CN102746846A - Preparation method of zinc oxide-titanium oxide composite semiconductor film with adjustable luminescent intensity - Google Patents
Preparation method of zinc oxide-titanium oxide composite semiconductor film with adjustable luminescent intensity Download PDFInfo
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- CN102746846A CN102746846A CN2012102452606A CN201210245260A CN102746846A CN 102746846 A CN102746846 A CN 102746846A CN 2012102452606 A CN2012102452606 A CN 2012102452606A CN 201210245260 A CN201210245260 A CN 201210245260A CN 102746846 A CN102746846 A CN 102746846A
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Abstract
The invention relates to a preparation method of a zinc oxide-titanium oxide composite semiconductor film with adjustable luminescent intensity, which is characterized by comprising the following steps: preparing a ZnO sol and a TiO2 sol, and mixing the two sols to obtain a TiO2-ZnO composite sol, wherein the two sol are mixed in any ratio, and the volume ratio is determined according to the luminescent intensity of the prepared zinc oxide-titanium oxide composite semiconductor film; and preparing a gel film on a glass substrate by a vertical dip coating method. According to the method, different volume ratios of sols are selected to regulate the luminescent intensity of the TiO2-ZnO composite film. The preparation technique is simple and easy to operate, has the advantage of low cost, can easily implement industrialization, and can be widely used in the aspect of regulation of luminescent intensity of luminescent film devices.
Description
Technical field
The invention belongs to transparent semiconductor light-emitting film preparation method field, relate to a kind of preparation method that can regulate the zinc oxide and the titanium oxide composite semiconductor films of luminous intensity, specifically is through selecting different ratios mixing TiO
2Luminous intensity with the laminated film of ZnO colloidal sol regulation and control sol-gel method preparation.
Background technology
Zinc oxide is direct band-gap semicondictor; Titanium oxide is indirect band-gap semiconductor; There is very big difference in both optical properties of difference decision on this band gap; Both energy gaps are very approaching simultaneously, are more or less the same with the top of valence band energy at the bottom of the conduction band, and both couplings have far-reaching influence to its optical property.The research of the nano combined system that therefore constitutes for both can not only be more deep the understanding characteristic of material under specific environment separately; But also can utilize the coupling between their nanoparticle; Make the performance of the two strengthen to some extent and improve, the interaction between them simultaneously also might derive some new physical phenomenons and available new function.
Summary of the invention
The technical problem that solves
Weak point for fear of prior art; The present invention proposes a kind of preparation method that can regulate the zinc oxide and the titanium oxide composite semiconductor films of luminous intensity; Luminosity research with compound system is attached most importance to, and explores compound system than new variation that single-material brought.
Technical scheme
A kind of preparation method that can regulate the zinc oxide and the titanium oxide composite semiconductor films of luminous intensity is characterized in that step is following:
The preparation of ZnO colloidal sol: with ZnAc
22H
2O is a raw material, and EGME is a solvent, and thanomin is a stablizer; The mol ratio of zine ion and thanomin is 1 ︰ 1; Raw material is dissolved in 30 ~ 50ml solvent according to above proportioning, obtains the colloidal sol of transparent and stable at 60 ~ 80 ℃ of stirring in water bath 2 ~ 3h, the concentration of colloidal sol is 0.5mol/L;
TiO
