CN107827457A - A kind of preparation method of porous oxidation zircon ceramic - Google Patents
A kind of preparation method of porous oxidation zircon ceramic Download PDFInfo
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- CN107827457A CN107827457A CN201711361658.5A CN201711361658A CN107827457A CN 107827457 A CN107827457 A CN 107827457A CN 201711361658 A CN201711361658 A CN 201711361658A CN 107827457 A CN107827457 A CN 107827457A
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- 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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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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Abstract
The invention discloses a kind of preparation method of porous oxidation zircon ceramic, is first well mixed zirconium oxide and yittrium oxide by weight ratio and prepares compound；Then the POLYPROPYLENE GLYCOL aqueous solution and aqueous ammonium chloride solution are prepared：Gained compound and solution are put into ball mill together and carry out ball milling；Binding agent, starch solution, surfactant are added into the slurry after ball milling, continues ball milling 30min；10% aqueous ammonium chloride solution is added afterwards, and lower ball milling 3min, pours into rapidly die for molding at a high speed；Slurry in mould and mould is put into baking oven and foamed；It is then placed in household freezer and freezes, forms gel；Gel sample is stripped, sintered after drying, obtains porous oxidation zircon ceramic.The present invention improves adhesion strength, reduces pollution, obtained porous zirconia ceramics porosity is high, uniform pore diameter, improves the performance of porous oxidation zircon ceramic by the use of trbasic zinc phosphate as binding agent.
Description
Technical field
The present invention relates to porous ceramic technology field, and in particular to a kind of preparation method of porous oxidation zircon ceramic.
Background technology
Porous ceramics is due to having good mechanical performance, chemically and thermally stability concurrently, as a kind of its filtering of green material
Performance extensive use.Zirconia material has excellent physics, chemical property, and making porous material with zirconia material can be simultaneous
Have good mechanical performance, chemically and thermally stability and selection oxygen permeability.
The preparation method of porous ceramics have it is a variety of, such as：Add pore creating material method, organic foam method and foaming.
Addition pore creating material method be using organic pore-forming agents at high temperature after-flame or volatilization and hole is left in ceramic body,
This method technique is simple, adjustable porosity section, but porosity is low, can be discharged pollutants in preparation process.
Organic foam method is the special construction using the three-dimensional netted skeleton of perforate possessed by organic foam, by what is prepared
Slurry is evenly coated on organic foam reticulate body, is burnt up Organic Foam Material after drying and is obtained a kind of screen like and porous ceramic.
The intensity of organism and elasticity have a significant impact to the structure and performance of porous material in this method preparation process, are also easy to produce simultaneously
Remained mass and toxic gas, are polluted to environment.
Porous ceramics hole rate prepared by foaming can typically be more than 70%, and it is organic that foaming can typically add some
Thing, in ceramic slurry foaming solidify afterwards slurry, these have an opportunity all burn in sintering or volatilization, pollute environment.
It is not high porosity to be present in the above method, the problem of discharging pollutants.
The content of the invention
The present invention is intended to provide a kind of preparation method of porous oxidation zircon ceramic, by the use of trbasic zinc phosphate as binding agent, is enhanced
The adaptability of binding agent and zirconia ceramics, adhesion strength is improved, and reduce pollution, done pore creating material with starch, obtain
Porous zirconia ceramics porosity it is high, can reach more than 80%, uniform pore diameter, without obvious especially big hole, using mesopore as
It is main, improve the performance of porous oxidation zircon ceramic.
The object of the invention to solve the technical problems is realized using following technical scheme.Itd is proposed according to the present invention
A kind of porous oxidation zircon ceramic preparation method, comprise the following steps：
(1) zirconium oxide compound is prepared：Zirconium oxide powder and yttrium oxide powder are well mixed according to weight proportion first；
(2) the POLYPROPYLENE GLYCOL aqueous solution is prepared：POLYPROPYLENE GLYCOL is mixed according to a certain percentage with deionized water, prepares polychlorostyrene third
The enol aqueous solution；
(3) aqueous ammonium chloride solution is prepared：With pure ammonium chloride is analyzed the chlorine that mass fraction is 15% is configured to deionized water
Change aqueous ammonium；
(4) slurry is prepared：Compound obtained by step (1)-(3) and solution are put into ball mill together, place into corundum
Ball, ball milling 3h, obtains slurry；
(5) binding agent is added into the slurry after ball milling, and adds the starch solution that mass fraction is 3%, is added simultaneously
Surfactant, then proceed to ball milling 30min；The aqueous ammonium chloride solution that a certain amount of mass fraction is 10% is added afterwards, then
Ball milling 3min at high speeds, pour into die for molding rapidly afterwards；
(6) slurry in mould and mould is put into baking oven and foamed；Then the slurry in mould and mould is put
Enter and 8h is freezed in household freezer, the temperature of freezing is subzero 15 degree, and gel is formed in refrigerating process；
(7) gel sample is stripped, gel sample is then put into 10h in ethanol water；
(8) gel sample is taken out from ethanol solution, 3h is sintered under argon atmospher protection after drying, after sintering
Room temperature is naturally cooled to, obtains porous oxidation zircon ceramic.
