CN107986637A - A kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization - Google Patents
A kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization, comprise the following steps that：Step 1, colloidal sol is prepared：The inorganic salts of benzoylacetone, indium are added in ethanol successively, when stirring 1 is small in 50 DEG C~60 DEG C of oil bath, after being cooled to room temperature, continue the chlorate and acetic anhydride of addition tin, be stirred at room temperature 2 it is small when, be eventually adding polyethylene glycol, ITO colloidal sols obtained after stirring evenly；Step 2, gel mould is prepared：By the ITO colloidal sols even application being prepared by step 1 on soda-lime glass substrate, gel mould is formed；Step 3, gel mould is heat-treated：By the gel mould being prepared by step 2 be put into heat-treatment furnace at 450 DEG C~550 DEG C insulation 2 it is small when, be air-cooled to room temperature and obtain the tin-doped indium oxide nano-crystal film of in-situ crystallization.Preparation method technique of the invention is simple, utilization rate of raw materials is high, can large area film.
Description
Technical field
The invention belongs to photoelectron technical field, and in particular to a kind of tin-doped indium oxide nano-crystal film of in-situ crystallization
Preparation method.
Background technology
Tin-doped indium oxide (Indium Tin Oxide, abbreviation ITO) film is visible with good electric conductivity, height because of it
Light transmission rate, senior middle school's far infrared reflectivity and ultraviolet shielded ability, can be applied to low emissivity glass (Low-e glass) field, rise
To daylighting and the effect of isolation mid and far infrared heat radiation, there is very big development prospect in building energy saving field.It is but traditional
The optical characteristics of Low-e glass is static, and intake of the house to sun heat radiation can not be adjusted according to human wants.It is logical
Refinement ito thin film crystal grain is crossed to nanoscale and is assembled into Electrochromic glass device, using ITO nano-crystal films as work electricity
Pole, the carbonic allyl ester solution etc. of lithium perchlorate are electrolyte, the transparent conductive film of low carrier concentration is to electrode, are used
The method of electrochemical doping can adjust the nanocrystalline local surface plasma oscillation frequencies of working electrode ITO, and then adjust ITO
The local surface plasmon absorption wave band of nano-crystal film, realizes its electrochromism near infrared region.So ITO is nanocrystalline
Film is expected to extend the use function of traditional Low-e glass, it is not only had static energy-saving effect, but also can basis
Perception of the mankind to environment temperature adjustment in due course reaches intelligence and adjusts living environment temperature through the sun heat radiation of windowpane
Purpose.The patent of invention of Application No. 201280036901.5 is exactly according to this nanocrystalline feature of ITO, discloses one kind " ITO
Nanocrystalline-oxide " laminated film and preparation method thereof, wherein being related to the nanocrystalline preparation methods of ITO indirectly, it uses glue
It is nanocrystalline that body chemical technology obtains the ITO with cap.Combined finally by with other materials, prepare colloidal sol, prepare film.This
In preparation method, crystallization with collosol and gel be film-made be carried out separately, complex process, and colloid chemistry technology need to comprising
Suspension nanocrystalline ITO such as is centrifuged, is dissolved and washed away, being purified at the process, and raw material losses are serious, in addition when producing in enormous quantities,
Since raw material usage is excessive, ITO is nanocrystalline easily to occur precipitation of reuniting, it is difficult to obtains the colloidal sol of performance stabilization, can not realize
Uniformly film.Therefore, a kind of preparation method of new ITO nano-crystal films is developed, abandons colloid technology of preparing, it is thin to shorten ITO
The preparation section of film, realizes that industrialization is produced in enormous quantities, extremely urgent.
The content of the invention
The object of the present invention is to provide a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization, its work
Skill is simple, utilization rate of raw materials is high, can large area film.
The technical solution adopted in the present invention is a kind of preparation side of the tin-doped indium oxide nano-crystal film of in-situ crystallization
Method, comprises the following steps that：
Step 1, colloidal sol is prepared：The inorganic salts of benzoylacetone, indium are added in ethanol successively, in 50 DEG C~60 DEG C of oil
In bath stirring 1 it is small when, after being cooled to room temperature, continue add tin chlorate and acetic anhydride, be stirred at room temperature 2 it is small when, be eventually adding
Polyethylene glycol, obtains ITO colloidal sols after stirring evenly；
Step 2, gel mould is prepared：By the ITO colloidal sols even application being prepared by step 1 on soda-lime glass substrate,
Form gel mould；
Step 3, gel mould is heat-treated：By the gel mould being prepared by step 2 be put into heat-treatment furnace in 450 DEG C~
When insulation 2 is small at 550 DEG C, it is air-cooled to room temperature and obtains the tin-doped indium oxide nano-crystal film of in-situ crystallization.
