CN103922609B - Preparation method of a kind of colloid ITO nano-crystal film and products thereof - Google Patents
Preparation method of a kind of colloid ITO nano-crystal film and products thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of colloid ITO nano-crystal film, first nanocrystalline for colloid ITO being dissolved in non-polar solvent is obtained solution, described solution is coated in substrate, obtains film; Configuration concentration is the alkali organic solution of 1 ~ 100g/L, and described film immerses 1 ~ 100s in alkali organic solution, obtains pretreated film; Again indium salt, pink salt and ignition dope are dissolved in organic solvent and obtain mixing solutions, described mixing solutions is coated on pretreated film, under vacuum condition, at 50 ~ 200 DEG C of thermal treatment 0.5 ~ 30h; Finally by deep UV (ultraviolet light) or plasma treatment 1 ~ 120min, obtain described colloid ITO nano-crystal film.Present method is simple, controllability good, with low cost, is easy to suitability for industrialized production; The transparent conductive film prepared has the advantages that transmitance is high, resistivity is low, film quality is good.
Description
Technical field
The present invention relates to the preparation field of nano material and device, be specifically related to preparation method of a kind of colloid ITO nano-crystal film and products thereof.
Background technology
ITO(tin-doped indium oxide IndiumTinOxide) be a kind of N-shaped oxide semiconductor material of degeneracy, it is usually used to as transparent conductive film, has the extraordinary transparency and the good electroconductibility of the metal that matches in excellence or beauty at visible light wave range.Energy gap under room temperature is about 4eV, having adjustable and higher work function, is the hole transport layer material of photoelectric device and the material of conductive electrode and electronic product touch-screen such as organic thin film solar cell, Organic Light Emitting Diode, light emitting diode with quantum dots under the gentle higher temperature of preparation room.
The surface atom number of nano-ITO is very big with the ratio of body phase atomicity, demonstrate volume effect, quantum size effect, surface effects and macro quanta tunnel effect thus, many performances are better than common ITO, purposes is more extensive, at present, the method preparing nano-ITO is a lot, as solid reaction process, chemical precipitation method and sol-gel method etc.
Colloid nanocrystalline (colloidalnanocrystal) not only has the character of solid nano material but also has according to the difference of its surface ligand and be dissolvable in water water and have or the feature of machine solvent, especially its synthesis device and technique are very simple, and cost is very cheap.
(the Zhou Limin such as Zhou Limin, Jin Yizheng, Ren Yuping, Yi Qing. the controlledly synthesis that indium tin oxygen (ITO) is nanocrystalline. Materials Science and Engineering journal, 30th volume the 6th phase) adopt easy " one kettle way ", in reaction system, adopt the n-caprylic acid salt of straight chain or have the 2-ethylhexoate of linear chain structure, prepare surperficial nanocrystalline with the colloid ITO of long-chain organism part under 280 degrees Celsius, this colloid ITO is nanocrystalline can be the good spherical nanocrystalline or nano flower of monodispersity.
But, the colloid ITO prepared due to solution method is with Long carbon chain part, have a strong impact on the electric conductivity after its film forming as insulation barrier, therefore often require high-temperature heat treatment (>300 DEG C) after its film forming, limit its application on organic flexible substrate.Do not have the report to colloid ITO nanocrystalline material low temperature (<200 DEG C) film forming and process thereof at present.
Summary of the invention
The invention provides a kind of preparation method of colloid ITO nano-crystal film, method is simple, controllability good, with low cost, is easy to suitability for industrialized production; The transparent conductive film prepared has the advantages that transmitance is high, resistivity is low, film quality is good.
