CN106747434A - Wear-resisting zirconia ceramics and preparation method thereof - Google Patents
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Abstract
The present invention proposes a kind of wear-resisting zirconia ceramics and preparation method thereof, in parts by weight, including following raw material：4~8 parts of 60~70 parts of zirconium oxide, 1~3 part of graphene oxide, 10~14 parts of hydroxyapatite, 12~16 parts of surfactant, 9~12 parts of crosslinking agent and additive.Preparation method, comprises the following steps：Zirconium oxide, the mixed liquor of graphene oxide and polysilazane, hydroxyapatite, surfactant, crosslinking agent are well mixed with additive, obtain raw mixture, then dumping treatment is carried out at 500~600 DEG C, raw mixture after dumping is placed in platinum crucible and melts 2~3h in 1150~1300 DEG C, go to 4~5h of heat treatment in annealing furnace, it is slowly cooled to room temperature, you can.The ceramics have good anti-wear performance, and reduce liquid phase sintering conditions.
Description
Technical field
The invention belongs to ceramic technology field, and in particular to a kind of wear-resisting zirconia ceramics and preparation method thereof.
Background technology
Zirconia ceramics has the intensity higher than aluminum oxide, toughness and corrosion-proof wear, is widely used in metallurgical, change
The fields such as work, machinery, electronics, oil, because of its unique stress-induced martensitic phase transformation Toughening Properties, the toughness that is otherwise known as pottery
Porcelain.Zirconium oxide has high chemical stability and heat endurance (Tm=2953K), and inertia is presented in physiological environment, has
Good biocompatibility.Pure zirconia has three kinds of allotropy bodies, and crystal transfer (phase can occur under certain condition
Become).When external force effect is born, the process of the opposite m phase in version of its t need to absorb energy higher, make crack tip stress relaxation,
Increase crackle diffusional resistance and toughness reinforcing, thus with fracture toughness very high.
The production requirement of zirconia ceramics prepares good high-purity, dispersive property, particles ultra fine, the powder of narrow particle size distribution, oxygen
The preparation method for changing zirconium superfines is a lot, the purification of zirconium oxide mainly have chlorination and thermal decomposition method, alkali metal oxidative decomposition process,
Lime melting method, plasma arc process, the precipitation method, colloid method, Hydrolyze method, spray pyrolysis etc..Powder process has co-precipitation
Method, sol-gel method, evaporation, overcritical synthetic method, microemulsion method, the Hydrothermal Synthesiss net of justice and vapour deposition process etc..
Zirconium oxide only occurs with monoclinic phase under normal temperature, is heated to 1100 DEG C or so and is changed into Tetragonal, is heated at higher temperature
Degree can be converted into Emission in Cubic.Due to that can produce larger Volume Changes when monocline opposite tetragonal phase converting, cooling when
Waiting can in the opposite direction occur larger Volume Changes again, easily cause the cracking of product, limit pure zirconia in high temperature
The application in field, its anti-wear performance is general.
The content of the invention
The present invention proposes a kind of wear-resisting zirconia ceramics, and the ceramics have good anti-wear performance, and reduce liquid phase
Sintering temperature.
The technical proposal of the invention is realized in this way：
A kind of wear-resisting zirconia ceramics, in parts by weight, including following raw material：
60~70 parts of zirconium oxide, 1~3 part of graphene oxide, 10~14 parts of hydroxyapatite, surfactant 12~16
4~8 parts of part, 9~12 parts of crosslinking agent and additive；
Wherein, the graphene oxide prepares graphene oxide dispersion in adding DMF solution
Liquid, then mix with polysilazane solution, then stirring, ultrasound obtain mixed liquor；In the mixed solution, in mass ratio, poly- silicon
The ratio of azane content and graphene oxide content is 1: 0.1~1.
In as preferred some embodiments of the present invention, the ratio between Ca and P are 1 in the hydroxyapatite:1.98.
In as preferred some embodiments of the present invention, the surfactant is glycerin monostearate, Sorbitan
One or more in alcohol sesquioleate, methyl glycol fatty acid ester or dioctyl sodium sulfosuccinate.
In as preferred some embodiments of the present invention, the crosslinking agent is N, N '-methylene-bisacrylamide, divinyl
One or more in triamine or divinylbenzene.
In as preferred some embodiments of the present invention, the additive is one kind in zinc oxide, barium carbonate and calcirm-fluoride
Or it is several.
It is a further object to provide a kind of preparation method of wear-resisting zirconia ceramics, comprise the following steps：
1) graphene oxide prepares graphene oxide dispersion in adding DMF solution, then with it is poly-
Silazane solution mix, then stirring, ultrasound obtain mixed liquor, in mixed solution, in mass ratio, polysilazane content with oxidation
The ratio of Graphene content is 1: 0.1~1；
2) by zirconium oxide, step 1) mixed liquor, hydroxyapatite, surfactant, crosslinking agent mix with additive
It is even, raw mixture is obtained, dumping treatment then is carried out at 500~600 DEG C, the raw mixture after dumping is placed on platinum crucible
It is interior to melt 2~3h in 1150~1300 DEG C, 4~5h of heat treatment in annealing furnace is gone to, it is slowly cooled to room temperature, you can.
