated article and semiconductor chamber apparatus formed from yttrium oxide and zirconium oxide |
| CN105294099A (en) * | 2014-07-22 | 2016-02-03 | 中国科学院兰州化学物理研究所 | ZrO2-MoS2-CaF2 high-temperature self-lubricating wear-resistant material |
| CN107082639A (en) * | 2017-04-23 | 2017-08-22 | 南京云启金锐新材料有限公司 | High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof |
| US11014853B2 (en) | 2018-03-07 | 2021-05-25 | Applied Materials, Inc. | Y2O3—ZrO2 erosion resistant material for chamber components in plasma environments |
| US11667577B2 (en) | 2018-03-07 | 2023-06-06 | Applied Materials, Inc. | Y2O3—ZrO2 erosion resistant material for chamber components in plasma environments |
| CN108395246A (en) * | 2018-05-15 | 2018-08-14 | 钱兴 | A kind of preparation method of high tenacity oral cavity Nano ceramic powder material |
| CN115677385A (en) * | 2022-10-25 | 2023-02-03 | 哈尔滨工业大学 | Preparation method of abradable composite coating with ceramic matrix composite surface capable of resisting temperature up to 1300 DEG C |
| CN115677385B (en) * | 2022-10-25 | 2023-09-08 | 哈尔滨工业大学 | Preparation method of abradable composite coating with surface temperature resistance reaching 1300 ℃ of ceramic matrix composite |
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