The invention discloses a kind of preparation method of colloid ITO nano-crystal film, comprise the following steps:
1) be mixed to get solution by nanocrystalline for colloid ITO with non-polar solvent, described solution be coated in substrate, obtain film;
Described non-polar solvent is the non-polar organic solvent that boiling point is less than 200 DEG C;
The concentration that in described solution, colloid ITO is nanocrystalline is 1 ~ 100g/L;
2) configuration concentration is the alkali organic solution of 1 ~ 100g/L, and film step 1) obtained immerses 1 ~ 100s in alkali organic solution, obtains pretreated film;
3) indium salt, pink salt and ignition dope be dissolved in organic solvent obtain mixing solutions, described mixing solutions is coated on step 2) on the pretreated film that obtains, under vacuum condition, at 50 ~ 200 DEG C of thermal treatment 0.5 ~ 30h;
Ammonium nitrate and the methyl ethyl diketone of described ignition dope to be mol ratio be 1:1 ~ 3;
In described mixing solutions, the concentration of indium salt is 0.2 ~ 0.6mol/L;
The mol ratio of described pink salt, indium salt and ignition dope is 1:6 ~ 12:6 ~ 12.
4) the film deep UV (ultraviolet light) after the thermal treatment that obtains of step 3) or plasma treatment 1 ~ 120min, obtain described colloid ITO nano-crystal film.
The present invention is nanocrystalline for raw material with colloid ITO, by after simple film forming again through ligand exchange reaction, directly can remove the long-chain organism part of colloid ITO nanocrystal surface; After above-mentioned steps process, film surface has more crackle or hole, therefore plugs the gap through spin coating one deck presoma again, ensures the complete of film; Finally by deep UV (ultraviolet light) or plasma treatment to remove the O-H key of film surface, prepare and there is the transparent conductive film that transmitance is high, resistivity is low, film quality is good.
The present invention adopt colloid ITO nanocrystalline can pass through " controlledly synthesis that indium tin oxygen (ITO) is nanocrystalline " (Zhou Limin, Jin Yizheng, Ren Yuping, Yi Qing. Materials Science and Engineering journal, the 30th volume the 6th phase) in method prepare.
The colloid ITO adopting above-mentioned preparation method to obtain is nanocrystalline, and surface ligand is mainly long-chain organism, has better solvability in non-polar solvent.As preferably, the nanocrystalline particle diameter of the colloid ITO described in step 1) is 1 ~ 100nm; Further preferably, the particle diameter that described colloid ITO is nanocrystalline is 10 ~ 30nm.When the size of colloid nanocrystalline particle is too large, can produce more space between colloid nanocrystalline particle, cause density to decline, resistivity rises; And when colloid nanocrystalline particle size is too little time, because the contact resistance between individual particle is comparatively large, and the resistance of granule interior is less, and resistivity also can be caused to rise.
As preferably, the concentration that in the solution described in step 1), colloid ITO is nanocrystalline is 30 ~ 40g/L.During excessive concentration, in solution, there is the reunion macrobead that colloid ITO is nanocrystalline, prepared film surface unfairness; When concentration is too low, prepared film thickness is less, and surface resistance is relatively large.
As preferably, the non-polar solvent described in step 1) is Skellysolve A, normal hexane, normal heptane, octane, zellon, tetracol phenixin, benzene, toluene or dimethylbenzene.When the boiling point of solvent is too high, the viscosity of solvent can be relatively large, affects uniformity coefficient and the thickness of film forming.
Described substrate can be glass.
Step 2) described in alkali organic solution with at least one in Tetramethylammonium hydroxide (TMAH), potassium hydroxide, sodium hydroxide, sodium sulphite, ammonium sulfide, ammoniacal liquor for solute, with at least one in ethanol, ethylene glycol monomethyl ether, methyl alcohol, acetone, ethyl acetate, Virahol, n-propyl alcohol, dimethyl formamide for solvent.The selection demand fulfillment of described solute and solvent: solute has good solvability in a solvent.
As preferably, described alkali organic solution is the ethanolic soln of Tetramethylammonium hydroxide, and concentration is 10 ~ 20g/L, and the time that described film immerses alkali organic solution is 10 ~ 20s.TMAH compares other alkali and is soluble in ethanolic soln, reaction temperature and; TMAH is organism simultaneously, and excessive TMAH is easy by thermal treatment and ultraviolet light irradiation removing again.
Indium salt described in step 3) is at least one in indium nitrate, indium acetate, Indium Tris acetylacetonate, indium chloride, pink salt is at least one of tin chloride, tin protochloride, tin oxalate, isocaprylic acid tin, and organic solvent is at least one in ethanol, ethylene glycol monomethyl ether, methyl alcohol, acetone, ethyl acetate, Virahol, n-propyl alcohol, dimethyl formamide.