It is of the invention to be further characterized in that,
In step 1, it is as follows to prepare the raw materials used proportioning of colloidal sol：The inorganic salts of indium, the chlorate of tin, ethanol, benzoyl third
The molar ratio of ketone, acetic anhydride and polyethylene glycol is 1：0.075~0.15：50~55：7~7.5：1.5~2：0.3~0.35.
In step 1, the inorganic salts of indium are indium nitrate or inidum chloride；The chlorate of tin is butter of tin or stannous chloride.
In step 1, the rh value in environment when preparing colloidal sol is 30%~100%.
In step 2, using Best-Effort request technology by the ITO colloidal sol even applications being prepared by step 1 in soda-lime glass
On substrate；The technological parameter of Best-Effort request technology is：Dip time is 1s~10s, and pull rate is 0.3cm/s~1.5cm/s,
Air humidity is not more than 40%.
In step 2, using spin coating technique by the ITO colloidal sols even application being prepared by step 1 in soda-lime glass substrate
On；The technological parameter of spin coating technique is：The rotating speed used is 2500 revs/min~4000 revs/min, needed for every milliliter of ITO colloidal sols
Spin-coating time is 150s~300s, and air humidity is not more than 40%.
The tin-doped indium oxide nano-crystalline thin film thickness for the in-situ crystallization that step 3 is prepared is 200nm~400nm.
The crystallite dimension of the tin-doped indium oxide nano-crystal film for the in-situ crystallization that step 3 is prepared is 5nm~20nm.
The carrier concentration of the tin-doped indium oxide nano-crystal film for the in-situ crystallization that step 3 is prepared is 5 × 1019
A/cm3~3 × 1021A/cm3。
The invention has the advantages that this preparation method need not dissolve and wash away colloidal sol, centrifuges, purify, production is avoided
The loss of thing, and special vacuum environment and reative cell is not required in this method, and appropriateness adjusts ambient humidity, general the South and the North
Room temperature environment can meet requirement of the film preparation to environment, thus manufacturing cost it is relatively low, can large area high-volume be film-made.
Embodiment
With reference to embodiment, the present invention is described in detail.
A kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization of the present invention, comprises the following steps that：
Step 1, colloidal sol is prepared：The inorganic salts of benzoylacetone, indium are added in ethanol successively, in 50 DEG C~60 DEG C of oil
In bath stirring 1 it is small when, after being cooled to room temperature, continue add tin chlorate and acetic anhydride, be stirred at room temperature 2 it is small when, be eventually adding
Polyethylene glycol, obtains ITO colloidal sols after stirring evenly；
In step 1, it is as follows to prepare the raw materials used proportioning of colloidal sol：The inorganic salts of indium, the chlorate of tin, ethanol, benzoyl third
The molar ratio of ketone, acetic anhydride and polyethylene glycol is 1：0.075~0.15：50~55：7~7.5：1.5~2：0.3~0.35；
In step 1, the inorganic salts of the indium are indium nitrate or inidum chloride；The chlorate of the tin is butter of tin or dichloro
Change tin；
In step 1, the rh value in environment when preparing colloidal sol is 30%~100%；
Step 2, gel mould is prepared：By the ITO colloidal sols even application being prepared by step 1 on soda-lime glass substrate,
Form gel mould；
In step 2, using Best-Effort request technology by the ITO colloidal sol even applications being prepared by step 1 in soda-lime glass
On substrate；The technological parameter of Best-Effort request technology is：Dip time is 1s~10s, and pull rate is 0.3cm/s~1.5cm/s,
Air humidity is not more than 40%；
In step 2, using spin coating technique by the ITO colloidal sols even application being prepared by step 1 in soda-lime glass substrate
On；The technological parameter of spin coating technique is：The rotating speed used is 2500 revs/min~4000 revs/min, needed for every milliliter of ITO colloidal sols
Spin-coating time is 150s~300s, and air humidity is not more than 40%；
Step 3, gel mould is heat-treated：By the gel mould being prepared by step 2 be put into heat-treatment furnace in 450 DEG C~
When insulation 2 is small at 550 DEG C, it is air-cooled to room temperature and obtains the tin-doped indium oxide nano-crystal film of in-situ crystallization.
