CN102760509A - ITO (Indium Tin Oxide) nanocrystal aqueous dispersion liquid and preparation method thereof - Google Patents
ITO (Indium Tin Oxide) nanocrystal aqueous dispersion liquid and preparation method thereof Download PDFInfo
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- CN102760509A CN102760509A CN2011101080866A CN201110108086A CN102760509A CN 102760509 A CN102760509 A CN 102760509A CN 2011101080866 A CN2011101080866 A CN 2011101080866A CN 201110108086 A CN201110108086 A CN 201110108086A CN 102760509 A CN102760509 A CN 102760509A
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Abstract
The invention discloses an ITO (Indium Tin Oxide) nanocrystal aqueous dispersion liquid and a preparation method thereof. The pure and stable ITO aqueous dispersion liquid with high solid content is prepared by adopting a simple hydrothermal synthesis and post treatment process, a sanding-ultrasonication-high-speed centrifugation optimization process for post treatment, and no additives. The aqueous dispersion liquid has the advantages that the aqueous dispersion liquid is high in purity and solid content, good in transparency and conductivity and stable in storage, is not condensed or settled, and the like. The application scope of the aqueous dispersion liquid is widened, and an excellent raw material is provided for studying the structures, synthesis mechanisms and aqueous dispersion mechanisms of crystalline nanomaterials.
Description
Technical field
The present invention relates to the manufacturing technology field of the brilliant conducting function material of transparent nano, is to use hydrothermal synthesis method to make ITO nano crystalline water dispersion and preparation method thereof specifically.
Background technology
At present; Common electric conducting material such as metal and graphite etc. all are opaque materials; The modern high technology technical field needs the new material of a large amount of not only transparent but also conduction; At present existing antimony oxide and tin ash (ATO) and indium sesquioxide and tin ash (ITO) transparent conductive material, these materials often contain impurity, particle diameter is big, solids content is low, unstable and easy cohesion and sedimentation when depositing, and should not be applied to the technical field of specific (special) requirements; In order to address these problems, people also begin one's study and produce nano level ITO material, adapting to the technical field of specific (special) requirements, like technical fields such as the antistatic of OLED display, EL luminous plaque, solar panel and glass, anti-dazzle, radiation proofs; But present nano level ITO material; Its preparation method commonly used is: 1, hydroxide co-precipitation-filtration washing-high-temperature roasting-broken classification; The disadvantage of this method is a very difficulty of broken classification, and the rate of recovery is low, and cost is high; And when making aqueous dispersion, need add a large amount of auxiliary agents, therefore the scope of application also is restricted; 2, hydroxide heavy altogether-filtration washing-hydro-thermal is synthetic-broken classification; The advantage of this method is that broken size scale is easier to; Shortcoming is mostly at the synthetic auxiliary agent that has added beyond the eutectic thing of hydro-thermal; Do not solve " segregation " problem, problems such as transparency is not high, conductivity is bad, bin stability difference often occur.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art, and a kind of ITO nano crystalline water dispersion is provided.
Another object of the present invention provides a kind of ITO nano crystalline water dispersion and preparation method thereof.
The present invention solved mainly that existing transparent conductive material contains impurity, particle diameter is big, solids content is low, unstable and be prone to problems such as cohesion and sedimentation when depositing.
In order to achieve the above object, the present invention is achieved in that the ITO nano crystalline water dispersion, is stannic chloride pentahydrate and indium trichloride are dissolved in the isopropyl alcohol; With in the above-mentioned solution impouring boiling water, be neutralized to neutrality again, be incubated 1 hour with ammoniacal liquor; After placing cooling, filter, filtrate is washed with pure water with funnel; The sediment that obtains adds pure water and stirs in container, reinstalls in the magnetic agitation high temperature and high pressure kettle; Be warming up to 300-400 ℃ after the sealing, pressure remains on 15-22Mpa, heat-insulation pressure keeping 3-5 hour; Stop heating and be cooled to room temperature, stir, move to standing demix in the container at the period refusal that is higher than 100 ℃; Another vessel in heating of supernatant liquor impouring is concentrated into thick, lower floor's dope or lower floor's dope and supernatant liquor concentrate is put in the sand mill ground half an hour, then disperses 1 hour with the ultrasonication of ultrasonication dispersion machine; Carry out high speed centrifugation again and separate, isolated corase particles can mix sand milling and ultrasonication dispersion again in the synthetic conducting liquid again, and isolated fine particle partly is the ITO nano crystalline water dispersion.