2The preparation of colloidal sol: with positive four butyl esters of metatitanic acid is raw material; Absolute ethyl alcohol is a solvent; Methyl ethyl diketone is a sequestrant, is catalyzer with acetate, and raw material is dissolved in the solvent; Stir under the room temperature and obtained A solution in 1 ~ 1.5 hour, then acetate, deionized water, sequestrant methyl ethyl diketone are dissolved in the absolute ethyl alcohol and obtained B solution at room temperature ultrasonic 10 ~ 15 minutes; The B drips of solution is added in the A solution of stirring, drips end back restir and obtained yellow limpid colloidal sol, material mol ratio in the colloidal sol: Ti (OC in 1 ~ 1.5 hour
4H
9)
4︰ catalyzer (H
+) ︰ H
2O ︰ AcAc=1 ︰ 0.25 ︰ 6 ︰ 0.5; Synthetic back TiO
2The concentration of colloidal sol is 0.4mol/L;
The preparation of complex sol: two kinds of colloidal sols mix, and mixed sols are at room temperature stirred 1 ~ 1.5 hour preparation TiO
2~ ZnO complex sol at room temperature left standstill in the air 24 ~ 36 hours, in order to plated film;
Step 2: clean substrate: glass substrate was soaked earlier 1 ~ 1.5 hour with washing composition, Hydrogen chloride, deionized water, acetone, ethanol successively separately; Ultrasonic cleaning is 10 ~ 15 minutes then; Removing the grease and the dirt on surface, and washed glass substrate is put into ethanol with subsequent use;
Step 3: glass substrate was soaked earlier 1 ~ 1.5 hour with washing composition, Hydrogen chloride, deionized water, acetone, ethanol successively separately; Ultrasonic cleaning is 10 ~ 15 minutes then; Remove the grease and the dirt on surface, and washed glass substrate is put into ethanol with subsequent use;
Step 4 is coated with film: after the glass substrate oven dry with cleaning, immerse the TiO that makes
2In ~ ZnO the complex sol, adopt vertically to lift plating method and lift with the speed of 4cm/min and obtain gel-film, each layer film is through pre-burning under 100 ℃ of dryings, the 500 ℃ of temperature, be cooled to room temperature again after repeated vertical lift plated film until desired thickness; With the gel film that makes 550 ℃ of annealing 1 hour in air, be placed in condition of high vacuum degree nitrogen and the argon gas zinc oxide and the titanium oxide composite semiconductor films that obtain recombination luminescence intensity in 550 ℃ of anneal 1h then; Said condition of high vacuum degree is 5 * 10
~ 3Pa.
Two kinds of colloidal sol is with mixed arbitrarily in the described step 1, and zinc oxide and the luminous intensity of titanium oxide composite semiconductor films of the volume ratio during mixing after according to preparation determines.
100 ℃ of exsiccant times are 10 ~ 15min in the described step 4.
In the described step 4 under 500 ℃ of temperature the pre-burning time be 15 ~ 20min.
Beneficial effect
A kind of preparation method that can regulate the zinc oxide and the titanium oxide composite semiconductor films of luminous intensity that the present invention proposes confirms suitable calcined temperature and annealing process, through selecting the different proportioning regulation and control of sol volume TiO
2The luminous intensity of-ZnO laminated film.
The present invention adopts the luminous intensity of the zinc oxide titanium oxide composite semiconductor films of regulation and control sol-gel method preparation.The composite semiconductor films that can realize making is to effective regulation and control of luminous intensity; And preparation technology is simple to operation, and is with low cost, is easy to realize industriallization; Can be applied in the regulation and control aspect of the luminous intensity of light-emitting film device widely, and then practical requirement.
Description of drawings
Fig. 1 is the schema that the present invention adopts the colloidal sol preparation;
Fig. 2 ~ Fig. 4 is the different ratios mixing TiO that the present invention obtains
2The pl-figure of-ZnO film (Zn/ among the figure (Zn+Ti) is the zinc oxide volume and the ratio of TV, and illustration is the variation diagram of luminous intensity with different mixing proportion);
The TiO of different proportionings under Fig. 2 vacuum annealing condition
2-ZnO film pl-figure;
Fig. 3 N
2The TiO of different proportionings under the annealing conditions
2-ZnO film pl-figure;
The TiO of different proportionings under Fig. 4 Ar annealing conditions
2-ZnO film pl-figure.