As preferably, in the ignition dope described in step 3), the mol ratio of ammonium nitrate and methyl ethyl diketone is 1:1.8 ~ 2.2.
As preferably, the mol ratio of the pink salt described in step 3) and indium salt is 1:8 ~ 10.
Described deep UV (ultraviolet light) is the UV-light of wavelength lower than 300nm, and as preferably, the illumination wavelength of the deep UV (ultraviolet light) described in step 4) is 100 ~ 300nm, more preferably 200nm, and the treatment time is 5 ~ 60min.
Compared with prior art, tool of the present invention has the following advantages:
The present invention uses colloid ITO nanocrystalline preparation good conductivity, transparent conductive film that transmitance is high first at low temperatures, and the method goes for flexible substrate.
Treatment process of the present invention is simple, cost is lower, reproducible, be easy to suitability for industrialized production, is expected to the various fields such as the organic thin film solar cell based on solution method, Organic Light Emitting Diode, light emitting diode with quantum dots and is applied.
Accompanying drawing explanation
Fig. 1 is the TEM figure of film prepared by embodiment 1;
Fig. 2 is the FTIR figure of pretreated film prepared by embodiment 1;
Fig. 3 is the SEM figure of the film after the spin coating presoma of embodiment 1 preparation;
Fig. 4 is the XPS figure of colloid ITO nano-crystal film prepared by embodiment 1;
Fig. 5 is the transmitance figure of colloid ITO nano-crystal film prepared by embodiment 1;
Fig. 6 is the TEM figure of film prepared by embodiment 2;
Fig. 7 is the transmitance figure of colloid ITO nano-crystal film prepared by embodiment 2;
Fig. 8 is the TEM figure of film prepared by embodiment 3;
Fig. 9 is the transmitance figure of colloid ITO nano-crystal film prepared by embodiment 3.
Embodiment
Example below for adopting the inventive method to prepare colloid ITO nano-crystal film, but the present invention is not limited to these embodiments.
Colloid ITO below in all embodiments is nanocrystalline all adopts the preparation method in " controlledly synthesis that indium tin oxygen (ITO) is nanocrystalline " (Materials Science and Engineering journal, the 30th volume the 6th phase) to obtain.
Embodiment 1
1) being averaged particle diameter is that the colloid ITO of 30nm is nanocrystalline, is dissolved in normal hexane, is made into the solution of 40g/L, be spin-coated in substrate, obtain film by described solution.
2) configure the ethanolic soln of the TMAH of 10g/L, film step 1) obtained immerses 20s in TMAH solution, obtains pretreated film.
3) indium nitrate, tin protochloride are mixed with 2.5mL ethylene glycol monomethyl ether, configuration mixing solutions, in mixing solutions, the concentration of indium nitrate is 0.4mol/L, the concentration of tin protochloride is 0.04mol/L, ammonium nitrate 1mmol is added again, methyl ethyl diketone 2mmol, mix and blend 8h in mixing solutions.Solution after mixing is spun on step 2) pretreated film on.Subsequently by film under 180 DEG C of vacuum conditions, thermal treatment 1h.
4) film after thermal treatment step 3) obtained, under 150 degrees Celsius of vacuum conditions, irradiates 30min by the deep UV (ultraviolet light) of 200nm.
Fig. 1 is the TEM figure of film prepared by the present embodiment step 1), and can count its median size from figure is 30nm.
Fig. 2 is the present embodiment step 2) process the FTIR figure of forward and backward pre-treatment film, observe known, at 2750 ~ 3000cm before ligand exchange
-1between have two CH
2characteristic peak, show there is the organic existence of long-chain in film, exchange after 20s, these two peaks disappear.
Fig. 3 is the SEM figure of the forward and backward colloid ITO nano-crystal film of the present embodiment step 3) spin coating presoma, and observe known, before spin coating presoma (left figure), pretreated film is through step 2) process after there is very many holes.After spin coating presoma (right figure), obtain fine and close and complete film.
