CN1410389A - Nano tetragonal phase zirconium oxide powder and preparation thereof - Google Patents
Nano tetragonal phase zirconium oxide powder and preparation thereof Download PDFInfo
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- CN1410389A CN1410389A CN 02135800 CN02135800A CN1410389A CN 1410389 A CN1410389 A CN 1410389A CN 02135800 CN02135800 CN 02135800 CN 02135800 A CN02135800 A CN 02135800A CN 1410389 A CN1410389 A CN 1410389A
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Abstract
A nanometre-class square-phase zirconium oxide powder is prepared through wrapping the Y-TZP ceramic nano-powder by organic substance, dewatering to obtain carbon-wrapped powder, and sintering to obtain the said powder. It has 50-80 nm of granularity, more than 97% of relative density, and better dispersity. Its surficial carbon film has good lubricating performance.
Description
Technical field:
The present invention's a kind of nanometer tetragonal phase zirconium oxide powder and preparation belong to the material field, in particular to the technical scheme of a kind of stupalith powder and preparation.
Technical background
The zirconium dioxide base ceramic material has premium propertiess such as high rigidity, high strength, wear-resistant, high temperature resistant and electrical isolation, is widely used on 26S Proteasome Structure and Function.Four main aspects that zirconium white is used are engineering ceramics, Zirconia electrolytic, heat insulating coat and high grade refractory.Position first of the room temperature strength of the tetragonal phase zirconium oxide pottery (processing of synthesizing nano Y-TZP pottery) of stabilized with yttrium oxide, fracture toughness property tool pottery.Because nano grain surface can be big, grain growing is rapid, even under the condition of Fast Sintering or under the very low temperature, also is easy to long to more than the 100nm.In the research of current nano ceramics, people have taked growing up of multiple means control crystal grain, in order to obtain the processing of synthesizing nano Y-TZP pottery, need excellent property powder, adopt the ultra-high voltage moulding, ceramic powder carried out surface treatment or the like.
At present Zirconium powder surface treatment method relatively more commonly used is had:
1. polymkeric substance is wrapped up on the nano zirconium oxide powder surface
Purpose at nano zirconium oxide powder surface parcel polymkeric substance is the sorbing agent that makes single stable.The polymer deposition method is adopted in the surface treatment of most of nano zirconium oxide powders.
2. chemical nickel plating
The main purpose of chemical nickel plating is the preparation ceramic-metal composite material.
3. composite nano particle is synthetic
This method is normally by the non-homogeneous phase deposition technique for packing, and at particulate surface parcel one deck nano-powder, thereby the various performances of change powder prepare composite ceramic material.
The method that present employed zirconium surface is modified, and fail to solve the problem that the processing of synthesizing nano Y-TZP ceramic powder is reunited and grown up in the agglomerating process, and address this problem the gordian technique for preparing nano ceramics just.
Summary of the invention
The present invention's a kind of nanometer tetragonal phase zirconium oxide powder and preparation purpose are to utilize the bag carbon modification of Zirconium powder to reach the purpose that inhibition is reunited and grown up in sintering process, thereby disclose the technical scheme of a kind of nanometer tetragonal phase zirconium oxide powder and preparation.Technical characterictic
A kind of nanometer tetragonal phase zirconium oxide of the present invention powder, the composition that it is characterized in that this powder is Y
2O
3Content is 2%～3%; ZrO
2Content is 92%～96.5%; The content of C is 1.5%～5%, and its crystalline structure is cubic phase, and integument is an amorphous carbon film, and thickness is about 1～2nm, and particle shape is the class sphere.
The preparation of a kind of nanometer tetragonal phase zirconium oxide of the present invention powder is characterized in that it is with the pack of organism liquid phase nanometer tetragonal phase zirconium oxide powder to be carried out surface bag carbon to modify, and its concrete preparation method is as follows: I, main raw material
The tetragonal phase zirconium oxide of stabilized nano yttrium oxide (Y-TZP) ceramic powder, dextrin ((C
6H
10O
5)
nXH
2O), polyvinyl alcohol ((C
2H
4O)
n), deionized water; II, device parameter (1) TEM model: H-800, parameter: operating voltage 200KV, some resolution 0.3nm; (2) XRD model: RAX-10, parameter: operating voltage 40KV, working current 0.1A target: copper target; (3) vacuum sintering furnace model: HZS-25, parameter: 2200 ℃ of top temperatures, power 25KW, final vacuum 6.6 * 10
-3Pa; (4) magnetic force heating stirrer model: 78-1 type; III, technical scheme (1) take by weighing organism polyvinyl alcohol, dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 5～1: 20 ratio; (2) organism polyvinyl alcohol, dextrin are heated to 80 ℃～90 ℃ dissolvings with 1～2% ratio in deionized water; (3) with the Zirconium powder of desire parcel ultra-sonic dispersion 30～60 minutes in above-mentioned solution; (4) make its thorough mixing with the magnetic force heating stirrer, heating, stirring, drying obtain the powder of surface parcel; (5) powder of above-mentioned surface parcel is put into vacuum sintering furnace, 400 ℃～600 ℃ insulations 1.5～3 hours down, carry out polyvinyl alcohol, the dextrin processed gets final product.