Embodiment
Combine embodiment, accompanying drawing that the present invention is further described at present:
1. the preparation of ZnO colloidal sol: with ZnAc
22H
2O is a raw material, and EGME is a solvent, and thanomin is a stablizer, synthetic ZnO colloidal sol, and the concentration of colloidal sol is 0.5mol/L.The mol ratio of metals ion and thanomin is 1:1, and raw material is dissolved in a certain amount of solvent according to above proportioning, obtains the colloidal sol of transparent and stable at 60 ℃ of left and right sides stirring in water bath 2-3h; 2. the preparation of TiO2 colloidal sol: with positive four butyl esters of metatitanic acid is raw material; Absolute ethyl alcohol is a solvent; Methyl ethyl diketone is a sequestrant, is catalyzer with acetate, and raw material is dissolved in the solvent; Stir about obtained A solution in 1 hour under the room temperature, acetate, deionized water, sequestrant (methyl ethyl diketone (AcAc)) was dissolved in also obtaining B solution in the absolute ethyl alcohol at room temperature ultrasonic about 10 minutes then.At last the B drips of solution is added in the intensively stirred A solution, drips end back restir and obtained yellow limpid colloidal sol in about 1 hour, the material mol ratio is Ti (OC in the colloidal sol
4H
9)
4: catalyzer (H
+): H
2O:AcAc=1:0.25:6:0.5, synthetic TiO
2Colloidal sol, the concentration of colloidal sol are 0.4mol/L; 3. the preparation of complex sol: according to the direct mixed sols stir about 1 hour at room temperature in volume/TV=0,0.2,0.4,0.6 of zinc oxide, 0.8 and 1.0 ratio (TV is 50ml), preparation TiO
2-ZnO complex sol; At room temperature left standstill in the air about 24-36 hour; Lift plating method with dipping and slowly lift in the glass of clean dried the speed with 4cm/min of sinking to the bottom and obtain gel-film, each layer film is through the about 10min of pre-burning under 100 ℃ of dry about 10min, the 500 ℃ of temperature, be cooled to room temperature again after the repetition plated film until desired thickness; Then the gel film that makes was annealed 1 hour in 550 ℃ of air, be placed on condition of high vacuum degree (5 * 10 then
-2Pa) in 550 ℃ of anneal 1h.The luminous intensity of PE LS55 spectrophotofluorometer test result show sample about the 400nm place of U.S. PE company is adjustable from 31.248arb.unit to 231.481arb.unit.
Embodiment 2
1. the preparation of ZnO colloidal sol: with ZnAc
22H
2O is a raw material, and EGME is a solvent, and thanomin is a stablizer, synthetic ZnO colloidal sol, and the concentration of colloidal sol is 0.5mol/L.The mol ratio of metals ion and thanomin is 1:1, and raw material is dissolved in a certain amount of solvent according to above proportioning, obtains the colloidal sol of transparent and stable at 60 ℃ of left and right sides stirring in water bath 2-3h; 2. TiO
2The preparation of colloidal sol: with positive four butyl esters of metatitanic acid is raw material; Absolute ethyl alcohol is a solvent; Methyl ethyl diketone is a sequestrant, is catalyzer with acetate, and raw material is dissolved in the solvent; Stir about obtained A solution in 1 hour under the room temperature, acetate, deionized water, sequestrant (methyl ethyl diketone (AcAc)) was dissolved in also obtaining B solution in the absolute ethyl alcohol at room temperature ultrasonic about 10 minutes then.At last the B drips of solution is added in the intensively stirred A solution, drips end back restir and obtained yellow limpid colloidal sol in about 1 hour, the material mol ratio is Ti (OC in the colloidal sol
4H
9)
4: catalyzer (H
+): H
2O:AcAc=1:0.25:6:0.5, synthetic TiO
2Colloidal sol, the concentration of colloidal sol are 0.4mol/L; 3. the preparation of complex sol: according to the direct mixed sols stir about 1 hour at room temperature in volume/TV=0,0.2,0.4,0.6 of zinc oxide, 0.8 and 1.0 ratio (TV is 50ml), preparation TiO
2-ZnO complex sol; At room temperature left standstill in the air 24-36 hour; Lift plating method with dipping and slowly lift in the glass of clean dried the speed with 4cm/min of sinking to the bottom and obtain gel-film, each layer film is through pre-burning 10min under 100 ℃ of dry 10min, the 500 ℃ of temperature, repeats plated film until desired thickness after being cooled to room temperature again; Then the gel film that makes was annealed 1 hour in 550 ℃ of air, be placed on 550 ℃ of anneal 1h in the nitrogen atmosphere then.The luminous intensity of PE LS55 spectrophotofluorometer test result show sample about the 400nm place of U.S. PE company is adjustable from 12.539arb.unit to 254.628arb.unit.