Fig. 4 is the XPS figure of the forward and backward colloid ITO nano-crystal film of the present embodiment step 4) process, as we can see from the figure, through deep UV (ultraviolet light) or the process of plasma cleaning instrument, XPS represents O-H key in conjunction with energy 532eV peak completely dissolve, only be left the peak being positioned at the In-O key of 530eV after process, show that processing rear O-H key is converted into In-O key.
Fig. 5 is the transmitance figure of colloid ITO nano-crystal film prepared by the present embodiment, and as we can see from the figure, the film of preparation has the transmitance of >90% at visible light wave range, have the extraordinary transparency.
Tested by Hall instrument, the resistivity of colloid ITO nano-crystal film prepared by the present embodiment is 8.23 × 10
-3Ω cm.The surface resistance obtaining the film of 280nm thickness after two-layer spin coating is 294 Ω/sq.
Embodiment 2
1) be averaged the colloid ITO being of a size of 10nm nanocrystalline, be dissolved in normal hexane, be mixed with the solution of 30g/L, described solution is coated in substrate, through spin-coat process, obtain film.
2) ethanolic soln of the TMAH of 20g/L is configured.Film step 1) obtained immerses 10s in alkaline solution, obtains pretreated film.
3) indium nitrate, tin protochloride are mixed with 2.5mL ethylene glycol monomethyl ether, configuration mixing solutions, in mixing solutions, the concentration of indium nitrate is 0.4mol/L, the concentration of tin protochloride is 0.04mol/L, ammonium nitrate 1mmol is added again, methyl ethyl diketone 2mmol, mix and blend 8h in mixing solutions.By on the film of the solution spin coating after mixing and step 1).Subsequently by film under 150 DEG C of vacuum conditions, thermal treatment 3h.
4) film after thermal treatment step 3) obtained, under 100 degrees Celsius of vacuum conditions, irradiates 60min by the deep UV (ultraviolet light) of 200nm.
Fig. 6 is the TEM figure of film prepared by the present embodiment step 1), and can count its median size from figure is 10nm.
Fig. 7 is the transmitance figure of colloid ITO nano-crystal film prepared by the present embodiment, and as we can see from the figure, the film of preparation has the transmitance of >90% at visible light wave range, have the extraordinary transparency.
Tested by Hall instrument, the resistivity of colloid ITO nano-crystal film prepared by the present embodiment is 2.6 × 10
-2Ω cm, the surface resistance obtaining the film of 200nm thickness after two-layer spin coating is 1300 Ω/sq.
Embodiment 3
1) be averaged the colloid ITO being of a size of 20nm nanocrystalline, be dissolved in normal hexane, be mixed with the solution of 35g/L, described solution is coated in substrate, through spin-coat process, obtain film.
2) ethanolic soln of the TMAH of 20g/L is configured.Film step 1) obtained immerses 10s in alkaline solution, obtains pretreated film.
3) indium nitrate, tin protochloride are mixed with 2.5mL ethylene glycol monomethyl ether, configuration mixing solutions, in mixing solutions, the concentration of indium nitrate is 0.4mol/L, the concentration of tin protochloride is 0.04mol/L, ammonium nitrate 1mmol is added again, methyl ethyl diketone 2mmol, mix and blend 8h in mixing solutions.Solution after mixing is spun on step 2) pretreated film on.Subsequently by film under 120 DEG C of vacuum conditions, thermal treatment 10h.
4) film after thermal treatment step 3) obtained puts into plasma cleaning instrument, because plasma body can produce heat in treating processes, is equivalent to, by film heating to 50 ~ 100 degree Celsius, use oxygen plasma treatment 10min.
Fig. 8 is the TEM figure of film prepared by the present embodiment step 1), and can count its median size from figure is 20nm.
Fig. 9 is the transmitance figure of colloid ITO nano-crystal film prepared by the present embodiment, and as we can see from the figure, the film of preparation has the transmitance of >90% at visible light wave range, have the extraordinary transparency.
Tested by Hall instrument, the resistivity of colloid ITO nano-crystal film prepared by the present embodiment is 1.02 × 10
-2Ω cm, the surface resistance obtaining the film of 240nm thickness after two-layer spin coating is 425 Ω/sq.
Embodiment 4
1) be averaged the colloid ITO being of a size of 30nm nanocrystalline, be dissolved in normal heptane, be mixed with the solution of 35g/L, described solution is coated in substrate, through spin-coat process, obtain film.
