CN102827606A - Method for adjusting Eu<3+> luminous intensity in oxide semiconductor substrate - Google Patents

Method for adjusting Eu<3+> luminous intensity in oxide semiconductor substrate Download PDF

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CN102827606A
CN102827606A CN2012103105928A CN201210310592A CN102827606A CN 102827606 A CN102827606 A CN 102827606A CN 2012103105928 A CN2012103105928 A CN 2012103105928A CN 201210310592 A CN201210310592 A CN 201210310592A CN 102827606 A CN102827606 A CN 102827606A
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colloidal sol
oxide semiconductor
tio
sio
film
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赵小如
孙慧楠
史小龙
关蒙萌
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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Abstract

The invention relates to a method for adjusting Eu<3+> luminous intensity in an oxide semiconductor substrate. The method is characterized by comprising the following steps of: preparing TiO2 sol and SiO2 sol, preparing the TiO2 sol and the SiO2 sol into a mixed solution, adding rare earth Eu<3+> into the sol, drying a glass substrate, soaking into prepared Eu<3+>-doped compound oxide semiconductor sol, and lifting with a vertical lifting film coating method to obtain a gel film; and repeatedly performing the vertical lifting film coating method till a required thickness is achieved to obtain a Eu<3+>-doped compound oxide semiconductor film. The Eu<3+>-doped compound oxide semiconductor film is regulated and controlled by selecting different mixture ratios of sol volume. A method for mixing two types of sol is adopted, so that adjustment of the Eu<3+> luminous intensity is realized, and future realization of the preparation of an oxide semiconductor device for a rare earth ion high-strength luminous film becomes possible.