Embodiment 3:
1. the preparation of ZnO colloidal sol: with ZnAc
22H
2O is a raw material, and EGME is a solvent, and thanomin is a stablizer, synthetic ZnO colloidal sol, and the concentration of colloidal sol is 0.5mol/L.The mol ratio of metals ion and thanomin is 1:1, and raw material is dissolved in a certain amount of solvent according to above proportioning, stirs the colloidal sol that 2-3h obtains transparent and stable down at 60 ℃; 2. TiO
2The preparation of colloidal sol: with positive four butyl esters of metatitanic acid is raw material; Absolute ethyl alcohol is a solvent; Methyl ethyl diketone is a sequestrant, is catalyzer with acetate, and raw material is dissolved in the solvent; Stir about obtained A solution in 1 hour under the room temperature, acetate, deionized water, sequestrant (methyl ethyl diketone (AcAc)) was dissolved in also obtaining B solution in the absolute ethyl alcohol at room temperature ultrasonic about 10 minutes then.At last the B drips of solution is added in the intensively stirred A solution, drips end back restir and obtained yellow limpid colloidal sol in about 1 hour, the material mol ratio is Ti (OC in the colloidal sol
4H
9)
4: catalyzer (H
+): H
2O:AcAc=1:0.25:6:0.5, synthetic TiO
2Colloidal sol, the concentration of colloidal sol are 0.4mol/L; 3. the preparation of complex sol: according to the direct mixed sols stir about 1 hour at room temperature in volume/TV=0,0.2,0.4,0.6 of zinc oxide, 0.8 and 1.0 ratio (TV is 50ml), preparation TiO
2-ZnO complex sol; At room temperature left standstill in the air 24-36 hour; Lift plating method with dipping and slowly lift in the glass of clean dried the speed with 4cm/min of sinking to the bottom and obtain gel-film, each layer film is through pre-burning 10min under 100 ℃ of dry 10min, the 500 ℃ of temperature, repeats plated film until desired thickness after being cooled to room temperature again; Then the gel film that makes was annealed 1 hour in 550 ℃ of air, be placed on 550 ℃ of anneal 1h in the argon gas atmosphere then.The luminous intensity of PE LS55 spectrophotofluorometer test result show sample about the 400nm place of U.S. PE company is adjustable from 31.302arb.unit to 594.595arb.unit.
Claims (4)
1. preparation method that can regulate the zinc oxide and the titanium oxide composite semiconductor films of luminous intensity is characterized in that step is following:
Step 1 preparation colloidal sol:
The preparation of ZnO colloidal sol: with ZnAc
22H
2O is a raw material, and EGME is a solvent, and thanomin is a stablizer; The mol ratio of zine ion and thanomin is 1 ︰ 1; Raw material is dissolved in 30 ~ 50ml solvent according to above proportioning, obtains the colloidal sol of transparent and stable at 60 ~ 80 ℃ of stirring in water bath 2 ~ 3h, the concentration of colloidal sol is 0.5mol/L;
TiO
2The preparation of colloidal sol: with positive four butyl esters of metatitanic acid is raw material; Absolute ethyl alcohol is a solvent; Methyl ethyl diketone is a sequestrant, is catalyzer with acetate, and raw material is dissolved in the solvent; Stir under the room temperature and obtained A solution in 1 ~ 1.5 hour, then acetate, deionized water, sequestrant methyl ethyl diketone are dissolved in the absolute ethyl alcohol and obtained B solution at room temperature ultrasonic 10 ~ 15 minutes; The B drips of solution is added in the A solution of stirring, drips end back restir and obtained yellow limpid colloidal sol, material mol ratio in the colloidal sol: Ti (OC in 1 ~ 1.5 hour
4H
9)
4︰ catalyzer (H
+) ︰ H
2O ︰ AcAc=1 ︰ 0.25 ︰ 6 ︰ 0.5; Synthetic back TiO
2The concentration of colloidal sol is 0.4mol/L;
The preparation of complex sol: two kinds of colloidal sols mix, and mixed sols are at room temperature stirred 1 ~ 1.5 hour preparation TiO
2~ ZnO complex sol at room temperature left standstill in the air 24 ~ 36 hours, in order to plated film;