In as preferred some embodiments of the present invention, the concentration of the DMF solution is 2~5mol/
L。
Used as in preferred some embodiments of the present invention, soak time is 0.5~1.5h.
Used as in preferred some embodiments of the present invention, heat treatment temperature is 200~300 DEG C.
Advantages of the present invention：
1st, the present invention substitutes traditional magnesia, silica as sintering aid using graphene oxide, finds oxidation stone
Black alkene acceleration of sintering, improves the hardness and anti-wear performance of ceramics.
2nd, present inventors have surprisingly found that it is surprisingly found by the inventors that being added to N, N- dimethyl after graphene oxide mixing
In formamide solution after dipping pretreatment, then mix with polysilazane solution, improve resistance to height of the graphene oxide at high temperature
Warm nature energy, is conducive to follow-up high temperature sintering, rapid to reduce the material porosity and improve density of material, so as to largely reduce
The sintering temperature of cubic polycrystal zirconia (TZP) material.
Specific embodiment
Embodiment 1
A kind of wear-resisting zirconia ceramics, in parts by weight, including following raw material：
65 parts of zirconium oxide, 2 parts of graphene oxide, 12 parts of hydroxyapatite, 14 parts of surfactant, 10 parts of crosslinking agent with add
Plus 6 parts of agent.
The ratio between Ca and P are 1 in hydroxyapatite:1.98.
Surfactant is the mixture of glycerin monostearate and sorbitan sesquioleate.
Crosslinking agent is N, N '-methylene-bisacrylamide.
Additive is zinc oxide and calcirm-fluoride.
Preparation method, comprises the following steps：
1) graphene oxide dispersion is prepared in the N,N-dimethylformamide solution of graphene oxide addition 4mol/L
Liquid, then mix with polysilazane solution, then stirring, ultrasound obtain mixed liquor, in mixed solution, in mass ratio, polysilazane
The ratio of content and graphene oxide content is 1: 0.6；
2) by zirconium oxide, step 1) mixed liquor, hydroxyapatite, surfactant, crosslinking agent mix with additive
It is even, obtain raw mixture, then carry out dumping treatment at 500 DEG C, the raw mixture after dumping be placed in platinum crucible in
1200 DEG C of fusing 3h, go to heat treatment 4h in annealing furnace, and heat treatment temperature is 260 DEG C, is slowly cooled to room temperature, you can.
Embodiment 2
A kind of wear-resisting zirconia ceramics, in parts by weight, including following raw material：
60 parts of zirconium oxide, 1 part of graphene oxide, 10 parts of hydroxyapatite, 16 parts of surfactant, 12 parts of crosslinking agent with add
Plus 8 parts of agent.
The ratio between Ca and P are 1 in hydroxyapatite:1.98.
Surfactant is the mixture of methyl glycol fatty acid ester and dioctyl sodium sulfosuccinate.
Crosslinking agent is in divinylbenzene.
Additive is calcirm-fluoride.
Preparation method, comprises the following steps：
1) graphene oxide dispersion is prepared in the N,N-dimethylformamide solution of graphene oxide addition 2mol/L
Liquid, then mix with polysilazane solution, then stirring, ultrasound obtain mixed liquor, in mixed solution, in mass ratio, polysilazane
The ratio of content and graphene oxide content is 1: 0.9；
2) by zirconium oxide, step 1) mixed liquor, hydroxyapatite, surfactant, crosslinking agent mix with additive
It is even, obtain raw mixture, then carry out dumping treatment at 550 DEG C, the raw mixture after dumping be placed in platinum crucible in
1150 DEG C of fusing 2h, go to heat treatment 4.5h in annealing furnace, and heat treatment temperature is 200 DEG C, is slowly cooled to room temperature, you can.
Embodiment 3
A kind of wear-resisting zirconia ceramics, in parts by weight, including following raw material：
70 parts of zirconium oxide, 3 parts of graphene oxide, 10 parts of hydroxyapatite, 16 parts of surfactant, 9 parts of crosslinking agent with add
Plus 4 parts of agent.
The ratio between Ca and P are 1 in hydroxyapatite:1.98.
Surfactant is the mixture of glycerin monostearate and dioctyl sodium sulfosuccinate.
Crosslinking agent is N, N '-methylene-bisacrylamide.
Preparation method, comprises the following steps：
1) graphene oxide dispersion is prepared in the N,N-dimethylformamide solution of graphene oxide addition 5mol/L
Liquid, then mix with polysilazane solution, then stirring, ultrasound obtain mixed liquor, in mixed solution, in mass ratio, polysilazane
The ratio of content and graphene oxide content is 1: 0.1；
2) by zirconium oxide, step 1) mixed liquor, hydroxyapatite, surfactant, crosslinking agent mix with additive
It is even, obtain raw mixture, then carry out dumping treatment at 600 DEG C, the raw mixture after dumping be placed in platinum crucible in
1250 DEG C of fusing 2h, go to heat treatment 5h in annealing furnace, and heat treatment temperature is 300 DEG C, is slowly cooled to room temperature, you can.