The tin-doped indium oxide nano-crystalline thin film thickness for the in-situ crystallization that step 3 is prepared is 200nm~400nm.
The crystallite dimension of the tin-doped indium oxide nano-crystal film for the in-situ crystallization that step 3 is prepared is 5nm~20nm.
The carrier concentration of the tin-doped indium oxide nano-crystal film for the in-situ crystallization that step 3 is prepared is 5 × 1019
A/cm3~3 × 1021A/cm3。
Embodiment 1
A kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization, comprises the following steps that：
With indium nitrate In (NO3)3·4.5H2O and butter of tin SnCl4·5H2O is raw material, and benzoylacetone (BzAcH) is change
Dressing agent is learned, ethanol is that solvent, acetic anhydride and polyethylene glycol prepare colloidal sol for additive.Gel is prepared using dip-coating method
Film, finally carries out heat treatment and obtains ito thin film.
The BzAcH of 14.87g is dissolved in the ethanol of 30.16g first, 5.00g indium nitrates are then added, in 50 DEG C of oil
In bath stirring 1 it is small when, obtain yellow solution, after colloidal sol is cooled to room temperature, thereto add 0.34g butter of tin and
The acetic anhydride of 2.00g, be stirred at room temperature 2 it is small when, be eventually adding the polyethylene glycol of 2.36g, bronzing character obtained after stirring evenly
Transparent ITO colloidal sols, wherein operation room ambient humidity are 30%, indium nitrate in colloidal sol：Butter of tin：Ethanol：Benzoylacetone：Second
Acid anhydrides：Polyethylene glycol=1：0.075：50：7：1.5：0.3 (molar ratio).
Then, using Best-Effort request technology, by the ITO colloidal sols even application prepared on common soda lime glass substrate,
Gel mould is formed, wherein, dip time is 1 second, pull rate 0.3cm/s, air humidity 10%.
Finally, by the gel mould of preparation be put into heat-treatment furnace at 450 DEG C insulation 2 it is small when, be then drawn off, it is air-cooled
The ITO nano-crystal films of water white transparency are obtained to room temperature.
Finally, the ito thin film thickness of preparation is 200nm, and crystallite dimension 5nm, carrier concentration is 5 × 1019A/cm3。
The film has preferable near-infrared electrochromic property, its at 2000nm colour fading contrast be 65%, coloration time
800ms, fading time 1s, colour fading circulation 50,000 times, colour fading contrast performance and decline only 3%.
Embodiment 2
A kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization, comprises the following steps that：
With indium nitrate In (NO3)3·4.5H2O and butter of tin SnCl4·5H2O is raw material, and benzoylacetone (BzAcH) is change
Dressing agent is learned, ethanol is that solvent, acetic anhydride and polyethylene glycol prepare colloidal sol for additive.Gel mould is prepared using spin-coating method, most
After carry out heat treatment obtain ito thin film.
The BzAcH of 15.93g is dissolved in the ethanol of 33.22g first, 5.00g indium nitrates are then added, in 60 DEG C of oil
In bath stirring 1 it is small when, obtain yellow solution, after colloidal sol is cooled to room temperature, thereto add 0.68g butter of tin and
The acetic anhydride of 2.67g, be stirred at room temperature 2 it is small when, be eventually adding the polyethylene glycol of 2.75g, bronzing character obtained after stirring evenly
Transparent ITO colloidal sols, wherein operation room ambient humidity are 100%, indium nitrate in colloidal sol：Butter of tin：Ethanol：Benzoylacetone：
Acetic anhydride：Polyethylene glycol=1：0.15：55：7.5：2：0.35 (molar ratio).
Then, using spin coating technique, by the ITO colloidal sols even application prepared on common soda lime glass substrate, formed
Gel mould, wherein, rotating speed is 4000 revs/min, and the spin-coating time needed for every milliliter of colloidal sol is 150s, air humidity 40%.
Finally, by the gel mould of preparation be put into heat-treatment furnace at 550 DEG C insulation 2 it is small when, be then drawn off, it is air-cooled
The ITO nano-crystal films of water white transparency are obtained to room temperature.
