CN103936059A - Preparation method of tin oxide film - Google Patents
Preparation method of tin oxide film Download PDFInfo
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- CN103936059A CN103936059A CN201410105524.7A CN201410105524A CN103936059A CN 103936059 A CN103936059 A CN 103936059A CN 201410105524 A CN201410105524 A CN 201410105524A CN 103936059 A CN103936059 A CN 103936059A
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Abstract
The invention discloses a preparation method of a tin oxide film, and belongs to the technical field of film preparation. The preparation method is as follows: a fluoride of antimony is used as a doping source, a chloride of tin is used as a starting raw material, after mixed atomization, the fluoride of antimony and the chloride of tin are deposited on the surface of a high temperature resistant substrate to from a transparent fluorine-antimony co-doping tin oxide thin film with good functions. According to the method, in a SnO2 crystal structure, fluoride ions replace part of oxygen ion positions, antimony ions replace part of tin ion positions for doping, and higher carrier density is obtained, so that the tin oxide film is better in electrical conductivity, atmosphere sensitivity, transmittance and the like than single fluorine or single antimony doping film, and is a very advanced and potential semiconductor functional thin film material.
Description
Technical field
The invention belongs to film preparing technology field, relate to the aqueous systems atomization heat deposition preparation method of the SnO 2 thin film of fluoro-antimony codoped.
Background technology
The preparation method of the SnO 2 thin film of current different ions doping mainly contains sputtering sedimentation (PVD), chemical vapor deposition (CVD) and spraying thermolysis (SP) technology plated film.Compare with PVD, CVD method, the equipment and technology of spraying thermolysis SP method is relatively simple, not only can the good film of preparation quality, and be easy to doping, be a kind of economy, high-level efficiency, mass-producing, industry method for manufacturing thin film.
Conventional spraying thermolysis at present adopts high pressure liquid stream and high pressure draft mixing jetting to form the atomizing droplet of high-speed motion conventionally, clash into and deposit to high-temperature substrates generation pyrolysis and form thin film deposition, this deposition process air turbulence, air-flow heat transfer simultaneously, solvent gasification, pyrolysis cause absorbing and cooling temperature remarkable, the problem such as be easy to cause that substrate surface deposition is inhomogeneous, temperature decrease, substrate burst, react not exclusively, conventionally except solvent conventionally adopts low-molecular-weight flammable organic solvent, also needs periodically, intermittent spraying.Not only affect film quality but also reduced production efficiency, large quantity of exhaust gas discharge and environmental pollution are also its problems that must face in addition.
The four problems that spraying pyrolysis technique exists: 1, adopt halogenide and hydrofluoric acid, the Neutral ammonium fluoride of antimony to adulterate, especially wherein fluorochemical is easy to volatilization, doping efficiency is extremely low, causes that fluoride pollution is serious, discharge can not be up to standard; 2, the spray pattern of pressurised fluid stream atomization causes atomizing droplet size large (m), atomization quantity is excessive and wayward for 5 μ m～20 μ, and substrate cooling is serious, film is inner and surface imperfection is more, meanwhile, objectively require intermittent, periodicity repeated spray, cause production efficiency to decline; 3, adopt organic solvent system, colloidal sol (solution) concentration is lower, in thermal decomposition process disposal of pollutants serious, and the coated film deposition cycle is long, production efficiency is low; 4, gas shock substrate causes gas smooth disorderly, deposits inhomogeneous low with sedimentation effect.
In addition, conventionally the atomization means that adopt are to adopt ultrasonic atomization, utilize ultrasonic energy that solution mist is changed into small droplet, the aerosol forming is gentle mild, but is subject to the restriction of four aspects: 1, ultrasonic wave wafer is not easy to be operated in the corrosive medium such as acidity, alkalescence environment; 2, be subject to ultrasonic energy quantitative limitation, can not haze to the solution of high density; 3, need blower fan air blast to complete aerosol delivery, working mechanism's complexity; 4, due to wafer heating in work engineering, cause the unstable and precipitation of solution system to produce, be not suitable for the suitability for industrialized production of film preparation.
