CN109336584A - The preparation method and TZO material of TZO ceramic coating material - Google Patents
The preparation method and TZO material of TZO ceramic coating material Download PDFInfo
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Abstract
The preparation method and TZO material of TZO ceramic coating material.The invention belongs to field of new materials, and in particular to a kind of preparation method of TZO material, comprising: preparation TZO raw material；Biscuit is prepared by TZO raw material；And by biscuit densified sintering product, the TZO material is formed, have the characteristics that film even compact, transmitance are high, performance is stable.Transmitance not only can be improved in preparation method of the invention, is further adapted for the application of the energy-saving glass industry of large-area coating film.
Description
Technical field
The present invention relates to field of new materials, and in particular to a kind of preparation method and TZO material of TZO ceramic coating material.
Background technique
According to statistics, nearly 50% building thermal energy is scattered and disappeared by door and window, and the use of energy-saving glass is the weight of building energy conservation
It is big to improve.Currently, energy-saving glass reaches 92% in the utilization rate of Germany, the U.S. 90%, Japan is 85%, Chinese utilization rate
Less than 10%.National requirements is to the year two thousand twenty, and newly-increased to build the target for reaching energy conservation 65%, there is energy-saving glass greatly application to dive
Power.
But with the raising of energy-saving glass technical standard, height of the shading coefficient less than 0.2, transmitance greater than 80% is thoroughly
LOW-E glass will gradually become mainstream, and traditional low-e properties of product have been unable to satisfy requirement.
The transmitance for being made into energy-saving glass using sputter materials such as Zinc-tin alloy, allumen, zinc oxide aluminums at present is general
70% or so.
Based on this, the application provides a kind of ZnO+SnO2The preparation method of (abbreviation TZO) semiconductor coated film material, system
Standby semiconductor material can be made of magnetron sputtering mode LOW-E can tempering energy-saving glass, the rate of passing it through reaches 85%
More than.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of TZO material and TZO materials, to improve transmitance.
In order to solve the above-mentioned technical problems, the present invention provides a kind of preparation methods of TZO material, comprising: preparation TZO is former
Material；Biscuit is prepared by TZO raw material；By biscuit densified sintering product, the TZO material is formed.
Further, it includes: first by ZnO powder and SnO that the preparation TZO raw material, which obtains method,2Powder mixing；It adds appropriate
Deionized water, additive and organic additive, ball milling obtain slurry；And last spray drying granulation processing, obtain TZO raw material.
Further, the ZnO powder is 50-90 parts by weight；The SnO2Powder is 10-50 parts by weight；And the ZnO
Powder and SnO2The partial size of powder is 0.01-20 μm.Wherein, the purity of the ZnO powder is at least 99.97%；SnO2Powder
Purity be at least 99.9%.
Further, the additive includes Al2O3Powder, AlF3Powder, Ga2O3Powder, In2O3One of powder is several
Kind；The additive is 0.1-0.5 parts by weight.
Further, the organic additive includes one or more of poly amic acid, polyvinyl alcohol.
Further, the biscuit is suitable for by by TZO raw material casting or cold isostatic compaction；The phase of the biscuit
50% is at least to density.
Further, biscuit is sintered 1-6h in 1000-1500 DEG C of air or argon gas atmosphere stove, is obtained by processing described
TZO material；Wherein, the relative density of the TZO material is 95% or more.
On the other hand, the present invention also provides a kind of preparation methods of TZO raw material, comprising: first by ZnO powder and SnO2Powder
Body mixing；Appropriate amount of deionized water, additive and organic additive are added, ball milling obtains slurry；And last spray drying granulation
Processing, obtains TZO raw material.
Further, the ZnO powder is 50-90 parts by weight；The SnO2Powder is 10-50 parts by weight；The ZnO powder
And SnO2The partial size of powder is 0.1-20 μm；The additive includes Al2O3Powder, AlF3Powder, Ga2O3Powder, In2O3Powder
One or more of body；The additive is 0.1-0.5 parts by weight；And the organic additive includes poly amic acid, gathers
One or more of vinyl alcohol.