Finally, the ito thin film thickness of preparation is 250nm, and crystallite dimension 20nm, carrier concentration is 3 × 1021A/
cm3.The film has preferable near-infrared electrochromic property, its at 2000nm colour fading contrast be 70%, coloring
Time 700ms, fading time 900ms, colour fading circulation 50,000 times, colour fading contrast performance and decline only 1%.
Embodiment 3
A kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization, comprises the following steps that：
With indium nitrate In (NO3)3·4.5H2O and butter of tin SnCl4·5H2O is raw material, and benzoylacetone (BzAcH) is change
Dressing agent is learned, ethanol is that solvent, acetic anhydride and polyethylene glycol prepare colloidal sol for additive.Gel is prepared using dip-coating method
Film, finally carries out heat treatment and obtains ito thin film.
The BzAcH of 15.30g is dissolved in the ethanol of 31.40g first, 5.00g indium nitrates are then added, in 55 DEG C of oil
In bath stirring 1 it is small when, obtain yellow solution, after colloidal sol is cooled to room temperature, thereto add 0.46g butter of tin and
The acetic anhydride of 2.41g, be stirred at room temperature 2 it is small when, be eventually adding the polyethylene glycol of 2.59g, bronzing character obtained after stirring evenly
Transparent ITO colloidal sols, wherein operation room ambient humidity are 70%, indium nitrate in colloidal sol：Butter of tin：Ethanol：Benzoylacetone：Second
Acid anhydrides：Polyethylene glycol=1：0.1：52：7.2：1.8：0.33 (molar ratio).
Then, using Best-Effort request technology, by the ITO colloidal sols even application prepared on common soda lime glass substrate,
Gel mould is formed, wherein, dip time is 10 seconds, pull rate 1.5cm/s, air humidity 30%.
Finally, by the gel mould of preparation be put into heat-treatment furnace at 500 DEG C insulation 2 it is small when, be then drawn off, it is air-cooled
The ITO nano-crystal films of water white transparency are obtained to room temperature.
Finally, the ito thin film thickness of preparation is 400nm, and crystallite dimension 12nm, carrier concentration is 8 × 1020A/
cm3.The film has preferable near-infrared electrochromic property, its at 2000nm colour fading contrast be 80%, coloring
Time 750ms, fading time 900s, colour fading circulation 50,000 times, colour fading contrast performance and decline only 1%.
Embodiment 4
A kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization, comprises the following steps that：
With indium nitrate In (NO3)3·4.5H2O and butter of tin SnCl4·5H2O is raw material, and benzoylacetone (BzAcH) is change
Dressing agent is learned, ethanol is that solvent, acetic anhydride and polyethylene glycol prepare colloidal sol for additive.Gel is prepared using dip-coating method
Film, finally carries out heat treatment and obtains ito thin film.
The BzAcH of 15.30g is dissolved in the ethanol of 30.20g first, 5.00g indium nitrates are then added, in 57 DEG C of oil
In bath stirring 1 it is small when, obtain yellow solution, after colloidal sol is cooled to room temperature, thereto add 0.55g butter of tin and
The acetic anhydride of 2.67g, be stirred at room temperature 2 it is small when, be eventually adding the polyethylene glycol of 2.75g, bronzing character obtained after stirring evenly
Transparent ITO colloidal sols, wherein operation room ambient humidity are 50%, indium nitrate in colloidal sol：Butter of tin：Ethanol：Benzoylacetone：Second
Acid anhydrides：Polyethylene glycol=1：0.12：50：7.2：2：0.35.
Then, using Best-Effort request technology, by the ITO colloidal sols even application prepared on common soda lime glass substrate,
Gel mould is formed, wherein, dip time is 5 seconds, pull rate 1.0cm/s, air humidity 35%.
Finally, by the gel mould of preparation be put into heat-treatment furnace at 520 DEG C insulation 2 it is small when, be then drawn off, it is air-cooled
The ITO nano-crystal films of water white transparency are obtained to room temperature.
Finally, the ito thin film thickness of preparation is 350nm, and crystallite dimension 15nm, carrier concentration is 9 × 1020A/
cm3.The film has preferable near-infrared electrochromic property, its at 2000nm colour fading contrast be 76%, coloring
Time 850ms, fading time 950s, colour fading circulation 50,000 times, colour fading contrast performance and decline only 2%.