2) (the NH of 20g/L is configured
4)
2the methanol solution of S.Film step 1) obtained immerses 15s in alkaline solution, obtains pretreated film.
3) indium nitrate, tin protochloride are mixed with 2.5mL ethylene glycol monomethyl ether, configuration mixing solutions, in mixing solutions, the concentration of indium nitrate is 0.4mol/L, the concentration of tin protochloride is 0.04mol/L, ammonium nitrate 1mmol is added again, methyl ethyl diketone 2mmol, mix and blend 8h in mixing solutions.Solution after mixing is spun on step 2) pretreated film on.Subsequently by film under 180 DEG C of vacuum conditions, thermal treatment 1h.
4) film after thermal treatment step 3) obtained, under 150 degrees Celsius of vacuum conditions, irradiates 30min by the deep UV (ultraviolet light) of 200nm.
Tested by Hall instrument, the resistivity of colloid ITO nano-crystal film prepared by the present embodiment is 9.2 × 10
-3Ω cm, the surface resistance obtaining the film of 220nm thickness after two-layer spin coating is 418 Ω/sq.
Embodiment 5
1) be averaged the colloid ITO being of a size of 30nm nanocrystalline, be dissolved in normal hexane, be mixed with the solution of 35g/L, described solution is coated in substrate, through spin-coat process, obtain film.
2) the DMF solution of the KOH of 30g/L is configured.Film step 1) obtained immerses 10s in alkaline solution, obtains pretreated film.
3) indium nitrate, tin protochloride are mixed with 2.5mL ethylene glycol monomethyl ether, configuration mixing solutions, in mixing solutions, the concentration of indium nitrate is 0.4mol/L, the concentration of tin protochloride is 0.04mol/L, ammonium nitrate 1mmol is added again, methyl ethyl diketone 2mmol, mix and blend 8h in mixing solutions.Solution after mixing is spun on step 2) pretreated film on.Subsequently by film under 120 DEG C of vacuum conditions, thermal treatment 10h.
4) film after thermal treatment step 3) obtained, under 150 degrees Celsius of vacuum conditions, irradiates 30min by the deep UV (ultraviolet light) of 200nm.
Tested by Hall instrument, the resistivity of colloid ITO nano-crystal film prepared by the present embodiment is 9.7 × 10
-2Ω cm, the surface resistance obtaining the film of 160nm thickness after two-layer spin coating is 606 Ω/sq.
Claims (10)
1. a preparation method for colloid ITO nano-crystal film, is characterized in that, comprises the following steps:
1) be mixed to get solution by nanocrystalline for colloid ITO with non-polar solvent, described solution be coated in substrate, obtain film;
Described non-polar solvent is the non-polar organic solvent that boiling point is less than 200 DEG C;
The concentration that in described solution, colloid ITO is nanocrystalline is 1 ~ 100g/L;
2) configuration concentration is the alkali organic solution of 1 ~ 100g/L, by step 1) film that obtains immerses 1 ~ 100s in alkali organic solution, obtains pretreated film;
3) indium salt, pink salt and ignition dope be dissolved in organic solvent obtain mixing solutions, described mixing solutions is coated on step 2) on the pretreated film that obtains, under vacuum condition, at 50 ~ 200 DEG C of thermal treatment 0.5 ~ 30h;
Ammonium nitrate and the methyl ethyl diketone of described ignition dope to be mol ratio be 1:1 ~ 3;
In described mixing solutions, the concentration of indium salt is 0.2 ~ 0.6mol/L;
The mol ratio of described pink salt, indium salt and ignition dope is 1:6 ~ 12:6 ~ 12;
4) step 3) film after the thermal treatment that obtains through deep UV (ultraviolet light) or plasma treatment 1 ~ 120min, obtain described colloid ITO nano-crystal film;
Step 2) described in alkali organic solution with at least one in Tetramethylammonium hydroxide, potassium hydroxide, sodium hydroxide, sodium sulphite, ammonium sulfide, ammoniacal liquor for solute, with at least one in ethanol, ethylene glycol monomethyl ether, methyl alcohol, acetone, ethyl acetate, Virahol, n-propyl alcohol, dimethyl formamide for solvent.