Organism polyvinyl alcohol, dextrin and processing of synthesizing nano Y-TZP ceramic powder optimum proportion are 1: 10～1: 15 in the technique scheme.Advantage and purposes
1. diameter of particle increased to some extent after the tem analysis before and after the powder parcel carbon film wrapped up carbon film as can be known, and particle diameter is about 12nm before the parcel, and parcel back particle diameter is about 15nm, shape class sphere.
2. can find out that by the XRD spectrum analysis before and after the powder parcel carbon film position of parcel front and back diffraction peak remains unchanged substantially, after also promptly wrapping up, the crystal formation of powder does not change, it still is cubic phase, just grain size increases to some extent, deducibility thus, the carbon that superscribes are decolorizing carbon, do not participate in diffraction.
3. after the powder sintering moulding, the relative density that is recorded sintered compact by drainage all reaches more than 97%, and particle grain size is about 15nm before the sintering, behind the sintering in the sintered compact particle grain size be approximately about 50～80nm, and do not need ultra-high voltage compression moulding, reach domestic and international advanced level.
4. behind oversintering, particle size reaches nano level, is better than the sintering character of not modified nano zirconium oxide powder, its good dispersion property, and also the top layer carbon film has good lubricity, is expected to become good lubricated Ji.
Embodiment
Mode 1: in 1: 5 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; Polyvinyl alcohol is heated to 80 ℃ of dissolvings with 1.5% ratio in deionized water; The processing of synthesizing nano Y-TZP ceramic powder is joined in the solution for preparing ultra-sonic dispersion 30 minutes; Make its thorough mixing with the magnetic force heating stirrer, heating, stirring, drying obtain the powder of surface parcel polyvinyl alcohol; This powder is put into vacuum sintering furnace, be incubated 3 hours down, carry out the polyvinyl alcohol processed at 400 ℃.
Mode 2: in 1: 5 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; Polyvinyl alcohol is heated to 85 ℃ of dissolvings with 2% ratio in deionized water; The processing of synthesizing nano Y-TZP ceramic powder is joined in the solution for preparing ultra-sonic dispersion 45 minutes; Make its thorough mixing with the magnetic force heating stirrer, heating, stirring, drying obtain the powder of surface parcel polyvinyl alcohol; This powder is put into vacuum sintering furnace, be incubated 1.5 hours down, carry out the polyvinyl alcohol processed at 500 ℃.
Mode 3: in 1: 5 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; Polyvinyl alcohol is heated to 90 ℃ of dissolvings with 1% ratio in deionized water; The processing of synthesizing nano Y-TZP ceramic powder is joined in the solution for preparing ultra-sonic dispersion 60 minutes; Make its thorough mixing with the magnetic force heating stirrer, heating, stirring, drying obtain the powder of surface parcel polyvinyl alcohol; This powder is put into vacuum sintering furnace, be incubated 2.5 hours down, carry out the polyvinyl alcohol processed at 600 ℃.
Mode 4: in 1: 8 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 1.
Mode 5: in 1: 10 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 1.
Mode 6: in 1: 12 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 1.
Mode 7: in 1: 15 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 1.
Mode 8: in 1: 18 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 1.
Mode 9: in 1: 20 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 1.
Mode 10: in 1: 10 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 2.
Mode 11: in 1: 15 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 2.
Mode 12: in 1: 20 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 2.
Mode 13: in 1: 10 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 3.
Mode 14: in 1: 15 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 3.
Mode 15: in 1: 20 ratio weighing polyvinyl alcohol and processing of synthesizing nano Y-TZP ceramic powder; As follows mode 3.
Mode 16: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 5 ratio; Dextrin is heated to 80 ℃ of dissolvings with 1% ratio in deionized water; The processing of synthesizing nano Y-TZP ceramic powder is joined in the solution for preparing ultra-sonic dispersion 30 minutes; Make its thorough mixing with the magnetic force heating stirrer, heating, stirring, drying obtain the powder of surface parcel dextrin; This powder is put into vacuum sintering furnace, be incubated 2 hours down, carry out the dextrin processed at 400 ℃.
Mode 17: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 5 ratio; Dextrin is heated to 90 ℃ of dissolvings with 2% ratio in deionized water; The processing of synthesizing nano Y-TZP ceramic powder is joined in the solution for preparing ultra-sonic dispersion 45 minutes; Make its thorough mixing with the magnetic force heating stirrer, heating, stirring, drying obtain the powder of surface parcel dextrin; This powder is put into vacuum sintering furnace, be incubated 3 hours down, carry out the dextrin processed at 500 ℃.
