CN108727015A - A kind of zirconium oxide base metal-ceramic material preparation method - Google Patents
A kind of zirconium oxide base metal-ceramic material preparation method Download PDFInfo
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- CN108727015A CN108727015A CN201810600248.XA CN201810600248A CN108727015A CN 108727015 A CN108727015 A CN 108727015A CN 201810600248 A CN201810600248 A CN 201810600248A CN 108727015 A CN108727015 A CN 108727015A
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- zirconium oxide
- hydroxide gel
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- zirconium
- ceramic
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
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Abstract
The invention discloses a kind of zirconium oxide base metal-ceramic material preparation methods, include the following steps：Step a. makes zirconium hydroxide gel and yttrium hydroxide gel：It takes out suitable lye such as sodium hydroxide, potassium hydroxide, ammonium hydroxide and urea etc. and makees precipitating reagent, from ZrOCl2·8H2Precipitation leaches zirconium hydroxide gel and yttrium hydroxide gel in the salting liquids such as O；Step b. makes zirconia superfine powder：By the zirconium hydroxide gel of leaching and yttrium hydroxide gel, zirconia superfine powder is made by the processes such as being filtered, washed, drying, calcine.A kind of zirconium oxide base metal-ceramic material preparation method; by suitably reducing calcination temperature; protective gas can be blown into simultaneously, and so that particle is formed dust poly- logical to reduce particles form clusters; the precipitation method are during making zirconium oxide micro powder; it is not in agglomeration; zirconium oxide micro powder dispersibility is strong, and sintering activity is high, and zirconium oxide base metal ceramic makees quality height.
Description
Technical field
The present invention relates to zirconia ceramics production equipment technology, specially a kind of zirconium oxide base metal-ceramic material system
Preparation Method.
Background technology
Zirconia ceramics is white, is in yellow or grey when impure, typically contains HfO2, be not readily separated.Under normal pressure
There are three types of crystalline state altogether by pure ZrO2.The production requirement of zirconia ceramics prepares that high-purity, dispersion performance is good, particles ultra fine, size distribution
There are many preparation method of narrow powder, zirconium oxide micro powder, and the purification of zirconium oxide mainly has 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., zirconium oxide is ultra-fine
Powder is most in enterprise produces and processes to use precipitation method processing and fabricating.
But the precipitation method are susceptible to agglomeration during making zirconium oxide micro powder, agglomeration is easy
Zirconium oxide micro powder bad dispersibility is influenced, sintering activity is low, and zirconium oxide base metal ceramic is caused to make poor quality, and produce
Wax embryo dimensioning accuracy is poor, and inside has structure distribution uneven, and die wear is higher, low production efficiency.
Invention content
The purpose of the present invention is to provide a kind of zirconium oxide base metal-ceramic material preparation methods, to solve existing technology
Defect and the requirement of inaccessiable technology.
To achieve the above object, the present invention provides the following technical solutions：A kind of zirconium oxide base metal-ceramic material preparation side
Method includes the following steps：
Step a. makes zirconium hydroxide gel and yttrium hydroxide gel：Take out suitable lye such as sodium hydroxide, hydroxide
Potassium, ammonium hydroxide and urea etc. make precipitating reagent, from ZrOCl2·8H2Precipitation leaches zirconium hydroxide gel and yttrium hydroxide in the salting liquids such as O
Gel；
Step b. makes zirconia superfine powder：By the zirconium hydroxide gel of leaching and yttrium hydroxide gel, by filtering,
Zirconia superfine powder is made in the processes such as washing, dry, calcining；
Step c. makes wax embryo：Zirconia superfine powder and paraffin are put into mixing machine, the rotating speed of mixing machine is 400r/
After min, zirconia superfine powder and paraffin process 2h in mixing machine, slurry is obtained, by slurry under the action of compressed air,
It injects in metal die, then pressurize cools down, and demoulding obtains wax embryo；
Step d. ceramic semi-finished products make：Wax embryo obtains plain embryo after dewaxing under inert powder, and plain embryo, which is put into vacuum, to be burnt
It heats in freezing of a furnace, is finally cooled to room temperature vacuum sintering furnace, ceramic semi-finished product is made；
Step e. polishing moldings：The semi-finished product of ceramic semi-finished product will be made, ceramics are made after correcting check and correction in manually polishing
Ceramic product is put into deionized water and cleans by finished product, after the completion of ceramic product cleaning, is put into dryer and is dried
It is dry.
Preferably, in step b in manufacturing process, the temperature after dry zirconium hydroxide gel and yttrium hydroxide gel detergent is answered
It it is 100-120 DEG C, a length of 2h when dry, calcining equipment therefor is calcining furnace, and calcination temperature is 700-900 DEG C, and when calcining is a length of
30min。
Preferably, step b in the production process, is worked as due to the warm temperature-rise period of calcining and completes amorphous state as crystalline state
Grow up segment at crystal grain has just been started after the process of drinking, and increased with temperature at the diffusion velocity of crystal structure unit in crystal grain and
Increase, particle close to each other is easy to form reunion.