ITO nano crystalline water dispersion of the present invention, the granularity of its described product are less than 50nm, and solids content reaches more than 25%.
The preparation method of ITO nano crystalline water dispersion of the present invention, it comprises following processing step:
A, dissolving: stannic chloride pentahydrate and indium trichloride are dissolved in the isopropyl alcohol;
B, co-precipitation and filtration: in above-mentioned solution impouring boiling water, be neutralized to neutrality with ammoniacal liquor, be incubated 70-90 ℃, temperature retention time 1 hour is placed cooling again, filters with funnel, and filtrate is washed ten times with pure water;
C puts suspension-turbid liquid: the above-mentioned sediment that obtains in container, is added pure water and stirs;
D, autoclave heating: above-mentioned suspension-turbid liquid is packed in the magnetic agitation high temperature and high pressure kettle, be warming up to 300-400 ℃ after the sealing, pressure remains on 15-22Mpa, and heat-insulation pressure keeping 3-5 hour, stop heating and be cooled to room temperature, stir at the period refusal that is higher than 100 ℃;
E, grind: product is moved to standing demix in the container, and another vessel in heating of supernatant liquor impouring is concentrated into thick, lower floor's dope or lower floor's dope and supernatant liquor concentrate is put in the sand mill ground half an hour;
F, fragmentation: above-mentioned product was disperseed 1 hour with the ultrasonication of ultrasonication dispersion machine;
G; The centrifugal product that gets: will disperse with high speed centrifugation through the product that ultrasonication disperses to obtain; Centrifugal condition is: 8000ram-10000ram; Time 10-20 minute, isolated corase particles can mix sand milling and ultrasonication dispersion again in the synthetic conducting liquid again, and isolated fine particle partly is the ITO nano crystalline water dispersion.
Compared with present technology ITO nano crystalline water dispersion of the present invention and preparation method thereof has outstanding substantive distinguishing features and marked improvement: 1, adopt hydro-thermal synthetic optimum temperature and pressure, improved transparency of products and conductivity; 2, adopt simple and direct technological process, refused stirring, avoided the generation of " segregation " phenomenon, make the quality of product high and stable in the temperature period that is higher than 100 ℃; 3, sand milling-ultrasonication-ultracentrifugal optimization technology is adopted in reprocessing, does not use any auxiliary agent to produce the aqueous dispersions of the steady I TO of pure high solid, and its particle maximum gauge is less than 50nm, and solids content is more than 25%; 4, because product has high, the advantages such as transparency is good, excellent conductivity of purity height, solids, under the condition of 5-50 ℃ and lucifuge, can steady in a long-termly store, do not condense, not sedimentation, thereby enlarge its range of application.
Embodiment
In order better to understand and to implement, specify ITO nano crystalline water dispersion of the present invention and preparation method thereof below in conjunction with embodiment:
Embodiment 1: 7g stannic chloride pentahydrate and 91g indium trichloride are dissolved in the 600ml isopropyl alcohol, in above-mentioned solution impouring 1200ml boiling water, are neutralized to neutrality with ammoniacal liquor; Put on the low-temperature furnace and be incubated 70-90 ℃, 1 hour time is then after the placement cooling; Filter with the Buchner funnel of completing fine and close filter paper, with pure water washing ten times, the sediment that obtains is transferred in the suitable vessel then; Add pure water to 800ml, stir, more above-mentioned suspension-turbid liquid is packed in the magnetic agitation high temperature and high pressure kettle of 2L; Be warming up to 300-400 ℃ after the sealing, pressure remains on 15-22Mpa, heat-insulation pressure keeping 3-5 hour; Stop heating and be cooled to room temperature, stir, product is moved to standing demix in the container at the period refusal that is higher than 100 ℃; Another vessel in heating of supernatant liquor impouring is concentrated into thick, also can the synthetic supernatant liquor that obtains repeatedly be concentrated to concentrate, and lower floor's dope also can be merged the supernatant liquor concentrate put in the sand mill and grind half an hour; Then disperseed 1 hour with the ultrasonication of ultrasonication dispersion machine; Carry out high speed centrifugation again and centrifugalize 10-20min at 800-1000ram, isolated corase particles can mix sand milling and ultrasonication dispersion again in the synthetic conducting liquid again, and isolated fine particle partly is the ITO nano crystalline water dispersion.
