CN104628264A - Film coating liquid for online CVD process sunshine control film and preparation method of film-coated glass - Google Patents
Film coating liquid for online CVD process sunshine control film and preparation method of film-coated glass Download PDFInfo
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- CN104628264A CN104628264A CN201510052663.2A CN201510052663A CN104628264A CN 104628264 A CN104628264 A CN 104628264A CN 201510052663 A CN201510052663 A CN 201510052663A CN 104628264 A CN104628264 A CN 104628264A
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Abstract
The invention belongs to the technical field of production of film-coated glass and mainly relates to a film coating liquid for an online CVD process sunshine control film and a preparation method of film-coated glass. The film coating liquid is prepared by the following steps: with solid SbCl3 as a doping agent and liquid monobutyltin trichloride MBTC or dimethyltin dichloride DMTC as a tin source, mixing SbCl3 with liquid monobutyltin trichloride MBTC or dimethyltin dichloride DMTC at a mass ratio of (0.01-0.12) to 1 without adding any solvent, and completely dissolving SbCl3 by virtue of a water bath method, so as to prepare the flavescent stibium-doped stannic oxide transparent conductive film coating liquid. The film coating liquid has the advantages that the preparation operation is simple and convenient, film coating equipment is simple, and the performance of a coated film is good.
Description
Technical field
The invention belongs to coated glass production technical field, relate generally to the preparation of a kind of online CVD solar control film coating liquid and coated glass.
Technical background
Online CVD coating technique refers on floatation glass production line, clean float glass that utilize high speed traction, that be in high temperature is substrate, plated film gas is introduced reactor, carries out on-line coating at glass baseplate surface through deposition, diffusion, film forming, parsing four CVD reaction process.
Antimony-doped tin oxide transparent conductive film (ATO) effectively can stop near infrared ray, there is good heat insulating function, there is the advantage that visible light transmissivity is higher, resistivity is low and chemical stability is high simultaneously, can be applied on top-grade building sunlight controlling coated glass.ATO film general at present adopts sol-gel method, CVD is coated with; Due to SbCl
3be at room temperature solid, by SbCl when therefore using CVD to carry out plated film
3gasification difficulty is comparatively large, and equipment is complicated, if pipeline heat insulation is bad, easily line clogging occurs.
Summary of the invention
For solving the problems of the technologies described above, the object of the invention is the preparation of a kind of online CVD solar control film coating liquid and coated glass.
The present invention adopts following technical scheme for completing above-mentioned purpose:
A kind of online CVD solar control film coating liquid, described coating liquid adopts solid-state SbCl
3as doping agent, liquid monobutyl-tin-trichloride MBTC or dimethyltin chloride DMTC as Xi Yuan, under the prerequisite of not adding any solvent, with SbCl
3the mass ratio mixing of/MBTC or DMTC=0.01 ~ 0.12:1, makes SbCl with immersion method
3dissolve completely, make the transparent conductive coatings liquid in lurid antimony-doped tin oxide.
The temperature of immersion method is 85 DEG C ~ 95 DEG C, and soaking time is 5 ~ 10min.
The conductivity experiment of film shows unadulterated SnO
2film is based on oxygen vacancy alms giver conduction, and appropriate Sb doping can significantly improve the conductivity of film, and keeps higher visible light transmissivity and lower reflectivity; The properties of infrared reflection of film and the carrier concentration of film and mobility have substantial connection, are only improved carrier concentration and the mobility of film, reduce the square resistance of film, significantly could improve the infrared reflectance of film; SbCl in coating liquid
3content when being less than 0.01, carrier concentration and the mobility of film are low, and the square resistance of film is large, and the low radiance of film is not good; SbCl in coating liquid
3content more than 0.12 time, the increase of film thickness and the raising of doping content can worsen the planeness of face, and simultaneously excessive doping also can affect the crystal property of film.Dopant ion solubleness is in the oxide limited, and dopant ion itself is a kind of lattice imperfection, has stronger scattering process to electronics, doping content is too high, then can have a strong impact on the mobility of electronics, worsens electroconductibility, the square resistance of film increases, and low radiance is affected.
The technique utilizing above-mentioned coating liquid to prepare coated glass includes the equipment of base plate glass and the gasification of coating liquid; The gasification of described coating liquid take coating liquid as precursor, H
2o is catalyzer, and using pressurized air as carrier gas, gasifies at the temperature of 150 DEG C ± 5 DEG C to coating liquid; And the coating liquid after gasification is sent into plated film device; Meanwhile, the base plate glass after cutting out just is heated to 550 DEG C ~ 650 DEG C; Coating liquid after gasification is ejected on the glass substrate at 550 DEG C ~ 650 DEG C and forms the sun light control film that thickness is 300nm ~ 500nm by plated film device, thus obtains coated glass.