Preferably, in the production process, the temperature in vacuum sintering furnace is first warming up to 400 DEG C to step d, and plain embryo is sintered
Then 3h heats up vacuum sintering furnace 1300 DEG C, by the heat preservation 2h of plain embryo in vacuum sintering furnace, then again by vacuum sintering furnace
350 DEG C are cooled to, vacuum sintering furnace is kept the temperature into 3h.
Preferably, in the production process, dryer temperature is 100-120 DEG C to step e, and drying time period is 3 hours.
Compared with prior art, beneficial effects of the present invention are as follows：
By suitably reducing calcination temperature, while can be blown into protective gas makes particle form dust to reduce granulated
Logical at reuniting, the precipitation method are not in agglomeration, zirconium oxide micro powder point during making zirconium oxide micro powder
It is strong to dissipate property, sintering activity is high, and zirconium oxide base metal ceramic makees quality height, while by by zirconia superfine powder and paraffin
It is put into mixing machine, the rotating speed of mixing machine is that 400r/min is obtained after zirconia superfine powder and paraffin process 2h in mixing machine
It to slurry, by slurry under the action of compressed air, injects in metal die, then pressurize cools down, and demoulding obtains wax embryo, produces
Wax embryo dimensioning accuracy it is stronger, inside has structure distribution uniform, and die wear is relatively low, and production efficiency is high.
Specific implementation mode
Below in conjunction with the present invention, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that
Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.
The present invention provides a kind of technical solution：A kind of zirconium oxide base metal-ceramic material preparation method, includes the following steps：
Step a. makes zirconium hydroxide gel and yttrium hydroxide gel：Take out suitable lye such as sodium hydroxide, hydroxide
Potassium, ammonium hydroxide and urea etc. make precipitating reagent, from ZrOCl2·8H2Precipitation leaches zirconium hydroxide gel and yttrium hydroxide in the salting liquids such as O
Gel；
Step b. makes zirconia superfine powder：By the zirconium hydroxide gel of leaching and yttrium hydroxide gel, by filtering,
Zirconia superfine powder is made in the processes such as washing, dry, calcining；
Step c. makes wax embryo：Zirconia superfine powder and paraffin are put into mixing machine, the rotating speed of mixing machine is 400r/
After min, zirconia superfine powder and paraffin process 2h in mixing machine, slurry is obtained, by slurry under the action of compressed air,
It injects in metal die, then pressurize cools down, and demoulding obtains wax embryo；
Step d. ceramic semi-finished products make：Wax embryo obtains plain embryo after dewaxing under inert powder, and plain embryo, which is put into vacuum, to be burnt
It heats in freezing of a furnace, is finally cooled to room temperature vacuum sintering furnace, ceramic semi-finished product is made；
Step e. polishing moldings：The semi-finished product of ceramic semi-finished product will be made, ceramics are made after correcting check and correction in manually polishing
Ceramic product is put into deionized water and cleans by finished product, after the completion of ceramic product cleaning, is put into dryer and is dried
It is dry.
In step b in manufacturing process, the temperature after dry zirconium hydroxide gel and yttrium hydroxide gel detergent should be 100-
120 DEG C, a length of 2h when dry, calcining equipment therefor is calcining furnace, and calcination temperature is 700-900 DEG C, when calcining a length of 30min.
Step b in the production process, since the warm temperature-rise period of calcining is crystalline state at drinking when complete amorphous state
Cheng Yihou has just started crystal grain and has grown up segment, and increases and increase with temperature at the diffusion velocity of crystal structure unit in crystal grain,
Particle close to each other is easy to form reunion.
In the production process, the temperature in vacuum sintering furnace is first warming up to 400 DEG C to step d, and plain embryo is sintered 3h, then will
Vacuum sintering furnace heats up 1300 DEG C, and by the heat preservation 2h of plain embryo in vacuum sintering furnace, vacuum sintering furnace is then cooled to 350 again
DEG C, vacuum sintering furnace is kept the temperature into 3h.
In the production process, dryer temperature is 100-120 DEG C to step e, and drying time period is 3 hours.
A kind of zirconium oxide base metal-ceramic material preparation method of the present invention, by suitably reducing calcination temperature, while can be with
Being blown into protective gas, so that particle is formed dust poly- logical to reduce particles form clusters, and the precipitation method are making
Be not in agglomeration, zirconium oxide micro powder dispersibility is strong, and sintering is lived during zirconium oxide micro powder
Property it is high, zirconium oxide base metal ceramic makees quality height, while by being put into mixing machine by zirconia superfine powder and paraffin,
The rotating speed of mixing machine is that 400r/min obtains slurry, by slurry after zirconia superfine powder and paraffin process 2h in mixing machine
It under the action of compressed air, injects in metal die, then pressurize cools down, and demoulding obtains wax embryo, the wax embryo size essence of production
True property is stronger, and inside has structure distribution uniform, and die wear is relatively low, and production efficiency is high.