2. the preparation method of colloid ITO nano-crystal film according to claim 1, is characterized in that, step 1) described in the nanocrystalline particle diameter of colloid ITO be 1 ~ 100nm.
3. the preparation method of colloid ITO nano-crystal film according to claim 2, is characterized in that, step 1) described in the nanocrystalline particle diameter of colloid ITO be 10 ~ 30nm.
4. the preparation method of the colloid ITO nano-crystal film according to claim 1 or 2 or 3, is characterized in that, step 1) described in solution in the nanocrystalline concentration of colloid ITO be 30 ~ 40g/L.
5. the preparation method of colloid ITO nano-crystal film according to claim 1, is characterized in that, step 1) described in non-polar solvent be Skellysolve A, normal hexane, normal heptane, octane, zellon, tetracol phenixin, benzene, toluene or dimethylbenzene.
6. the preparation method of colloid ITO nano-crystal film according to claim 1, it is characterized in that, described alkali organic solution is the ethanolic soln of Tetramethylammonium hydroxide, and concentration is 10 ~ 20g/L, and the time that described film immerses alkali organic solution is 10 ~ 20s.
7. the preparation method of colloid ITO nano-crystal film according to claim 1, it is characterized in that, step 3) described in indium salt be at least one in indium nitrate, indium acetate, Indium Tris acetylacetonate, indium chloride, pink salt is at least one of tin chloride, tin protochloride, tin oxalate, isocaprylic acid tin, and organic solvent is at least one in ethanol, ethylene glycol monomethyl ether, methyl alcohol, acetone, ethyl acetate, Virahol, n-propyl alcohol, dimethyl formamide.
8. the preparation method of colloid ITO nano-crystal film according to claim 1, is characterized in that, step 3) described in ignition dope in, the mol ratio of ammonium nitrate and methyl ethyl diketone is 1:1.8 ~ 2.2; The mol ratio of pink salt and indium salt is 1:8 ~ 10.
9. the preparation method of colloid ITO nano-crystal film according to claim 1, is characterized in that, step 4) described in the illumination wavelength of deep UV (ultraviolet light) be 100 ~ 300nm, the treatment time is 5 ~ 60min.
10. the colloid ITO nano-crystal film that obtains of the preparation method according to the arbitrary claim of claim 1 ~ 9.
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| CN105776321B (en) * | 2014-12-23 | 2017-07-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Indium tin oxide nanocomposite solution, its preparation method and application |
| CN107512854B (en) * | 2017-08-17 | 2020-05-08 | 浙江大学 | ITO/WO with nano mosaic structure3Composite electrochromic film and preparation method thereof |
| CN108389801A (en) * | 2018-02-25 | 2018-08-10 | 青岛大学 | The method that one step photoetching process prepares metal-oxide semiconductor (MOS) and dielectric film |
| CN108807724B (en) * | 2018-06-14 | 2020-10-16 | 香港中文大学（深圳） | Preparation method and application of perovskite luminescent layer, perovskite luminescent device and preparation method thereof |
| CN111979561B (en) * | 2019-05-21 | 2022-08-26 | 南京理工大学 | SnOx/BiVO 4 Electrode, preparation method thereof and application of electrode in photoelectrocatalysis hydrogen peroxide synthesis |
| CN111599925B (en) * | 2020-05-29 | 2021-09-21 | 河南大学 | Solar cell with dimethyl tin bis (formate) N-type semiconductor film as electron transport layer and preparation method thereof |
| CN112420878B (en) * | 2020-12-21 | 2022-07-15 | 暨南大学 | All-inorganic CsPbBr3 perovskite solar cell with high-temperature-resistant flexible transparent electrode and preparation method and application thereof |
| CN113816615B (en) * | 2021-08-31 | 2023-06-16 | 西安理工大学 | Ultrahigh transparent conductive ITO film and preparation method thereof |
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| JP4512940B2 (en) * | 2003-12-24 | 2010-07-28 | 三菱マテリアル株式会社 | Tin-doped indium oxide fine particle dispersion and method for producing the same, interlayer film for laminated glass having heat ray shielding properties using the dispersion, and laminated glass thereof |
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