Embodiment 5
A kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization, comprises the following steps that：
With indium nitrate In (NO3)3·4.5H2O and butter of tin SnCl4·5H2O is raw material, and benzoylacetone (BzAcH) is change
Dressing agent is learned, ethanol is that solvent, acetic anhydride and polyethylene glycol prepare colloidal sol for additive.Gel mould is prepared using spin-coating method, most
After carry out heat treatment obtain ito thin film.
The BzAcH of 14.87g is dissolved in the ethanol of 33.22g first, 5.00g indium nitrates are then added, in 53 DEG C of oil
In bath stirring 1 it is small when, obtain yellow solution, after colloidal sol is cooled to room temperature, thereto add 0.51g butter of tin and
The acetic anhydride of 2.00g, be stirred at room temperature 2 it is small when, be eventually adding the polyethylene glycol of 2.36g, bronzing character obtained after stirring evenly
Transparent ITO colloidal sols, wherein operation room ambient humidity are 50%, indium nitrate in colloidal sol：Butter of tin：Ethanol：Benzoylacetone：Second
Acid anhydrides：Polyethylene glycol=1：0.11：55：7：1.5：0.3.
Then, using spin coating technique, by the ITO colloidal sols even application prepared on common soda lime glass substrate, formed
Gel mould, wherein, rotating speed is 2500 revs/min, and the spin-coating time needed for every milliliter of colloidal sol is 300s, air humidity 20%.
Finally, by the gel mould of preparation be put into heat-treatment furnace at 500 DEG C insulation 2 it is small when, be then drawn off, it is air-cooled
The ITO nano-crystal films of water white transparency are obtained to room temperature.
Finally, the ito thin film thickness of preparation is 380nm, and crystallite dimension 11nm, carrier concentration is 8.5 × 1020A/
cm3.The film has preferable near-infrared electrochromic property, its at 2000nm colour fading contrast be 72%, coloring
Time 1s, fading time 1.5s, colour fading circulation 50,000 times, colour fading contrast performance and decline only 4%.
Embodiment 6
A kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization, comprises the following steps that：
With indium nitrate In (NO3)3·4.5H2O and butter of tin SnCl4·5H2O is raw material, and benzoylacetone (BzAcH) is change
Dressing agent is learned, ethanol is that solvent, acetic anhydride and polyethylene glycol prepare colloidal sol for additive.Gel mould is prepared using spin-coating method, most
After carry out heat treatment obtain ito thin film.
The BzAcH of 15.72g is dissolved in the ethanol of 30.80g first, 5.00g indium nitrates are then added, in 60 DEG C of oil
In bath stirring 1 it is small when, obtain yellow solution, after colloidal sol is cooled to room temperature, thereto add 0.39g butter of tin and
The acetic anhydride of 2.34g, be stirred at room temperature 2 it is small when, be eventually adding the polyethylene glycol of 2.44g, bronzing character obtained after stirring evenly
Transparent ITO colloidal sols, wherein operation room ambient humidity are 40%, indium nitrate in colloidal sol：Butter of tin：Ethanol：Benzoylacetone：Second
Acid anhydrides：Polyethylene glycol=1：0.085：51：7.4：1.75：0.31.
Then, using spin coating technique, by the ITO colloidal sols even application prepared on common soda lime glass substrate, formed
Gel mould, wherein, rotating speed is 3000 revs/min, and the spin-coating time needed for every milliliter of colloidal sol is 200s, air humidity 35%.
Finally, by the gel mould of preparation be put into heat-treatment furnace at 480 DEG C insulation 2 it is small when, be then drawn off, it is air-cooled
The ITO nano-crystal films of water white transparency are obtained to room temperature.
Finally, the ito thin film thickness of preparation is 300nm, and crystallite dimension 8nm, carrier concentration is 4.5 × 1020A/
cm3.The film has preferable near-infrared electrochromic property, its at 2000nm colour fading contrast be 68%, coloring
Time 1.5s, fading time 2s, colour fading circulation 50,000 times, colour fading contrast performance and decline only 3.5%.