Summary of the invention
The object of this invention is to provide the preparation method of the SnO 2 thin film of a kind of low exhaust gas emission, low environment pollution, high quality, high-level efficiency film preparation.
The present invention includes following steps:
1) preparation of forerunner's coated solution: under room temperature, normal pressure, dry environment, the fluorochemical mix and blend of water and antimony is formed to doped solution, the muriate mix and blend of Yi Shui and tin is formed to tin-salt solution, then doped solution is added drop-wise in tin-salt solution under agitation condition, through regulating mixing solutions
pbehind H value to 2～3, airtight ageing 6～10h forms forerunner's coated solution;
2) atomization of forerunner's coated solution: adopt gas compression formula spraying gun, with air after pure nitrogen gas or filtration, purification, forerunner's coated solution is carried out to atomization;
3) film forming: forerunner's coated solution of atomization is deposited on to the temperature of advancing taking 30cm～100cm/min as the high temperature resistant substrate surface of 550 DEG C～650 DEG C, through cooling formation SnO 2 thin film.
The present invention for the raw material that sets out, is deposited on high temperature resistant substrate surface taking the fluorochemical of antimony as doped source, with the muriate of tin after mixed aerosol, forms a kind of transparently and have the SnO 2 thin film of good function with this, and its fluoro-antimony codoped, by SnO
2in crystalline structure, adulterate in fluorion Substitute For Partial oxonium ion position, antimony ion Substitute For Partial tin ion position, form higher carrier density, thereby having than the doping of single fluorine or the more superior electroconductibility of single antimony doping, atmosphere susceptibility, transmitance etc., is the semi-conductor film material with function of a kind of very advantageous, potentiality.
Compared with prior art, its superiority and key problem in technology are in the present invention:
1, adopt the fluorochemical (antimony trifluoride or antimony pentafluoride) of antimony as fluorine, the antimony codoped raw material that sets out, solve the fluorochemicals such as hydrofluoric acid, Neutral ammonium fluoride and be easy to volatilization, unsettled problem, reduce cost and solved a large amount of waste gas containing fluorides and polluted, ensured reliable, the Effective Doping of antimony and fluorine simultaneously.
2, adopting deionized water or distilled water is solvent, can effectively improve the concentration of tin chloride solution and the stability of the tin-salt solution that antimony, fluorine adulterate, and can prepare high performance film for single deposition provides feasibility.
3, adopt gas compression formula spraying gun, by the forerunner's coated solution after gas atomization, realize micron order uniform atomizing, reach mild, the gentle object of aerosol motion, to production unit noresidue, evenly, the SnO 2 thin film thick consistency of formation is good for deposition.
4, the coated basal plate of homogeneous heating to 550～650 DEG C is at the uniform velocity by this sedimentary province, is then evenly cooled to room temperature and prepares the SnO 2 thin film of fluoro-antimony codoped, and single can be prepared high performance film, and production process is simplified, production efficiency is high.
5, prepare SnO 2 thin film inherence and surface uniform densification, high-quality fluoro-antimony codoped by pyrolysis, its optical property, electric property reach the corresponding index of the film of CVD, PVD method substantially, and the resistivity of film can reach 10
-5the Ω cm order of magnitude, on high transmission glass substrate, visible light transmissivity can reach more than 90%.
In addition, muriate of the present invention adopts tin tetrachloride or the tin tetrachloride containing crystal water.Tin tetrachloride or be 4 valencys containing the valence state of tin in the tin tetrachloride of crystal water, consistent with the valence state of tin in final fluoro-antimony codoped SnO 2 thin film, compare with conventional tin protochloride (valence state of tin is divalent), the variation of valence of having avoided tin in pyrolysis and film crystallization change process subsequently, is conducive to obtain single crystallized product thing phase and good transmitance, electric property.
The present invention regulates mixing solutions with hydrochloric acid or trifluoroacetic acid
ph value.Because being easy to hydrolysis under water solution system, the fluorochemical of adopted antimony and the muriate of tin cause plated film precursor aqueous solution stable not, the acidity that adopts hydrochloric acid or trifluoroacetic acid can improve solution provides excessive chlorion or fluorion simultaneously, can suppress its hydrolysis reaction, improve the stability of forerunner's coated solution and do not introduce extra acid ion, the chemical reaction being beneficial in coating process is simplified, and product thing is mutually single.