The ceramic material and zirconium oxide base metal-ceramic material preparation method system prepared to general ceramic material preparation method
The ceramic material of work compares, and is experimental data below：
Conclusion：Zirconium oxide base metal-ceramic material that the present invention makes compares ceramic material, in performance in all fields
All it is remarkably enhanced.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of zirconium oxide base metal-ceramic material preparation method, it is characterised in that：Include the following steps：
Step a. makes zirconium hydroxide gel and yttrium hydroxide gel：Take out suitable lye such as sodium hydroxide, potassium hydroxide, ammonia
Water and urea etc. make precipitating reagent, from ZrOCl2·8H2Precipitation leaches zirconium hydroxide gel and yttrium hydroxide gel in the salting liquids such as O；
Step b. makes zirconia superfine powder：By the zirconium hydroxide gel of leaching and yttrium hydroxide gel, by filtering, washing
It the processes such as washs, dry, calcining and zirconia superfine powder is made；
Step c. makes wax embryo：Zirconia superfine powder and paraffin are put into mixing machine, the rotating speed of mixing machine is 400r/min,
After zirconia superfine powder and paraffin process 2h in mixing machine, slurry is obtained, by slurry under the action of compressed air, injection
In metal die, then pressurize cools down, and demoulding obtains wax embryo；
Step d. ceramic semi-finished products make：Wax embryo obtains plain embryo after dewaxing under inert powder, and plain embryo is put into vacuum sintering furnace
Vacuum sintering furnace, is finally cooled to room temperature by middle heating, and ceramic semi-finished product is made；
Step e. polishing moldings：The semi-finished product of ceramic semi-finished product being made, ceramic product is made after correcting check and correction in manually polishing,
Ceramic product is put into deionized water and is cleaned, after the completion of ceramic product cleaning, is put into dryer and is dried.
2. a kind of zirconium oxide base metal-ceramic material preparation method according to claim 1, it is characterised in that：In step b
In manufacturing process, dries the temperature after zirconium hydroxide gel and yttrium hydroxide gel detergent and should be 100-120 DEG C, it is a length of when drying
2h, calcining equipment therefor are calcining furnace, and calcination temperature is 700-900 DEG C, when calcining a length of 30min.
3. a kind of zirconium oxide base metal-ceramic material preparation method according to claim 1, it is characterised in that：Step b exists
In manufacturing process, since the warm temperature-rise period of calcining is crystalline state at just having started crystalline substance after the process of drinking when completing amorphous state
The big segment of grain length, and increase and increase with temperature at the diffusion velocity of crystal structure unit in crystal grain, particle close to each other holds
It is easily formed and is reunited.
4. a kind of zirconium oxide base metal-ceramic material preparation method according to claim 1, it is characterised in that：Step d exists
In manufacturing process, the temperature in vacuum sintering furnace is first warming up to 400 DEG C, and plain embryo is sintered 3h, then vacuum sintering furnace heats up
1300 DEG C, by the heat preservation 2h of plain embryo in vacuum sintering furnace, vacuum sintering furnace is then cooled to 350 DEG C again, by vacuum-sintering
Stove keeps the temperature 3h.
5. a kind of zirconium oxide base metal-ceramic material preparation method according to claim 1, it is characterised in that：Step e exists
In manufacturing process, dryer temperature is 100-120 DEG C, and drying time period is 3 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111574222A (en) * | 2020-05-17 | 2020-08-25 | 陕西励峰德精密陶瓷科技有限公司 | Technology for preparing ceramic rear cover through grouting |
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|---|---|---|---|---|
| CN102674834A (en) * | 2012-05-22 | 2012-09-19 | 江西理工大学 | Preparation method of zirconium oxide structural ceramics |
| CN102976762A (en) * | 2012-11-07 | 2013-03-20 | 洛阳北苑特种陶瓷有限公司 | Method for preparing zirconia ceramic product |
| KR101248855B1 (en) * | 2010-12-23 | 2013-03-29 | 한국교통대학교산학협력단 | Preparation method for ultrafine powders of zirconia by precipitation method |
| CN105272226A (en) * | 2015-10-28 | 2016-01-27 | 金业新材料科技(昆山)有限公司 | Preparation method of composite stabilized zirconia feed for injection molding by thermal release |
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2018
- 2018-06-12 CN CN201810600248.XA patent/CN108727015A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101248855B1 (en) * | 2010-12-23 | 2013-03-29 | 한국교통대학교산학협력단 | Preparation method for ultrafine powders of zirconia by precipitation method |
| CN102674834A (en) * | 2012-05-22 | 2012-09-19 | 江西理工大学 | Preparation method of zirconium oxide structural ceramics |
| CN102976762A (en) * | 2012-11-07 | 2013-03-20 | 洛阳北苑特种陶瓷有限公司 | Method for preparing zirconia ceramic product |
| CN105272226A (en) * | 2015-10-28 | 2016-01-27 | 金业新材料科技(昆山)有限公司 | Preparation method of composite stabilized zirconia feed for injection molding by thermal release |
Non-Patent Citations (1)
| Title |
|---|
| 陈木青等: "《材料物理实验教程》", 28 February 2018, 华中科技大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111574222A (en) * | 2020-05-17 | 2020-08-25 | 陕西励峰德精密陶瓷科技有限公司 | Technology for preparing ceramic rear cover through grouting |
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Application publication date: 20181102 |