The object of the invention to solve the technical problems can be also applied to the following technical measures to achieve further.
A kind of preparation method of foregoing porous oxidation zircon ceramic, wherein, step (1) Zirconium oxide powder and yittrium oxide
The weight ratio of powder is 20:1.
A kind of preparation method of foregoing porous oxidation zircon ceramic, wherein, step (2) presses POLYPROPYLENE GLYCOL and deionized water
After being mixed according to certain proportion, in 70 degrees Celsius of lower ultrasonic disperse 1h, the POLYPROPYLENE GLYCOL aqueous solution that mass fraction is 10% is configured to.
A kind of preparation method of foregoing porous oxidation zircon ceramic, wherein, step (5) binding agent bonds for trbasic zinc phosphate
Agent, the addition of the trbasic zinc phosphate binding agent are the 2-6% of step (1) zirconium oxide mixture quality.
A kind of preparation method of foregoing porous oxidation zircon ceramic, wherein, the surfactant described in step (5) is 12
Sodium alkyl sulfate, the addition of lauryl sodium sulfate are the 2-4% of step (1) zirconium oxide mixture quality.
A kind of preparation method of foregoing porous oxidation zircon ceramic, wherein, the addition of step (5) described aqueous ammonium chloride solution
Measure as the 3-5% of step (1) zirconium oxide mixture quality.
A kind of preparation method of foregoing porous oxidation zircon ceramic, wherein, step (6) oven temperature is 90 DEG C, during foaming
Between be 2h.
A kind of preparation method of foregoing porous oxidation zircon ceramic, wherein, the temperature that step (8) is dried is 120 DEG C, is dried
Time be 12h, described sintering temperature is 1600 DEG C.
The present invention enhances the adaptability of binding agent and zirconia ceramics, improves bonding by the use of trbasic zinc phosphate as binding agent
Intensity, and pollution is reduced, pore-creating is carried out using starch solution, does not produce pernicious gas, and obtained porous zirconia
Ceramic porosity is high, can reach more than 80%, and uniform pore diameter, without obvious especially big hole, based on mesopore, improves more
The performance of hole zirconia ceramics, its compressive resistance can reach 2.2MPa.
Embodiment
Illustrate the present invention referring to specific embodiment.These embodiments are merely to illustrate the present invention, its not with appoint
Where formula limits the scope of the present invention.
The invention provides a kind of preparation method of porous oxidation zircon ceramic, 8 steps are specifically divided into：
(1) zirconium oxide compound is prepared：According to weight ratio it is 20 first by Zirconium oxide powder and yttrium oxide powder:1 ratio
Example is well mixed；
(2) the POLYPROPYLENE GLYCOL aqueous solution is prepared, POLYPROPYLENE GLYCOL is mixed according to a certain percentage with deionized water, in 70 degrees Celsius
Lower ultrasonic disperse 1h, prepare the POLYPROPYLENE GLYCOL aqueous solution that mass fraction is 10%；
(3) aqueous ammonium chloride solution is prepared：With pure ammonium chloride is analyzed the chlorine that mass fraction is 15% is configured to deionized water
Change aqueous ammonium；
(4) slurry is prepared：Compound obtained by step (1)-(3) and solution are put into ball mill together, place into corundum
Ball, ball milling 3h, obtains slurry；
(5) trbasic zinc phosphate is added into the slurry after ball milling, the addition of the trbasic zinc phosphate is step (1) zirconium oxide compound matter
The 2-6% of amount, and starch solution that mass fraction is 3% is added as pore creating material, while add lauryl sodium sulfate conduct
Surfactant, then proceed to ball milling 30min；The aqueous ammonium chloride solution that a certain amount of mass fraction is 10% is added afterwards, now,
The addition of aqueous ammonium chloride solution accounts for the 3-5% of step (1) zirconium oxide mixture quality, then ball milling 3min at high speeds, fast
Speed pours into die for molding；
(6) slurry in mould and mould is put into baking oven and foamed, starch solution pore-creating in the slurry, baking oven temperature
Spend for 90 degree, foamed time 2h；Then the slurry in mould and mould is put into household freezer and freezes 8h, the temperature of freezing is
Subzero 15 degree；Gel is formed in refrigerating process；
(7) gel sample is stripped, gel sample is then put into 12h in ethanol water, it is replaced with ethanol
In moisture content, avoid the later stage dry and sintering process in moisture evaporation cause sample to shrink.
(8) gel sample is taken out from ethanol, 12h is dried at 120 DEG C, is then sintered under nitrogen atmosphere protection
3h, sintering temperature are 1600 DEG C.Room temperature is naturally cooled to after sintering, obtains porous oxidation zircon ceramic.
After tested, the porosity of gained porous oxidation zircon ceramic is 85%, compression strength 2.2MPa.
The above described is only a preferred embodiment of the present invention, any formal limitation not is done to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit according to the present invention
To any simple modification, equivalent change and modification made for any of the above embodiments, in the range of still falling within technical solution of the present invention.