In described forerunner's coated solution, the volumetric molar concentration of Sn atom is 2～3.5mol/L, and the mol ratio of F and Sn is 0.18～0.30 ︰ 1, and the mol ratio of Sb and Sn is 0.036～0.08 ︰ 1.The high density of forerunner's coated solution is conducive to the raising of single deposit film thickness, but too high concentration can cause, forerunner's coated solution is unstable, resting period is short, simultaneously after atomization droplet dia large, be unfavorable for high-quality film preparation, therefore, taking into account under the prerequisite of the stable and atomizing effect of forerunner's coated solution, 2～3.5mol/L is suitable concentration span of control.Be entrained in raising carrier density at fluorine, antimony ion itself is also to produce high defect concentrations in crystals simultaneously, transmitance, specific conductivity are brought to negative impact, there is suitable doping ratio, under the condition of fluoro-antimony codoped, under the transmitance prerequisite that ensures～90%, the doping content of the fluorion that high conductivity is corresponding is between 0.18～0.30, and the doping content of antimony ion is between 0.036～0.08.
The flow of forerunner's coated solution of atomization is 30～500 ml/minm
2.The film thickness of single deposition is proportional to the spray deposition amount of per area per time, under the certain condition of effective depositional area of sediment chamber, this spray deposition amount is proportional to again the atomization flow of forerunner's coated solution, therefore can control the flow of atomization forerunner coated solution and realize different thin film deposition thickness demands, in addition, spray deposition amount is larger, substrate cooling is faster, can have influence on thoroughness that pyrolysis carries out and the crystallization change of product, therefore, there is a suitable spray deposition amount.In the flow control of forerunner's coated solution of the present invention at 30～500 ml/minm
2can obtain good coating quality.
The present invention adopts gas compression formula spraying gun, can avoiding the spray pattern of conventional pressurised fluid stream atomization to cause atomizing droplet size, large (5 μ m～20 μ m), excessive and the uppity problem of atomization quantity and gas shock substrate cause gas flowfield disorder, deposit inhomogeneous and sedimentation effect is low.Can overcome in ultrasonic atomization method simultaneously ultrasonic wave wafer not resistant to corrosive media, can not haze to the solution of high density, the heating of ultrasonic wave wafer causes the problems such as the unstable and working mechanism of solution system is complicated; Adopt gas compression formula spraying gun, can realize high density forerunner coated solution is realized to micron order uniform atomizing, aerosol motion is mild, gentle, and thin film deposition is even, simple in structure, acid-alkali-corrosive-resisting, the suitability for industrialized production of applicable film preparation.
Brief description of the drawings
Fig. 1 is the XRD phenogram of the SnO 2 thin film crystalline structure made of the inventive method.
Fig. 2 is the SnO 2 thin film surface topography SEM photo that the inventive method is made.
Fig. 3 is the transmission measurement graphic representation of the SnO 2 thin film representative instance sample made of the inventive method.
Embodiment
One, production technique:
Embodiment 1:
1, under room temperature, normal pressure, dry environment, employing antimony trifluoride is that raw material, deionized water are solvent, and mix and blend forms doped solution.Adopt tin tetrachloride (SnCl
4) for raw material, deionized water are solvent, mix and blend forms tin-salt solution.Then doped solution is added drop-wise in tin-salt solution under agitation condition, form mixing solutions, doping ratio in this mixing solutions forming: fluorine is 18mol%, antimony is 6 mol %, tin volumetric molar concentration is 3.5mol/L, adopt again hydrochloric acid conditioning solution pH to be about 2～3, after airtight ageing 6h, obtain forerunner's coated solution.
Then forerunner's coated solution is joined in gas compression formula spraying gun.
2, choose high transmission glass (low Fe glass), silica glass, corning glass, high alumina ceramic tile etc. wherein a kind of high temperature material as plated film substrate.