In order to make glass plated film evenly, need repeatedly plated film be carried out to base plate glass, after each plated film terminates, after glass substrate being rotated 180 °, carry out next plated film again.
In the process of coating liquid gasification, coating liquid sample size is 15ml/hr, catalyzer H
2o sample size is 0.8225ml/hr, and plating skim depositing time used is 15s ~ 75s.
The square resistance of coated glass is greater than 20/, and infrared transmittivity is less than 40%, visible region transmitance 40% ~ 60%, and coated glass is light blue.
The preparation of a kind of online CVD solar control film coating liquid that the present invention proposes and coated glass, under the condition of not adding any solvent, by solid feed SbCl
3mix with monobutyl-tin-trichloride MBTC or dimethyltin chloride DMTC, immersion method is used to promote to dissolve, make light yellow clear settled solution, and success is implemented on CVD coating system, the transparent conductive film of obtained antimony-doped tin oxide, have that coating liquid formulation operations is easy, filming equipment simple, plate the good advantage of film performance.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of coated glass.
Embodiment
With specific embodiment, the present invention is illustrated by reference to the accompanying drawings:
According to SbCl
3/ monobutyl-tin-trichloride MBTC or dimethyltin chloride DMTC is the ratio of 0.01 ~ 0.12:1, adopts ten thousand/electronic balance to take SbCl
3x gram, put into 50ml beaker, v=m/ ρ is utilized to calculate the volume v of monobutyl-tin-trichloride MBTC used or dimethyltin chloride DMTC liquid, measuring the monobutyl-tin-trichloride MBTC of v ml or dimethyltin chloride DMTC with 20ml liquid-transfering gun adds in beaker, with preservative film, beaker mouth is sealed, then 50ml beaker is put into the water-bath of 1000ml large beaker, electric furnace heats, at 85 DEG C ~ 95 DEG C insulation 5 ~ 10min, make SbCl
3dissolve completely, then be cooled to the transparent conductive coatings liquid that namely room temperature obtain in lurid antimony-doped tin oxide.
Embodiment 1:
In this embodiment, with SbCl
3the ratio of/monobutyl-tin-trichloride MBTC=0.01 is mixed with coating liquid; With prepared coating liquid for precursor, H
2o is catalyzer, and using pressurized air as carrier gas, gasifies at 150 DEG C of temperature, and glass substrate (150mm*150mm*4 mm) temperature is carry out plated film under 590 DEG C of conditions.Self-control coating liquid sample size is 15ml/hr, catalyzer H
2o sample size is 0.8225ml/hr, and the one single deposition time is 75s, after each plated film terminates, glass substrate is rotated 180 °, repeats four plated films, make plated film evenly, the square resistance of last gained sample is 20/, and visible light transmissivity is 61.02%.
Embodiment 2:
In this embodiment, with SbCl
3the ratio of/monobutyl-tin-trichloride MBTC=0.05 is mixed with coating liquid; With prepared coating liquid for precursor, H
2o is catalyzer, and using pressurized air as carrier gas, gasifies at 150 DEG C of temperature, and glass substrate (150mm*150mm*4 mm) temperature is carry out plated film under 610 DEG C of conditions.Self-control coating liquid sample size is 15ml/hr, catalyzer H
2o sample size is 0.8225ml/hr, and the one single deposition time is 55s, after each plated film terminates, glass substrate is rotated 180 °, repeats four plated films, make plated film evenly, the square resistance of last gained sample is 87/, and visible light transmissivity is 55.79%.
Embodiment 3:
In this embodiment, with SbCl
3the ratio of/monobutyl-tin-trichloride MBTC=0.09 is mixed with coating liquid; With prepared coating liquid for precursor, H
2o is catalyzer, and using pressurized air as carrier gas, gasifies at 150 DEG C of temperature, and glass substrate (150mm*150mm*4 mm) temperature is carry out plated film under 620 DEG C of conditions.Self-control coating liquid sample size is 15ml/hr, catalyzer H
2o sample size is 0.8225ml/hr, and the one single deposition time is 35s, after each plated film terminates, glass substrate is rotated 180 °, repeats four plated films, make plated film evenly, the square resistance of last gained sample is greater than 1000/, and visible light transmissivity is 47.30%.