Claims (8)
1. a kind of preparation method of porous oxidation zircon ceramic, it is characterised in that comprise the following steps：
(1) zirconium oxide compound is prepared：Zirconium oxide powder and yttrium oxide powder are well mixed according to weight proportion first；
(2) the POLYPROPYLENE GLYCOL aqueous solution is prepared：POLYPROPYLENE GLYCOL is mixed according to a certain percentage with deionized water, prepares polychloroprene alcohol
The aqueous solution；
(3) aqueous ammonium chloride solution is prepared：With pure ammonium chloride is analyzed the ammonium chloride that mass fraction is 15% is configured to deionized water
The aqueous solution；
(4) slurry is prepared：Compound obtained by step (1)-(3) and solution are put into ball mill together, place into corundum ball, ball
3h is ground, obtains slurry；
(5) binding agent is added into the slurry after ball milling, and adds mass fraction and is 3% starch solution, while adds surface
Activating agent, then proceed to ball milling 30mi n；The aqueous ammonium chloride solution that a certain amount of mass fraction is 10% is added afterwards, then in height
The lower ball milling 3mi n of speed, pour into rapidly die for molding afterwards；
(6) slurry in mould and mould is put into baking oven and foamed；Then the slurry in mould and mould is put into cold
Freeze in case and freeze 8h, the temperature of freezing is subzero 15 degree, and gel is formed in refrigerating process；
(7) gel sample is stripped, gel sample is then put into 10h in ethanol water；
(8) gel sample is taken out from ethanol solution, is sintered 3h under argon atmospher protection after drying, it is natural after sintering
Room temperature is cooled to, obtains porous oxidation zircon ceramic.
2. the method as described in claim 1, it is characterised in that：The weight of step (1) Zirconium oxide powder and yttrium oxide powder
Amount is than being 20:1.
3. the method as described in claim 1, it is characterised in that：Step (2) is by POLYPROPYLENE GLYCOL and deionized water according to certain ratio
After example mixing, in 70 degrees Celsius of lower ultrasonic disperse 1h, the POLYPROPYLENE GLYCOL aqueous solution that mass fraction is 10% is configured to.
4. the method as described in claim 1, it is characterised in that：Step (5) described binding agent is trbasic zinc phosphate binding agent, the phosphoric acid
The addition of zinc binding agent is the 2-6% of step (1) zirconium oxide mixture quality.
5. the method as described in claim 1, it is characterised in that：Surfactant described in step (5) is dodecyl sulphate
Sodium, the addition of lauryl sodium sulfate are the 2-4% of step (1) zirconium oxide mixture quality.
6. the method as described in claim 1, it is characterised in that：The addition of step (5) described aqueous ammonium chloride solution is step
(1) 3-5% of zirconium oxide mixture quality.
7. the method as described in claim 1, it is characterised in that：Step (6) oven temperature is 90 DEG C, foamed time 2h.
8. the method as described in claim 1, it is characterised in that：The temperature that step (8) is dried is 120 DEG C, and the dry time is
12h, described sintering temperature are 1600 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109608193A (en) * | 2018-12-10 | 2019-04-12 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of high-purity zirconia light-weight refractory aggregate and preparation method thereof |
| CN113068991A (en) * | 2021-03-03 | 2021-07-06 | 葛亚国 | Electromagnetic heating low-noise stainless steel pot and manufacturing method thereof |
| CN115849440A (en) * | 2023-01-29 | 2023-03-28 | 宁波卿甬新材料科技有限公司 | Preparation method of porous zirconia |
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| CN102424603A (en) * | 2011-09-07 | 2012-04-25 | 陕西理工学院 | Method for preparing zirconia gradient porous ceramics with ice as template |
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Patent Citations (2)
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| CN102424603A (en) * | 2011-09-07 | 2012-04-25 | 陕西理工学院 | Method for preparing zirconia gradient porous ceramics with ice as template |
| CN107188610A (en) * | 2017-06-01 | 2017-09-22 | 洛阳师范学院 | A kind of preparation method of porous silicon carbide ceramic |
Non-Patent Citations (1)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109608193A (en) * | 2018-12-10 | 2019-04-12 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of high-purity zirconia light-weight refractory aggregate and preparation method thereof |
| CN109608193B (en) * | 2018-12-10 | 2021-01-22 | 中钢集团洛阳耐火材料研究院有限公司 | High-purity zirconia light refractory aggregate and preparation method thereof |
| CN113068991A (en) * | 2021-03-03 | 2021-07-06 | 葛亚国 | Electromagnetic heating low-noise stainless steel pot and manufacturing method thereof |
| CN113068991B (en) * | 2021-03-03 | 2022-08-23 | 宁波喜尔美厨房用品有限公司 | Electromagnetic heating low-noise stainless steel pot and manufacturing method thereof |
| CN115849440A (en) * | 2023-01-29 | 2023-03-28 | 宁波卿甬新材料科技有限公司 | Preparation method of porous zirconia |
| CN115849440B (en) * | 2023-01-29 | 2023-06-23 | 宁波卿甬新材料科技有限公司 | Preparation method of porous zirconia |
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Application publication date: 20180323 |