Additive is zinc oxide.
Embodiment 4
A kind of wear-resisting zirconia ceramics, in parts by weight, including following raw material：
66 parts of zirconium oxide, 2 parts of graphene oxide, 13 parts of hydroxyapatite, 15 parts of surfactant, 12 parts of crosslinking agent with add
Plus 8 parts of agent.
The ratio between Ca and P are 1 in hydroxyapatite:1.98.
Surfactant is glycerin monostearate, sorbitan sesquioleate and dioctyl sodium sulfosuccinate
Mixture.
Crosslinking agent is diethylenetriamine.
Additive is the mixture of zinc oxide and calcirm-fluoride.
Preparation method, comprises the following steps：
1) graphene oxide dispersion is prepared in the N,N-dimethylformamide solution of graphene oxide addition 5mol/L
Liquid, then mix with polysilazane solution, then stirring, ultrasound obtain mixed liquor, in mixed solution, in mass ratio, polysilazane
The ratio of content and graphene oxide content is 1: 1；
2) by zirconium oxide, step 1) mixed liquor, hydroxyapatite, surfactant, crosslinking agent mix with additive
It is even, obtain raw mixture, then carry out dumping treatment at 540 DEG C, the raw mixture after dumping be placed in platinum crucible in
1300 DEG C of fusing 2h, go to heat treatment 5h in annealing furnace, and heat treatment temperature is 300 DEG C, is slowly cooled to room temperature, you can.
Comparative example 1
Same as Example 1, difference is：Graphene oxide is replaced with barium monoxide.
Performance test
Ceramics to embodiment 1~4 and comparative example 1 carry out performance test, the results are shown in Table 1.
The ceramic performance test result of the embodiment 1~4 of table 1 and comparative example 1
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (9)
1. a kind of wear-resisting zirconia is ceramic, it is characterised in that in parts by weight, including following raw material：
60~70 parts of zirconium oxide, 1~3 part of graphene oxide, 10~14 parts of hydroxyapatite, 12~16 parts of surfactant, friendship
4~8 parts of 9~12 parts of connection agent and additive；
Wherein, the graphene oxide prepares graphene oxide dispersion in adding DMF solution, then
Mix with polysilazane solution, then stirring, ultrasound obtain mixed liquor；In the mixed solution, in mass ratio, polysilazane contains
Amount is 1: 0.1~1 with the ratio of graphene oxide content.
2. wear-resisting zirconia according to claim 1 is ceramic, it is characterised in that the ratio between Ca and P in the hydroxyapatite
It is 1:1.98.
3. wear-resisting zirconia according to claim 1 is ceramic, it is characterised in that the surfactant is that monostearate is sweet
One or more in grease, sorbitan sesquioleate, methyl glycol fatty acid ester or dioctyl sodium sulfosuccinate.
4. wear-resisting zirconia according to claim 1 is ceramic, it is characterised in that the crosslinking agent is N, N '-di-2-ethylhexylphosphine oxide
One or more in acrylamide, diethylenetriamine or divinylbenzene.
5. wear-resisting zirconia according to Claims 1-4 any one is ceramic, it is characterised in that the additive is oxygen
Change one or more in zinc, barium carbonate and calcirm-fluoride.
6. it is a kind of as described in claim 1 to 5 any one wear-resisting zirconia ceramics preparation method, it is characterised in that bag
Include following steps：
1) graphene oxide prepares graphene oxide dispersion in adding DMF solution, then with poly- silicon nitrogen
Alkane solution mixes, and then stirring, ultrasound obtain mixed liquor, in mixed solution, in mass ratio, polysilazane content and graphite oxide
The ratio of alkene content is 1: 0.1~1；
2) by zirconium oxide, step 1) mixed liquor, hydroxyapatite, surfactant, crosslinking agent be well mixed with additive, obtain
To raw mixture, then carry out dumping treatment at 500~600 DEG C, the raw mixture after dumping be placed in platinum crucible in
1150~1300 DEG C of 2~3h of fusing, go to 4~5h of heat treatment in annealing furnace, are slowly cooled to room temperature, you can.
7. the preparation method of wear-resisting zirconia according to claim 6 ceramics, it is characterised in that the N, N- dimethyl methyl
The concentration of amide solution is 2~5mol/L.
8. the preparation method of wear-resisting zirconia according to claim 6 ceramics, it is characterised in that soak time is 0.5~
1.5h。
9. the preparation method of wear-resisting zirconia according to claim 6 ceramics, it is characterised in that heat treatment temperature is 200
~300 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437904A (en) * | 2018-12-29 | 2019-03-08 | 南京宝淳新材料科技有限公司 | A kind of oxide ceramic powder body and preparation method thereof |
| CN116514533A (en) * | 2023-05-31 | 2023-08-01 | 宜兴兴贝耐火材料制品有限公司 | Special corrosion-resistant wear-resistant plastic for SNCR (selective non-catalytic reduction) of CFB (CFB) target area and preparation method of special corrosion-resistant wear-resistant plastic |
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