Mode 18: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 5 ratio; Dextrin is heated to 85 ℃ of dissolvings with 1.5% ratio in deionized water; The processing of synthesizing nano Y-TZP ceramic powder is joined in the solution for preparing ultra-sonic dispersion 60 minutes; Make its thorough mixing with the magnetic force heating stirrer, heating, stirring, drying obtain the powder of surface parcel dextrin; This powder is put into vacuum sintering furnace, be incubated 1.5 hours down, carry out the dextrin processed at 600 ℃.
Mode 19: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 8 ratio; As follows mode 16.
Mode 20: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 10 ratio; As follows mode 16.
Mode 21: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 12 ratio; As follows mode 16.
Mode 22: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 15 ratio; As follows mode 16.
Mode 23: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 18 ratio; As follows mode 16.
Mode 24: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 20 ratio; As follows mode 16.
Mode 25: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 10 ratio; As follows mode 17.
Mode 26: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 15 ratio; As follows mode 17.
Mode 27: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 20 ratio; As follows mode 17.
Mode 28: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 10 ratio; As follows mode 18.
Mode 29: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 15 ratio; As follows mode 18.
Mode 30: take by weighing dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 20 ratio; As follows mode 18.
Claims (3)
1. nanometer tetragonal phase zirconium oxide powder, the composition that it is characterized in that this powder is Y
2O
3Content is 2%～3%; ZrO
2Content is 92%～96.5%; The content of C is 1.5%～5%; Crystalline structure is cubic phase, and integument is an amorphous carbon film, and thickness is about 1～2nm, and particle shape is the class sphere.
2. the preparation of a nanometer tetragonal phase zirconium oxide powder is characterized in that it being with the pack of organism liquid phase nanometer tetragonal phase zirconium oxide powder to be carried out surface bag carbon to modify, and its concrete preparation method is as follows: I, main raw material
The tetragonal phase zirconium oxide of stabilized nano yttrium oxide (Y-TZP) ceramic powder, dextrin ((C
6H
10O
5)
nXH
2O) analytical pure, polyvinyl alcohol ((C
2H
4O)
n), deionized water; II, device parameter
(1) TEM model: H-800, parameter: operating voltage 200KV, some resolution 0.3nm;
(2) XRD model: RAX-10, parameter: operating voltage 40KV, working current 0.1A target: copper target;
(3) vacuum sintering furnace model: HZS-25, parameter: 2200 ℃ of top temperatures, power 25KW, final vacuum 6.6 * 10
-3Pa, effectively heating zone size (mm): φ 200 * 300;
(4) magnetic force heating stirrer model: 78-1 type; III, technical scheme
(1) takes by weighing organism polyvinyl alcohol, dextrin and processing of synthesizing nano Y-TZP ceramic powder in 1: 5～1: 20 ratio;
(2) organism polyvinyl alcohol, dextrin are heated to 80 ℃～90 ℃ dissolvings with 1～2% ratio in deionized water;
(3) with the Zirconium powder of desire parcel ultra-sonic dispersion 30～60 minutes in above-mentioned solution;
(4) make its thorough mixing with the magnetic force heating stirrer, heating, stirring, drying obtain the powder of surface parcel;
(5) powder of above-mentioned surface parcel is put into vacuum sintering furnace, 400 ℃～600 ℃ insulations 1.5～3 hours down, carry out polyvinyl alcohol, the dextrin processed gets final product.
3. according to the preparation of the described nanometer tetragonal phase zirconium oxide of claim 2 powder, it is characterized in that described organism polyvinyl alcohol, dextrin and processing of synthesizing nano Y-TZP ceramic powder optimum proportion are 1: 10～1: 15.
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|---|---|---|---|
| CN 02135800 CN1229304C (en) | 2002-11-16 | 2002-11-16 | Nano tetragonal phase zirconium oxide powder and preparation thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02135800 CN1229304C (en) | 2002-11-16 | 2002-11-16 | Nano tetragonal phase zirconium oxide powder and preparation thereof |
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| Publication Number | Publication Date |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100341791C (en) * | 2005-12-28 | 2007-10-10 | 中国科学院长春应用化学研究所 | Method for synthesizing organic ligand coated zirconium oxide nano crystal |
| CN102765935A (en) * | 2011-05-05 | 2012-11-07 | 中国农业机械化科学研究院 | Yttria stabilized zirconia powder, its preparation method and formed coating |
| CN101081735B (en) * | 2005-10-07 | 2013-03-13 | 苏舍美特科（美国）公司 | Optimized high temperature thermal heat barrier |
-
2002
- 2002-11-16 CN CN 02135800 patent/CN1229304C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101081735B (en) * | 2005-10-07 | 2013-03-13 | 苏舍美特科（美国）公司 | Optimized high temperature thermal heat barrier |
| CN100341791C (en) * | 2005-12-28 | 2007-10-10 | 中国科学院长春应用化学研究所 | Method for synthesizing organic ligand coated zirconium oxide nano crystal |
| CN102765935A (en) * | 2011-05-05 | 2012-11-07 | 中国农业机械化科学研究院 | Yttria stabilized zirconia powder, its preparation method and formed coating |
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| CN1229304C (en) | 2005-11-30 |
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