Another aspect, the present invention also provides a kind of TZO material, the TZO material is suitable for by preparing as previously described
Method preparation.
The invention has the advantages that preparation method of the invention prepares biscuit by TZO raw material；Biscuit is sintered and is caused
It is close, the TZO material is formed, has the characteristics that film even compact, transmitance are high, performance is stable.Transmission not only can be improved
Rate is further adapted for the application of the energy-saving glass industry of large-area coating film.
Specific embodiment
Embodiment 1
Weighing purity is 4N (purity 99.99%), 1.0 μm of average grain diameter of 500g ZnO powder and 5 μm of average grain diameter
500g SnO2Powder simultaneously mixes.1 μm of average grain diameter of 1g AlF is first added3Powder adds the deionization pure water of 450g and fits
It measures organic additive (poly amic acid of 5g and the polyvinyl alcohol of 4g), with ball mill ball milling mixing 2h or more, slurry spray drying
Granulation processing obtains the TZO raw material that average grain diameter is 50 μm.Relative density is obtained using the pressure forming of isostatic cool pressing 200Mp
Biscuit greater than 60%, by this biscuit, 450 DEG C of heat preservation 14h remove organic additive in air furnace, are then warming up to 1450 DEG C
Densified sintering product obtains the TZO material of relative density 95%.
Embodiment 2
Weighing purity is 4N (purity 99.99%), 1.0 μm of average grain diameter of 900g ZnO powder and 5 μm of average grain diameter
100g SnO2Powder simultaneously mixes.1 μm of average grain diameter of 5g AlF is first added3Powder adds the deionization pure water of 450g and fits
It measures organic additive (poly amic acid of 5g and the polyvinyl alcohol of 4g), with ball mill ball milling mixing 2h or more, dried 100 mesh
Sieve, being then charged into internal diameter 120mm has the high-strength graphite mold of BN coating, 1000 DEG C of hot pressed sintering 1h in hot pressing furnace, cooling
Demoulding machining obtains the TZO material (diameter 76mm, thickness 6mm) of relative density 95%.
Embodiment 3
Pure water, methyl acrylamide monomer, N-N bismethacrylamide is sufficiently molten with the ratio of 100:13-20:0.6-1
Solution composition premixed liquid, does dispersing agent with suitable tetramethyl aqua ammonia (0.1-1.5%).Weighing purity is 4N, average grain diameter 2
μm ZnO powder 1000g, be added 5 μm of SnO of weight 650g average grain diameter2Powder is added in above-mentioned premixed liquid.Add weight 5g
1 μm of AlF of average grain diameter3Powder, stirring pulping；Wherein, in slurry powder solid concentration 55-65%.The slurry made is fallen
In goal mould machine, medium is done with zirconia ball, ball milling 12h or more adds organic degasser such as n-butanol of 0.1-1% volume
And the ‰ tetramethylethylenediamine catalyst of 0.1-1.5wt of slurry gross weight and ‰ ammonium persulfate of 0.01-0.5wt of slurry gross weight cause
Agent, stirring degassing 10 minutes, sieve with 100 mesh sieve in de-airing mixer, are poured into the non-porous mold of diameter 150mm, and wet green body is solid
After changing demoulding, dry to obtain highdensity TZO biscuit in an oven through 60-110 DEG C.450 DEG C of heat preservation 4h in air furnace
After removing organic additive, it is continuously heating to 1480 DEG C of sintering 6h and is slowly dropped to room temperature.Machining obtains relative density 99%TZO
Material (diameter 76mm, thickness 6mm).