Adopt cleaning process flow pickling, the washing of toughened glass production line and dry substrate, being then positioned on transfer roller or Special sample bracket.Be sent to heating chamber by roller-way, two-sided reciprocating heating, homogeneous heating to 550 DEG C in 3～25min～650 DEG C, stand-by.
3, after employing high pure nitrogen or filtration, purification, air is source of the gas, start spraying gun, forerunner's coated solution is carried out to atomization, and by sealed gas pipeline, aerosol delivery, to aerosol sedimentary province, is regulated stream pressure and atomization screen gap to control atomized liquid stream flow and is about 500 ml/minm
2.
4, be that the substrate of 550 DEG C～650 DEG C evenly transmits by aerosol sedimentary province with 80cm/min by roller-way by temperature, can complete single fast deposition.
5, post-depositional substrate slowly cools to room temperature or forces cooling (tempering processing) to room temperature, the coating operation of completing substrate by enter subregion cooling room by roller-way transmission.
6, the doped stannum oxide film resiativity of preparation is about 9 × 10
-4Ω cm, thickness is about 160nm left and right, and average visible light transmissivity is 90%～91%.
Embodiment 2:
1, under room temperature, normal pressure, dry environment, employing antimony trifluoride is that raw material, deionized water are solvent, and mix and blend forms doped solution.Adopt tin tetrachloride (SnCl
4) for raw material, deionized water are solvent, mix and blend forms tin-salt solution.Then doped solution is added drop-wise in tin-salt solution under agitation condition, form mixing solutions, control doping ratio in mixing solutions: fluorine is 24mol%, antimony is 8 mol %, tin volumetric molar concentration is 3.5mol/L, adopt trifluoroacetic acid to regulate pH value to 2～3 of mixing solutions, through airtight ageing 10h, obtain forerunner's coated solution.
Then forerunner's coated solution is joined in gas compression formula spraying gun.
2, choose high transmission glass (low Fe glass), silica glass, corning glass, high alumina ceramic tile etc. wherein a kind of high temperature material as plated film substrate.
Adopt cleaning process flow pickling, the washing of toughened glass production line and dry substrate, being then positioned on transfer roller or Special sample bracket.Be sent to heating chamber by roller-way, two-sided reciprocating heating, through 25min homogeneous heating to 600 DEG C～610 DEG C, stand-by.
3, after employing high pure nitrogen or filtration, purification, air is source of the gas, start hydrocone type and clash into spraying gun, forerunner's coated solution is carried out to atomization, and by sealed gas pipeline, aerosol delivery, to aerosol sedimentary province, is regulated stream pressure and atomization screen gap to control atomized liquid stream flow and is about 300 ml/minm
2.
4, be that the substrate of 600 DEG C～610 DEG C evenly transmits by aerosol sedimentary province with 50cm/min by roller-way by temperature, can complete single fast deposition.
5, post-depositional substrate slowly cools to room temperature or forces cooling (tempering processing) to room temperature, the coating operation of completing substrate by enter subregion cooling room by roller-way transmission.
6, the doped stannum oxide film resiativity of preparation is about 1 × 10
-4Ω cm, thickness is about 210nm left and right, and average visible light transmissivity is 92%～93%.
Embodiment 3
1, under room temperature, normal pressure, dry environment, employing antimony pentafluoride is that raw material, deionized water are solvent, and mix and blend forms doped solution.Adopt tin tetrachloride (SnCl
45H
2o) for raw material, deionized water are solvent, mix and blend forms tin-salt solution.Then doped solution is added drop-wise in tin-salt solution under agitation condition, forms mixing solutions, control doping ratio in mixing solutions: fluorine is 24mol%, and antimony is 4.8 mol %, and tin is: 2.5mol/L, employing hydrochloric acid adjusting mixing solutions
ph value to 2～3, through airtight ageing 10h, obtain forerunner's coated solution.
Then forerunner's coated solution is joined in gas compression formula spraying gun.
2, choose high transmission glass (low Fe glass), silica glass, corning glass, high alumina ceramic tile etc. wherein a kind of high temperature material as plated film substrate.