Embodiment 2: will: 35g stannic chloride pentahydrate and 455g indium trichloride are dissolved in the 3000ml isopropyl alcohol, in above-mentioned solution impouring 6000ml boiling water, are neutralized to neutrality with ammoniacal liquor; Put on the low-temperature furnace and be incubated 70-90 ℃, 1 hour time is then after the placement cooling; Filter with the Buchner funnel of completing fine and close filter paper, with pure water washing ten times, the sediment that obtains is transferred in the suitable vessel then; Add pure water to 4000ml, stir, more above-mentioned suspension-turbid liquid is packed in the magnetic agitation high temperature and high pressure kettle of 10L; Be warming up to 300-400 ℃ after the sealing, pressure remains on 15-22Mpa, heat-insulation pressure keeping 3-5 hour; Stop heating and be cooled to room temperature, stir, product is moved to standing demix in the container at the period refusal that is higher than 100 ℃; Another vessel in heating of supernatant liquor impouring is concentrated into thick, also can the synthetic supernatant liquor that obtains repeatedly be concentrated to concentrate, and lower floor's dope also can be merged the supernatant liquor concentrate put in the sand mill and grind half an hour; Then disperseed 1 hour with the ultrasonication of ultrasonication dispersion machine; Carry out high speed centrifugation again and centrifugalize 10-20min at 800-1000ram, isolated corase particles can mix sand milling and ultrasonication dispersion again in the synthetic conducting liquid again, and isolated fine particle partly is the ITO nano crystalline water dispersion.
The above execution mode only is that preferred implementation of the present invention is described; Be not that scope of the present invention is limited; Under the spiritual prerequisite that does not break away from the present invention's technology; Various distortion and improvement that this area engineers and technicians make technical scheme of the present invention all should fall in the definite protection range of claims of the present invention.
Claims (4)
1.ITO nano crystalline water dispersion is that stannic chloride pentahydrate and indium trichloride are dissolved in the isopropyl alcohol, with in the above-mentioned solution impouring boiling water, is neutralized to neutrality with ammoniacal liquor again; Be incubated 1 hour, after the placement cooling, filter with funnel; Filtrate is washed with pure water, and the sediment that obtains adds pure water and stirs in container; Reinstall in the magnetic agitation high temperature and high pressure kettle, be warming up to 300-400 ℃ after the sealing, pressure remains on 15-22Mpa; Heat-insulation pressure keeping 3-5 hour, stop heating and be cooled to room temperature, move to standing demix in the container; Another vessel in heating of supernatant liquor impouring is concentrated into thick, lower floor's dope or lower floor's dope and supernatant liquor concentrate is put in the sand mill ground half an hour, then disperses 1 hour with the ultrasonication of ultrasonication dispersion machine; Carry out high speed centrifugation again and separate, isolated corase particles can mix sand milling and ultrasonication dispersion again in the synthetic conducting liquid again, and isolated fine particle partly is the ITO nano crystalline water dispersion.
2. ITO nano crystalline water dispersion according to claim 1, the granularity that it is characterized in that described ITO nano crystalline water dispersion are less than 50nm, and solids content reaches more than 25%.