Embodiment 4
The preparation method of the application passes through to TZO raw material proportioning (ZnO powder and SnO2Powder quality ratio), TZO raw material prepare work
Skill, the factors such as biscuit preparation process, sintering temperature are probed into, and are improved the transmitance and stability of TZO material, are especially adapted to
The application of the energy-saving glass industry of large-area coating film.As space is limited, some embodiments are only only listed in embodiment 1-3,
The major parameter of other embodiment is as shown in table 1, and specific implementation process is referring to associated description in embodiment 1-3.
Major parameter in 1 preparation method of table.
Embodiment 5
Coating performance test is done to the TZO material of the preparation method preparation of the application: the DC magnetic in SIM560 magnetron sputter
Control plated film, power 100W, Ar2Pressure 0.6Pa, glass substrate temperature room temperature, sputtering process stablize easily-controllable splash.Conclusion is as follows:
TZO material prepared by embodiment 1 XP-1 step instrument measurement measures 400 nanometers of film thickness, CARY-100 light splitting
The visible light transmittance that photometer measures 400-700 nanometers is greater than 90%, film 300 DEG C of heating 1h in air, or 90%
100 degree of heating 2h in humidity box, transmitance is substantially unchanged, high comprehensive performance.
TZO material prepared by embodiment 2 XP-1 step instrument measurement measures 200 nanometers of film thickness, CARY-100 light splitting
The visible light transmittance that photometer measures 400-700 nanometers is greater than 90%, film 300 DEG C of heating 1h in air, or 90%
100 degree of heating 2h in humidity box, transmitance is substantially unchanged, film high comprehensive performance.
TZO material prepared by embodiment 3 XP-1 step instrument measurement measures 100 nanometers of film thickness, CARY-100 light splitting
The visible light transmittance that photometer measures 400-700 nanometers is greater than 93%, film 300 DEG C of heating 1h in air, or 90%
100 degree of heating 2h, high comprehensive performance in humidity box.
Embodiment 6
To TZO material manufactured by embodiment 1-3, according to Film Design: glass substrate-TZO-Ag- nickel chromium triangle-silicon nitride-TZO-
Ag- silicon nitride-TZO；Double-silver LOW-E glass sample is manufactured, after 420-470 degree tempering, is measured with CARY-100 spectrophotometric
Obtaining transmitance is respectively 89%, 84%, 90%, and comprehensive performance is superior to double silver products currently on the market.
In conclusion the transmitance that TZO material can be improved in the preparation method of the application is high, make its even compact, performance
Stablize, while being suitable for the application of the energy-saving glass industry of large-area coating film.In addition, TZO material prepared by the preparation method of the application
Material also has the advantage that relative to materials such as traditional Zinc-tin alloy, allumen, zinc oxide aluminums
(1) bulk resistor Shuai≤8 × 10-3 Ω .cm, can be used for magnetron sputtering production can tempering energy-saving glass, transmitance is up to 85%
More than, even as high as 93%.
(2) it can be used for magnetron sputtering production energy-saving glass, d.c. sputtering or alternating-current pulse sputtering can be produced, be sputtered
Rate is high, and production efficiency improves 15% or more.
(3) energy-saving glass is produced by TZO material, process is easier to control, straight argon sputtering, does not need to adjust in sputtering process
Whole partial pressure of oxygen；The target position number for reducing equipment simultaneously, the requirement to production equipment reduce, so that manufacture is double in single silver production equipment
Silver products are possibly realized, and reduce production equipment investment.
(4) the film even compact manufactured by TZO material, in wet air, thin in oxygen or in reducing atmosphere
The stability of film properties is very good, this performance is significantly better than to be manufactured using Zinc-tin alloy, allumen, zinc-tin oxide
Film, the following application range are more extensive.
(5) it is better than the other materials of current open source information report by the energy-saving glass comprehensive performance that TZO material manufactures, especially
It is the application for being suitable for the energy-saving glass industry of large-area coating film.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (10)
1. a kind of preparation method of TZO material characterized by comprising
Prepare TZO raw material；
Biscuit is prepared by TZO raw material；And
By biscuit densified sintering product, the TZO material is formed.