Embodiment 4:
In this embodiment, with SbCl
3the ratio of/monobutyl-tin-trichloride MBTC=0.12 is mixed with coating liquid; With prepared coating liquid for precursor, H
2o is catalyzer, and using pressurized air as carrier gas, gasifies at 150 DEG C of temperature, and glass substrate (150mm*150mm*4 mm) temperature is carry out plated film under 630 DEG C of conditions.Self-control coating liquid sample size is 15ml/hr, catalyzer H
2o sample size is 0.8225ml/hr, and the one single deposition time is 15s, after each plated film terminates, glass substrate is rotated 180 °, repeats four plated films, make plated film evenly, the square resistance of last gained sample is greater than 1000/, and visible light transmissivity is 42.38%.
Claims (6)
1. an online CVD solar control film coating liquid, is characterized in that: described coating liquid adopts solid-state SbCl
3as doping agent, liquid monobutyl-tin-trichloride MBTC or dimethyltin chloride DMTC is as Xi Yuan; Under the prerequisite of not adding any solvent, by SbCl
3mix with the mass ratio of 0.01 ~ 0.12:1 with monobutyl-tin-trichloride MBTC or dimethyltin chloride DMTC, make SbCl with immersion method
3dissolve completely, make the transparent conductive coatings liquid in lurid antimony-doped tin oxide.
2. one according to claim 1 online CVD solar control film coating liquid, is characterized in that: the temperature of immersion method is 85 DEG C ~ 95 DEG C, and soaking time is 5 ~ 10min.
3. utilize a kind of online CVD solar control film coating liquid described in claim 1 to prepare the technique of coated glass, it is characterized in that: described technique includes the equipment of base plate glass and the gasification of coating liquid; The gasification of described coating liquid take coating liquid as precursor, H
2o is catalyzer, and using pressurized air as carrier gas, gasifies at the temperature of 150 DEG C ± 5 DEG C to coating liquid; And the coating liquid after gasification is sent into plated film device; Meanwhile, the base plate glass after cutting out is heated to 550 DEG C ~ 650 DEG C; Coating liquid after gasification is ejected on the glass substrate at 550 DEG C ~ 650 DEG C and forms the sun light control film that thickness is 300nm ~ 500nm by plated film device, thus obtains coated glass.
4. the preparation of a kind of online CVD coated glass according to claim 3, it is characterized in that: in order to make glass plated film evenly, need repeatedly plated film be carried out to base plate glass, after each plated film terminates, after glass substrate being rotated 180 °, carry out next plated film again.
5. the preparation of a kind of online CVD coated glass according to claim 3, is characterized in that: in the process of coating liquid gasification, coating liquid sample size is 15ml/hr, catalyzer H
2o sample size is 0.8225ml/hr, and plating skim depositing time used is 15s ~ 75s.
6. the preparation of a kind of online CVD coated glass according to claim 3, it is characterized in that: the square resistance of coated glass is greater than 20/, and infrared transmittivity is less than 40%, visible region transmitance 40% ~ 60%, coated glass is light blue.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510052663.2A CN104628264A (en) | 2015-02-02 | 2015-02-02 | Film coating liquid for online CVD process sunshine control film and preparation method of film-coated glass |
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|---|---|---|---|
| CN201510052663.2A CN104628264A (en) | 2015-02-02 | 2015-02-02 | Film coating liquid for online CVD process sunshine control film and preparation method of film-coated glass |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106116171A (en) * | 2016-05-23 | 2016-11-16 | 漳州旗滨玻璃有限公司 | A kind of light blue low reflection sunlight controlling coated glass preparation technology |
| CN113929313A (en) * | 2021-10-18 | 2022-01-14 | 西安电子科技大学 | Three-dimensional conductive nanorod and preparation method of array electron transport layer thereof |
| CN115196884A (en) * | 2022-06-30 | 2022-10-18 | 深圳市楠轩光电科技有限公司 | Optical glass coating method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1350990A (en) * | 2000-10-30 | 2002-05-29 | 阿托费纳化学股份有限公司 | Sunshine controlled coated glass |
-
2015
- 2015-02-02 CN CN201510052663.2A patent/CN104628264A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1350990A (en) * | 2000-10-30 | 2002-05-29 | 阿托费纳化学股份有限公司 | Sunshine controlled coated glass |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106116171A (en) * | 2016-05-23 | 2016-11-16 | 漳州旗滨玻璃有限公司 | A kind of light blue low reflection sunlight controlling coated glass preparation technology |
| CN106116171B (en) * | 2016-05-23 | 2019-09-24 | 漳州旗滨玻璃有限公司 | A kind of light blue low reflection sunlight controlling coated glass preparation process |
| CN113929313A (en) * | 2021-10-18 | 2022-01-14 | 西安电子科技大学 | Three-dimensional conductive nanorod and preparation method of array electron transport layer thereof |
| CN115196884A (en) * | 2022-06-30 | 2022-10-18 | 深圳市楠轩光电科技有限公司 | Optical glass coating method |
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