3. the preparation method of the described ITO nano crystalline water dispersion of claim 1, it comprises following processing step:
A, dissolving: stannic chloride pentahydrate and indium trichloride are dissolved in the isopropyl alcohol;
B, co-precipitation and filtration: in above-mentioned solution impouring boiling water, be neutralized to neutrality with ammoniacal liquor, be incubated 70-90 ℃, temperature retention time 1 hour is placed cooling again, filters with funnel, and filtrate is washed ten times with pure water;
C puts suspension-turbid liquid: the above-mentioned sediment that obtains in container, is added pure water and stirs;
D, autoclave heating: above-mentioned suspension-turbid liquid is packed in the magnetic agitation high temperature and high pressure kettle, be warming up to 300-400 ℃ after the sealing, pressure remains on 15-22Mpa, and heat-insulation pressure keeping 3-5 hour, stop heating and be cooled to room temperature, stir at the period refusal that is higher than 100 ℃;
E, grind: product is moved to standing demix in the container, and another vessel in heating of supernatant liquor impouring is concentrated into thick, lower floor's dope or lower floor's dope and supernatant liquor concentrate is put in the sand mill ground half an hour;
F, fragmentation: above-mentioned product was disperseed 1 hour with the ultrasonication of ultrasonication dispersion machine;
G, the centrifugal product that gets: will disperse with high speed centrifugation through the product that ultrasonication disperses to obtain, isolated corase particles can mix sand milling and ultrasonication dispersion again in the synthetic conducting liquid again, and isolated fine particle partly is the ITO nano crystalline water dispersion.
4. the preparation method of ITO nano crystalline water dispersion according to claim 3 is characterized in that centrifugal condition is in described centrifugal the product step: 8000ram-10000ram, time 10-20 minute.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102683087A (en) * | 2012-05-31 | 2012-09-19 | 张文知 | Three-way multi-point nano conducting liquid switch and equilibrium state and all-way dip-angle measurement and display instrument including same |
| CN108142059A (en) * | 2018-03-12 | 2018-06-12 | 长春大学 | It is a kind of to promote method of the Chinese rose of cut flower to light absorption as foliar fertilizer using ITO nanoparticle sols |
| CN108201885A (en) * | 2016-12-19 | 2018-06-26 | 赵爱玲 | The anatase titanium dioxide of hydrothermal synthesis method manufacture cladding aluminium |
| CN111423819A (en) * | 2020-04-17 | 2020-07-17 | 深圳市朗纳研磨材料有限公司 | Polishing solution and preparation method thereof |
| CN111498810A (en) * | 2019-01-31 | 2020-08-07 | 北京卫蓝新能源科技有限公司 | Nano material dispersion liquid and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1314871A (en) * | 1998-09-06 | 2001-09-26 | 新材料公共服务公司研究所 | Method for preparing suspensions and powders based on indium tin oxide and the use thereof |
| CN1864834A (en) * | 2006-04-04 | 2006-11-22 | 张文知 | An addictive-free, long-term stable, high-solid, transparent and conductive nano crystalline water dispersion and method for preparing same |
-
2011
- 2011-04-26 CN CN2011101080866A patent/CN102760509A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1314871A (en) * | 1998-09-06 | 2001-09-26 | 新材料公共服务公司研究所 | Method for preparing suspensions and powders based on indium tin oxide and the use thereof |
| CN1864834A (en) * | 2006-04-04 | 2006-11-22 | 张文知 | An addictive-free, long-term stable, high-solid, transparent and conductive nano crystalline water dispersion and method for preparing same |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102683087A (en) * | 2012-05-31 | 2012-09-19 | 张文知 | Three-way multi-point nano conducting liquid switch and equilibrium state and all-way dip-angle measurement and display instrument including same |
| CN108201885A (en) * | 2016-12-19 | 2018-06-26 | 赵爱玲 | The anatase titanium dioxide of hydrothermal synthesis method manufacture cladding aluminium |
| CN108142059A (en) * | 2018-03-12 | 2018-06-12 | 长春大学 | It is a kind of to promote method of the Chinese rose of cut flower to light absorption as foliar fertilizer using ITO nanoparticle sols |
| CN108142059B (en) * | 2018-03-12 | 2020-07-07 | 长春大学 | Method for promoting light absorption of cut roses by applying ITO nano particle sol as foliar fertilizer |
| CN111498810A (en) * | 2019-01-31 | 2020-08-07 | 北京卫蓝新能源科技有限公司 | Nano material dispersion liquid and preparation method thereof |
| CN111498810B (en) * | 2019-01-31 | 2022-07-12 | 北京卫蓝新能源科技有限公司 | Nano material dispersion liquid and preparation method thereof |
| CN111423819A (en) * | 2020-04-17 | 2020-07-17 | 深圳市朗纳研磨材料有限公司 | Polishing solution and preparation method thereof |
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Application publication date: 20121031 |