Step 2: clean substrate: glass substrate was soaked earlier 1 ~ 1.5 hour with washing composition, Hydrogen chloride, deionized water, acetone, ethanol successively separately; Ultrasonic cleaning is 10 ~ 15 minutes then; Removing the grease and the dirt on surface, and washed glass substrate is put into ethanol with subsequent use;
Step 3: glass substrate was soaked earlier 1 ~ 1.5 hour with washing composition, Hydrogen chloride, deionized water, acetone, ethanol successively separately; Ultrasonic cleaning is 10 ~ 15 minutes then; Remove the grease and the dirt on surface, and washed glass substrate is put into ethanol with subsequent use;
Step 4 is coated with film: after the glass substrate oven dry with cleaning, immerse the TiO that makes
2In ~ ZnO the complex sol, adopt vertically to lift plating method and lift with the speed of 4cm/min and obtain gel-film, each layer film is through pre-burning under 100 ℃ of dryings, the 500 ℃ of temperature, be cooled to room temperature again after repeated vertical lift plated film until desired thickness; With the gel film that makes 550 ℃ of annealing 1 hour in air, be placed in condition of high vacuum degree nitrogen and the argon gas zinc oxide and the titanium oxide composite semiconductor films that obtain recombination luminescence intensity in 550 ℃ of anneal 1h then; Said condition of high vacuum degree is 5 * 10
～3Pa.
2. the preparation method that can regulate the zinc oxide and the titanium oxide composite semiconductor films of luminous intensity according to claim 1; It is characterized in that: two kinds of colloidal sol is with mixed arbitrarily in the described step 1, and zinc oxide and the luminous intensity of titanium oxide composite semiconductor films of the volume ratio during mixing after according to preparation determines.
3. the preparation method that can regulate the zinc oxide and the titanium oxide composite semiconductor films of luminous intensity according to claim 1 is characterized in that: 100 ℃ of exsiccant times are 10 ~ 15min in the described step 4.
4. the preparation method that can regulate the zinc oxide and the titanium oxide composite semiconductor films of luminous intensity according to claim 1 is characterized in that: in the described step 4 under 500 ℃ of temperature the pre-burning time be 15 ~ 20min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103409738A (en) * | 2013-07-23 | 2013-11-27 | 西北工业大学 | Method used for adjusting optical band gaps of zinc oxide and titanium oxide (ZnO-TiO2) composite semiconductor films |
| CN103409139A (en) * | 2013-07-23 | 2013-11-27 | 西北工业大学 | Method used for adjusting luminous intensity of tin oxide and titanium oxide (TiO2-SnO2) composite semiconductor films |
| CN105349953A (en) * | 2015-10-12 | 2016-02-24 | 哈尔滨工业大学 | Method for preparing p-type zinc oxide from Zn3N2:elements of group three through thermal oxidation |
| CN108786780A (en) * | 2018-06-03 | 2018-11-13 | 常州德维勒新材料科技有限公司 | A kind of nano combined Zn2TiO4The preparation method of functional material and its dispersion liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409738A (en) * | 2013-07-23 | 2013-11-27 | 西北工业大学 | Method used for adjusting optical band gaps of zinc oxide and titanium oxide (ZnO-TiO2) composite semiconductor films |
| CN103409139A (en) * | 2013-07-23 | 2013-11-27 | 西北工业大学 | Method used for adjusting luminous intensity of tin oxide and titanium oxide (TiO2-SnO2) composite semiconductor films |
| CN105349953A (en) * | 2015-10-12 | 2016-02-24 | 哈尔滨工业大学 | Method for preparing p-type zinc oxide from Zn3N2:elements of group three through thermal oxidation |
| CN105349953B (en) * | 2015-10-12 | 2018-07-03 | 哈尔滨工业大学 | Thermal oxide Zn3N2：The method that group-III element prepares p-type zinc oxide |
| CN108786780A (en) * | 2018-06-03 | 2018-11-13 | 常州德维勒新材料科技有限公司 | A kind of nano combined Zn2TiO4The preparation method of functional material and its dispersion liquid |
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Application publication date: 20121024 |