Description

Eu in a kind of adjusting oxide semiconductor matrix 3+The method of luminous intensity
Technical field
The present invention relates to Eu in a kind of adjusting oxide semiconductor matrix 3+The method of luminous intensity belongs to the rare earth ion doped oxide semiconductor transparent film method field of preparation, is specially through regulating TiO 2And SiO 2The colloidal sol proportioning is regulated Eu 3+The luminous intensity of adulterated oxide semiconductor thin-film.
Background technology
TiO 2, SiO 2And their laminated film has obtained in fields such as optical thin film and microtronics using widely because its high thermostability and chemicalstability, low thermal expansivity and adjustable specific refractory power.Especially to TiO 2-SiO 2Laminated film is because its specific refractory power can be regulated in the scope of a broad.Therefore, can be used for preparing optical waveguide film and gradient-index film etc. easily.In recent years, the optical property of rare earth ion doped collosol and gel oxide semiconductor material is because its potential application at aspects such as laserable material, transmitter, highdensity frequency domain optical storage and optical fiber communication amplifiers has obtained concern widely.Therefore, rare earth ion doped TiO 2-SiO 2The luminosity of laminated film can be because TiO 2And SiO 2Coupling improve and strengthen physical phenomenon and the available new function that possibly also can derive and make new advances.
Summary of the invention
The technical problem that solves
For fear of the weak point of prior art, the present invention proposes Eu in a kind of adjusting oxide semiconductor matrix 3+The method of luminous intensity is an experimental technique with a kind of preparation technology sol-gel method simple to operation, the adjustable rare earth ion doped oxide semiconductor thin-film of preparation luminous intensity.
Technical scheme
Eu in a kind of adjusting oxide semiconductor matrix 3+The method of luminous intensity is characterized in that step is following:
Step 1 preparation TiO 2Colloidal sol and SiO 2Colloidal sol:
Preparation TiO 2Colloidal sol: positive four butyl esters of metatitanic acid are dissolved in the absolute ethyl alcohol, at room temperature stir and obtained A solution in 0.5 ~ 1 hour, then acetate, deionized water and methyl ethyl diketone are dissolved in the absolute ethyl alcohol and obtained B solution at room temperature ultrasonic 10 ~ 15 minutes; In stirring, B solution is dripped in the A solution then, drip end back restir and obtained yellow limpid TiO in 0.5 ~ 1 hour 2Colloidal sol; Said TiO 2The material mol ratio is Ti (OC in the colloidal sol 4H 9) 4: acetate (H+): H 2O: methyl ethyl diketone=1:0.25:6:0.5; Said TiO 2The concentration of colloidal sol is 0.4mol/L;
Preparation SiO 2Colloidal sol: tetraethoxy, deionized water, absolute ethyl alcohol and Virahol are mixed, and 50 ℃ of stirring in water bath and dripping hydrochloric acid continue to stir the SiO that 2 ~ 3h obtains transparent and stable 2Colloidal sol; Said SiO 2The volume ratio of material is a tetraethoxy in the colloidal sol: deionized water: absolute ethyl alcohol: Virahol=16:4:15:15; The amount of said hydrochloric acid is 8/50ml;
Step 2 preparation Eu 3+Adulterated composite oxide semiconductor colloidal sol: according to TiO 2/ (TiO 2+ SiO 2Two kinds of TiO of the mixed of)=0.2 ~ 1.0 2And SiO 2Colloidal sol is stir about 1 hour at room temperature, again with rare earth Eu 3+, according to Eu 3+/ (TiO 2+ SiO 2) mol ratio 1.4% join in the above-mentioned colloidal sol, continue to stir and to obtain Eu in 0.5 ~ 1 hour 3+Adulterated composite oxide semiconductor colloidal sol at room temperature left standstill in the air 24 ~ 48 hours;
Step 3: after the glass substrate oven dry, immerse the Eu that makes 3+In the adulterated composite oxide semiconductor colloidal sol, adopt vertically to lift plating method and slowly lift with the speed of 4 ~ 6cm/min and obtain gel-film; Gel-film is dry under 100 ℃, and 300 ℃ ~ 550 ℃ following pre-burnings are cooled to room temperature again;
Step 4: repeating step 3 plated films are until desired thickness, with the gel film that makes 500 ℃ of annealing 4 ~ 5 hours in air, obtain Eu then 3+Adulterated composite oxide semiconductor film.
Said glass substrate was soaked earlier 1 ~ 2 hour with washing composition, Hydrogen chloride, deionized water, acetone, ethanol successively separately, and ultrasonic cleaning is 10 ~ 15 minutes then, and washed glass substrate is put into ethanol.
Beneficial effect
Eu in a kind of adjusting oxide semiconductor matrix that the present invention proposes 3+The method of luminous intensity is crucial suitable calcined temperature and the annealing process of confirming, through selecting the different proportioning regulation and control of sol volume Eu 3+Adulterated oxide semiconductor thin-film.Through adopting the method for mixing two kinds of colloidal sols, realized Eu 3+The adjusting of luminous intensity is for the preparation of the oxide semiconductor element of realization rare earth ion HS light-emitting film later on provides a kind of possibility.
Description of drawings
Fig. 1 is the schema that the present invention adopts the colloidal sol preparation;
Fig. 2 is the different ratios blended Eu under the different calcined temperatures that make of the present invention 3+Adulterated composite oxides are partly led the pl-figure of film;
Fig. 2 is Eu under ℃ pre-burning a.300 3+Adulterated composite oxide semiconductor film light photoluminescence figure;
Fig. 2 is Eu under ℃ pre-burning b.400 3+Adulterated composite oxide semiconductor film light photoluminescence figure;
Fig. 2 is Eu under ℃ pre-burning c.500 3+Adulterated composite oxide semiconductor film light photoluminescence figure;
Fig. 2 is Eu under ℃ pre-burning d.550 3+Adulterated composite oxide semiconductor film light photoluminescence figure.
Embodiment
Combine embodiment, accompanying drawing that the present invention is further described at present:
Embodiment 1
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 0.5 ~ 1 hour, then acetate, deionized water, sequestrant (methyl ethyl diketone (AcAc)) are dissolved in the absolute ethyl alcohol and obtained B solution at room temperature ultrasonic 10 ~ 15 minutes.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 0.5 ~ 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;
SiO 2The preparation of colloidal sol: tetraethoxy, deionized water, absolute ethyl alcohol, Virahol are mixed; 50 ℃ of left and right sides stirring in water bath also drip several hydrochloric acid; Continue to stir the colloidal sol that 2 ~ 3h obtains transparent and stable; The volume ratio of material is a tetraethoxy in the colloidal sol: deionized water: absolute ethyl alcohol: Virahol=16:4:15:15, and the amount of hydrochloric acid is 8/50ml;