Adopt cleaning process flow pickling, the washing of toughened glass production line and dry substrate, being then positioned on transfer roller or Special sample bracket.Be sent to heating chamber by roller-way, two-sided reciprocating heating, through 3min homogeneous heating to 550 DEG C～580 DEG C, stand-by.
3, after employing high pure nitrogen or filtration, purification, air is source of the gas, start hydrocone type and clash into spraying gun, forerunner's coated solution is carried out to atomization, and by sealed gas pipeline, aerosol delivery, to aerosol sedimentary province, is regulated stream pressure and atomization screen gap to control atomized liquid stream flow and is about 100 ml/minm
2.
4, be that the substrate of 600 DEG C～610 DEG C evenly transmits by aerosol sedimentary province with 50cm/min by roller-way by temperature, can complete single fast deposition.
5, post-depositional substrate slowly cools to room temperature or forces cooling (tempering processing) to room temperature, the coating operation of completing substrate by enter subregion cooling room by roller-way transmission.
6, the doped stannum oxide film resiativity of preparation is about 8 × 10
-4Ω cm, thickness is about 240nm left and right, and average visible light transmissivity is 95%～98%.
Embodiment 4:
1, under room temperature, normal pressure, dry environment, employing antimony pentafluoride is that raw material, deionized water are solvent, and mix and blend forms doped solution.Adopt tin tetrachloride (SnCl
45H
2o) for raw material, deionized water are solvent, mix and blend forms tin-salt solution.Then doped solution is added drop-wise in tin-salt solution under agitation condition, forms mixing solutions, control doping ratio in mixing solutions: fluorine is 18mol%, and antimony is 3.6 mol %, and the volumetric molar concentration of tin is about 2mol/L, employing trifluoroacetic acid adjusting mixing solutions
ph value to 2～3, through airtight ageing 6h, obtain forerunner's coated solution.
Then forerunner's coated solution is joined in gas compression formula spraying gun.
2, choose high transmission glass (low Fe glass), silica glass, corning glass, high alumina ceramic tile etc. wherein a kind of high temperature material as plated film substrate.
Adopt cleaning process flow pickling, the washing of toughened glass production line and dry substrate, being then positioned on transfer roller or Special sample bracket.Be sent to heating chamber by roller-way, two-sided reciprocating heating, through 25min homogeneous heating to 640 DEG C～650 DEG C, stand-by.
3, after employing high pure nitrogen or filtration, purification, air is source of the gas, start hydrocone type and clash into spraying gun, forerunner's coated solution is carried out to atomization, and by sealed gas pipeline, aerosol delivery, to aerosol sedimentary province, is regulated stream pressure and atomization screen gap to control atomized liquid stream flow and is about 30 ml/minm
2.
4, be that the substrate of 640 DEG C～650 DEG C evenly transmits by aerosol sedimentary province with 100cm/min by roller-way by temperature, can complete single fast deposition.In 60min, be down to below 100 DEG C.
5, post-depositional substrate slowly cools to room temperature or forces cooling (tempering processing) to room temperature, the coating operation of completing substrate by enter subregion cooling room by roller-way transmission.
6, the doped stannum oxide film resiativity of preparation is about 1 × 10
-3Ω cm, thickness is about 90nm left and right, is 92%～94% at LCD with average visible light transmissivity on corning glass substrate.
Two, performance:
As seen from Figure 1: adopt the inventive method to obtain the stannic oxide crystal film of the Rutile Type of well-crystallized.
As seen from Figure 2: film surface densification evenly reaches the quality of CVD, PVD film.
Fig. 3 shows: prepared fluorine antimony codoped SnO 2 thin film have do can be by transmitance, reach more than 90%, reach the service requirements of solar battery panel, LCD, PDP high-performance glass panel.