Advantages of the present invention is that this preparation method need not dissolve and wash away colloidal sol, centrifuges, purify, and avoid product
It is lost in, and special vacuum environment and reative cell is not required in this method, and appropriateness adjusts ambient humidity, general southern and northern room temperature
Environment can meet requirement of the film preparation to environment, thus manufacturing cost it is relatively low, can large area high-volume be film-made；By this system
Nanocrystalline size in film prepared by Preparation Method is controllable, is firmly combined with substrate, the electroluminescent change of ITO nano-crystal films of acquisition
Color better performances.
Claims (9)
1. the preparation method of the tin-doped indium oxide nano-crystal film of a kind of in-situ crystallization, it is characterised in that comprise the following steps that：
Step 1, colloidal sol is prepared：The inorganic salts of benzoylacetone, indium are added in ethanol successively, in 50 DEG C~60 DEG C of oil bath
Stir 1 it is small when, after being cooled to room temperature, continue add tin chlorate and acetic anhydride, be stirred at room temperature 2 it is small when, be eventually adding poly- second
Glycol, obtains ITO colloidal sols after stirring evenly；
Step 2, gel mould is prepared：By the ITO colloidal sols even application being prepared by step 1 on soda-lime glass substrate, formed
Gel mould；
Step 3, gel mould is heat-treated：The gel mould being prepared by step 2 is put into heat-treatment furnace in 450 DEG C~550 DEG C
It is lower insulation 2 it is small when, be air-cooled to room temperature and obtain the tin-doped indium oxide nano-crystal film of in-situ crystallization.
2. a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization according to claim 1, it is special
Sign is, in step 1, it is as follows to prepare the raw materials used proportioning of colloidal sol：The inorganic salts of indium, the chlorate of tin, ethanol, benzoyl third
The molar ratio of ketone, acetic anhydride and polyethylene glycol is 1：0.075~0.15：50~55：7~7.5：1.5~2：0.3~0.35.
3. a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization according to claim 1, it is special
Sign is, in step 1, the inorganic salts of the indium are indium nitrate or inidum chloride；The chlorate of the tin is butter of tin or dichloro
Change tin.
4. a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization according to claim 1, it is special
Sign is, in step 1, the rh value in environment when preparing colloidal sol is 30%~100%.
5. a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization according to claim 1, it is special
Sign is, in step 2, using Best-Effort request technology by the ITO colloidal sols even application being prepared by step 1 in soda-lime glass base
On plate；The technological parameter of Best-Effort request technology is：Dip time is 1s~10s, and pull rate is 0.3cm/s~1.5cm/s, empty
Air humidity degree is not more than 40%.
6. a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization according to claim 1, it is special
Sign is, in step 2, using spin coating technique by the ITO colloidal sols even application being prepared by step 1 in soda-lime glass substrate
On；The technological parameter of spin coating technique is：The rotating speed used is 2500 revs/min~4000 revs/min, needed for every milliliter of ITO colloidal sols
Spin-coating time is 150s~300s, and air humidity is not more than 40%.
7. a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization according to claim 1, it is special
Sign is that the tin-doped indium oxide nano-crystalline thin film thickness for the in-situ crystallization that step 3 is prepared is 200nm~400nm.
8. a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization according to claim 1, it is special
Sign is that the crystallite dimension of the tin-doped indium oxide nano-crystal film for the in-situ crystallization that step 3 is prepared is 5nm~20nm.
9. a kind of preparation method of the tin-doped indium oxide nano-crystal film of in-situ crystallization according to claim 1, it is special
Sign is that the carrier concentration of the tin-doped indium oxide nano-crystal film for the in-situ crystallization that step 3 is prepared is 5 × 1019A/
cm3~3 × 1021A/cm3。
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| CN1599024A (en) * | 2004-07-30 | 2005-03-23 | 西安理工大学 | Tin-doped indium oxide film and making process of fine pattern |
| CN105036564A (en) * | 2015-06-25 | 2015-11-11 | 西安理工大学 | Nanocrystalline enhanced tungsten oxide electrochromic film and preparation method thereof |
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| CN1599024A (en) * | 2004-07-30 | 2005-03-23 | 西安理工大学 | Tin-doped indium oxide film and making process of fine pattern |
| CN105036564A (en) * | 2015-06-25 | 2015-11-11 | 西安理工大学 | Nanocrystalline enhanced tungsten oxide electrochromic film and preparation method thereof |
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| CN113816615A (en) * | 2021-08-31 | 2021-12-21 | 西安理工大学 | Ultrahigh-transparency conductive ITO film and preparation method thereof |
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