Eu 3+The preparation of adulterated composite oxide semiconductor colloidal sol: according to TiO 2/ (TiO 2+ SiO 2)=0.2,0.5,0.8 and 1.0 ratio (TV is 50ml) be mixed sols stir about 1 hour at room temperature directly, again with a certain amount of rare earth Eu 3+, with Eu 3+With (TiO 2+ SiO 2) mol ratio be 1.4% to join in the above-mentioned colloidal sol, continue to stir 0.5 ~ 1 hour Eu 3+Adulterated composite oxide semiconductor colloidal sol at room temperature left standstill in the air 24 ~ 48 hours;
Lifting plating method with dipping slowly lifts with the speed of 4 ~ 6cm/min on the glass substrate of clean dried and obtains gel-film; Each layer film is through pre-burning 15 ~ 20min under 100 ℃ of drying 10 ~ 15min, the 300 ℃ of temperature; Repeat plated film until desired thickness after being cooled to room temperature again, then the gel film that makes was annealed 4 ~ 5 hours in 500 ℃ of air.The luminous intensity of PE LS55 spectrophotofluorometer test result show sample about the 615nm place of U.S. PE company is adjustable from 2.046arb.unit to 75.684arb.unit.
Embodiment 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 under the room temperature and obtained A solution in 0.5 ~ 1 hour, then acetate, deionized water, sequestrant (methyl ethyl diketone (AcAc)) are dissolved in the absolute ethyl alcohol and obtained B solution at room temperature ultrasonic 10 ~ 15 minutes.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 0.5 ~ 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;
SiO 2The preparation of colloidal sol: tetraethoxy, deionized water, absolute ethyl alcohol, Virahol are mixed; 50 ℃ of left and right sides stirring in water bath also drip several hydrochloric acid; Continue to stir the colloidal sol that 2 ~ 3h obtains transparent and stable; The volume ratio of material is a tetraethoxy in the colloidal sol: deionized water: absolute ethyl alcohol: Virahol=16:4:15:15, and the amount of hydrochloric acid is 8/50ml;
Eu 3+The preparation of adulterated composite oxide semiconductor colloidal sol: according to TiO 2/ (TiO 2+ SiO 2)=0.2,0.5,0.8 and 1.0 ratio (TV is 50ml) be mixed sols stir about 1 hour at room temperature directly, again with a certain amount of rare earth Eu 3+, with Eu 3+With (TiO 2+ SiO 2) mol ratio be 1.4% to join in the above-mentioned colloidal sol, continue to stir 0.5 ~ 1 hour Eu 3+Adulterated composite oxide semiconductor colloidal sol at room temperature left standstill in the air 24 ~ 48 hours;
Lifting plating method with dipping slowly lifts with the speed of 4cm/min on the glass substrate of clean dried and obtains gel-film; Each layer film is through pre-burning 15 ~ 20min under 100 ℃ of drying 10 ~ 15min, the 400 ℃ of temperature; Repeat plated film until desired thickness after being cooled to room temperature again, then the gel film that makes was annealed 4 ~ 5 hours in 500 ℃ of air.The luminous intensity of PE LS55 spectrophotofluorometer test result show sample about the 615nm place of U.S. PE company is adjustable from 1.58arb.unit to 72.924arb.unit.
Embodiment 3
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 0.5 ~ 1 hour, then acetate, deionized water, sequestrant (methyl ethyl diketone (AcAc)) are dissolved in the absolute ethyl alcohol and obtained B solution at room temperature ultrasonic 10 ~ 15 minutes.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 0.5 ~ 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;
SiO 2The preparation of colloidal sol: tetraethoxy, deionized water, absolute ethyl alcohol, Virahol are mixed; 50 ℃ of left and right sides stirring in water bath also drip several hydrochloric acid; Continue to stir the colloidal sol that 2 ~ 3h obtains transparent and stable; The volume ratio of material is a tetraethoxy in the colloidal sol: deionized water: absolute ethyl alcohol: Virahol=16:4:15:15, and the amount of hydrochloric acid is 8/50ml;
Eu 3+The preparation of adulterated composite oxide semiconductor colloidal sol: according to TiO 2/ (TiO 2+ SiO 2)=0.2,0.5,0.8 and 1.0 ratio (TV is 50ml) be mixed sols stir about 1 hour at room temperature directly, again with a certain amount of rare earth Eu 3+, with Eu 3+With (TiO 2+ SiO 2) mol ratio be 1.4% to join in the above-mentioned colloidal sol, continue to stir 0.5 ~ 1 hour Eu 3+Adulterated composite oxide semiconductor colloidal sol at room temperature left standstill in the air 24 ~ 48 hours;
Lifting plating method with dipping slowly lifts with the speed of 4 ~ 6cm/min on the glass substrate of clean dried and obtains gel-film; Each layer film is through pre-burning 15 ~ 20min under 100 ℃ of drying 10 ~ 15min, the 500 ℃ of temperature; Repeat plated film until desired thickness after being cooled to room temperature again, then the gel film that makes was annealed 4 ~ 5 hours in 500 ℃ of air.The luminous intensity of PE LS55 spectrophotofluorometer test result show sample about the 615nm place of U.S. PE company is adjustable from 7.76arb.unit to 120.556arb.unit.
Embodiment 4
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 0.5 ~ 1 hour, then acetate, deionized water, sequestrant (methyl ethyl diketone (AcAc)) are dissolved in the absolute ethyl alcohol and obtained B solution at room temperature ultrasonic 10 ~ 15 minutes.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 0.5 ~ 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;
SiO 2The preparation of colloidal sol: tetraethoxy, deionized water, absolute ethyl alcohol, Virahol are mixed; 50 ℃ of left and right sides stirring in water bath also drip several hydrochloric acid; Continue to stir the colloidal sol that 2 ~ 3h obtains transparent and stable; The volume ratio of material is a tetraethoxy in the colloidal sol: deionized water: absolute ethyl alcohol: Virahol=16:4:15:15, and the amount of hydrochloric acid is 8/50ml;
Eu 3+The preparation of adulterated composite oxide semiconductor colloidal sol: according to TiO 2/ (TiO 2+ SiO 2)=0.2,0.5,0.8 and 1.0 ratio (TV is 50ml) be mixed sols stir about 1 hour at room temperature directly, again with a certain amount of rare earth Eu 3+, with Eu 3+With (TiO 2+ SiO 2) mol ratio be 1.4% to join in the above-mentioned colloidal sol, continue to stir 0.5 ~ 1 hour Eu 3+Adulterated composite oxide semiconductor colloidal sol at room temperature left standstill in the air 24 ~ 48 hours;
Lifting plating method with dipping slowly lifts with the speed of 4 ~ 6cm/min on the glass substrate of clean dried and obtains gel-film; Each layer film is through pre-burning 15 ~ 20min under 100 ℃ of drying 10 ~ 15min, the 550 ℃ of temperature; Repeat plated film until desired thickness after being cooled to room temperature again, then the gel film that makes was annealed 4 ~ 5 hours in 500 ℃ of air.The luminous intensity of PE LS55 spectrophotofluorometer test result show sample about the 615nm place of U.S. PE company is adjustable from 3.589arb.unit to 159.812arb.unit.