Claims (6)
1. a preparation method for SnO 2 thin film, is characterized in that comprising the following steps:
1) preparation of forerunner's coated solution: under room temperature, normal pressure, dry environment, the fluorochemical mix and blend of water and antimony is formed to doped solution, the muriate mix and blend of Yi Shui and tin is formed to tin-salt solution, then doped solution is added drop-wise in tin-salt solution under agitation condition, through regulating mixing solutions
pbehind H value to 2～3, airtight ageing 6～10h forms forerunner's coated solution; The muriate of described tin is tin tetrachloride or the tin tetrachloride containing crystal water;
2) atomization of forerunner's coated solution: adopt gas compression formula spraying gun, with air after pure nitrogen gas or filtration, purification, forerunner's coated solution is carried out to atomization;
3) film forming: forerunner's coated solution of atomization is deposited on to the temperature of advancing taking 30cm～100cm/min as the high temperature resistant substrate surface of 550 DEG C～650 DEG C, through cooling formation SnO 2 thin film.
2. the preparation method of SnO 2 thin film according to claim 1, the fluorochemical that it is characterized in that described antimony is antimony trifluoride or antimony pentafluoride.
3. the preparation method of SnO 2 thin film according to claim 1, is characterized in that regulating mixing solutions with hydrochloric acid or trifluoroacetic acid
ph value.
4. the preparation method of SnO 2 thin film according to claim 1, the volumetric molar concentration that it is characterized in that Sn atom in described forerunner's coated solution is 2～3.5mol/L, and the mol ratio of F and Sn is 0.18～0.30 ︰ 1, and the mol ratio of Sb and Sn is 0.036～0.08 ︰ 1.
5. the preparation method of SnO 2 thin film according to claim 1, the flow that it is characterized in that forerunner's coated solution of atomization is 30～500 ml/minm
2.
6. according to the preparation method of SnO 2 thin film described in claim 1 or 9, it is characterized in that first high temperature resistant base-plate cleaning post-drying, then in 3～25min, be preheated to 550 DEG C～650 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699870A (en) * | 2017-09-18 | 2018-02-16 | 中山大学 | Method for manufacturing thin film and system in hypergravity chemical deposition pipe |
| CN108409154A (en) * | 2018-03-22 | 2018-08-17 | 燕山大学 | A kind of preparation method of the FTO-G laminated films with micro-nano cluster surface topography |
| CN110256070A (en) * | 2019-07-31 | 2019-09-20 | 三祥新材股份有限公司 | A kind of preparation method of zirconia film material |
| CN111293230A (en) * | 2018-12-10 | 2020-06-16 | 广东聚华印刷显示技术有限公司 | Thin film packaging layer and preparation method thereof, and preparation method of display panel |
| CN113526877A (en) * | 2021-07-27 | 2021-10-22 | 中国航发北京航空材料研究院 | Preparation method and device of coated glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686891A (en) * | 2005-04-29 | 2005-10-26 | 西安陆通科技发展有限公司 | Method for preparing nano multiple films on surface of glass |
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2014
- 2014-03-20 CN CN201410105524.7A patent/CN103936059B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1686891A (en) * | 2005-04-29 | 2005-10-26 | 西安陆通科技发展有限公司 | Method for preparing nano multiple films on surface of glass |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699870A (en) * | 2017-09-18 | 2018-02-16 | 中山大学 | Method for manufacturing thin film and system in hypergravity chemical deposition pipe |
| CN108409154A (en) * | 2018-03-22 | 2018-08-17 | 燕山大学 | A kind of preparation method of the FTO-G laminated films with micro-nano cluster surface topography |
| CN108409154B (en) * | 2018-03-22 | 2020-11-06 | 燕山大学 | Preparation method of FTO-G composite film with micro-nano cluster surface morphology |
| CN111293230A (en) * | 2018-12-10 | 2020-06-16 | 广东聚华印刷显示技术有限公司 | Thin film packaging layer and preparation method thereof, and preparation method of display panel |
| CN110256070A (en) * | 2019-07-31 | 2019-09-20 | 三祥新材股份有限公司 | A kind of preparation method of zirconia film material |
| CN110256070B (en) * | 2019-07-31 | 2022-05-17 | 三祥新材股份有限公司 | Preparation method of zirconia film material |
| CN113526877A (en) * | 2021-07-27 | 2021-10-22 | 中国航发北京航空材料研究院 | Preparation method and device of coated glass |
| CN113526877B (en) * | 2021-07-27 | 2023-04-14 | 中国航发北京航空材料研究院 | Preparation method and device of coated glass |
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