2. preparation method according to claim 1, which is characterized in that
The preparation TZO raw material obtains method and includes:
First by ZnO powder and SnO2Powder mixing；
Appropriate amount of deionized water, additive and organic additive are added, ball milling obtains slurry；And
Last spray drying granulation processing, obtains TZO raw material.
3. preparation method according to claim 2, which is characterized in that
The ZnO powder is 50-90 parts by weight；
The SnO2Powder is 10-50 parts by weight；And
The ZnO powder and SnO2The partial size of powder is 0.1-20 μm.
4. preparation method according to claim 2, which is characterized in that
The additive includes Al2O3Powder, AlF3Powder, Ga2O3Powder, In2O3One or more of powder；
The additive is 0.1-0.5 parts by weight.
5. preparation method according to claim 2, which is characterized in that
The organic additive includes one or more of poly amic acid, polyvinyl alcohol.
6. preparation method according to claim 1, which is characterized in that
The biscuit is suitable for by by TZO raw material casting or cold isostatic compaction；
The relative density of the biscuit is at least 50%.
7. preparation method according to claim 1, which is characterized in that
Biscuit is sintered 1-6h in 1000-1500 DEG C of air or argon gas atmosphere stove, obtains the TZO material by processing.
8. a kind of preparation method of TZO raw material characterized by comprising
First by ZnO powder and SnO2Powder mixing；
Appropriate amount of deionized water, additive and organic additive are added, ball milling obtains slurry；And
Last spray drying granulation processing, obtains TZO raw material.
9. preparation method according to claim 7, which is characterized in that
The ZnO powder is 50-90 parts by weight；
The SnO2Powder is 10-50 parts by weight；
The ZnO powder and SnO2The partial size of powder is 0.1-20 μm；
The additive includes Al2O3Powder, AlF3Powder, Ga2O3Powder, In2O3One or more of powder；
The additive is 0.1-0.5 parts by weight；And
The organic additive includes one or more of poly amic acid, polyvinyl alcohol.
10. a kind of TZO material, which is characterized in that
The TZO material is suitable for preparing by preparation method as described in claim 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101038796A (en) * | 2006-03-15 | 2007-09-19 | 住友金属矿山株式会社 | Oxide sintered body, manufacturing method therefor, manufacturing method for transparent conductive film using the same, and resultant transparent conductive film |
| CN104087906A (en) * | 2014-07-29 | 2014-10-08 | 林嘉佑 | Preparation technology of ZnSnOx ceramic target and method for preparing ZnSnOx coated film by using same |
| CN105272210A (en) * | 2015-11-18 | 2016-01-27 | 南京迪纳科光电材料有限公司 | Preparation method of TZO semiconductor material for high-transmittance energy-saving glass |
| CN108046767A (en) * | 2017-12-08 | 2018-05-18 | 郑州大学 | A kind of method for preparing oxide ceramics target material blank body |
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2018
- 2018-11-13 CN CN201811349096.7A patent/CN109336584A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101038796A (en) * | 2006-03-15 | 2007-09-19 | 住友金属矿山株式会社 | Oxide sintered body, manufacturing method therefor, manufacturing method for transparent conductive film using the same, and resultant transparent conductive film |
| CN104087906A (en) * | 2014-07-29 | 2014-10-08 | 林嘉佑 | Preparation technology of ZnSnOx ceramic target and method for preparing ZnSnOx coated film by using same |
| CN105272210A (en) * | 2015-11-18 | 2016-01-27 | 南京迪纳科光电材料有限公司 | Preparation method of TZO semiconductor material for high-transmittance energy-saving glass |
| CN108046767A (en) * | 2017-12-08 | 2018-05-18 | 郑州大学 | A kind of method for preparing oxide ceramics target material blank body |
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