Claims (2)

1. regulate Eu in the oxide semiconductor matrix for one kind 3+The method of luminous intensity is characterized in that step is following:
Step 1 preparation TiO 2Colloidal sol and SiO 2Colloidal sol:
Preparation TiO 2Colloidal sol: positive four butyl esters of metatitanic acid are dissolved in the absolute ethyl alcohol, at room temperature stir and obtained A solution in 0.5 ~ 1 hour, then acetate, deionized water and methyl ethyl diketone are dissolved in the absolute ethyl alcohol and obtained B solution at room temperature ultrasonic 10 ~ 15 minutes; In stirring, B solution is dripped in the A solution then, drip end back restir and obtained yellow limpid TiO in 0.5 ~ 1 hour 2Colloidal sol; Said TiO 2The material mol ratio is Ti (OC in the colloidal sol 4H 9) 4: acetate (H+): H 2O: methyl ethyl diketone=1:0.25:6:0.5; Said TiO 2The concentration of colloidal sol is 0.4mol/L;
Preparation SiO 2Colloidal sol: tetraethoxy, deionized water, absolute ethyl alcohol and Virahol are mixed, and 50 ℃ of stirring in water bath and dripping hydrochloric acid continue to stir the SiO that 2 ~ 3h obtains transparent and stable 2Colloidal sol; Said SiO 2The volume ratio of material is a tetraethoxy in the colloidal sol: deionized water: absolute ethyl alcohol: Virahol=16:4:15:15; The amount of said hydrochloric acid is 8/50ml;
Step 2 preparation Eu 3+Adulterated composite oxide semiconductor colloidal sol: according to TiO 2/ (TiO 2+ SiO 2Two kinds of TiO of the mixed of)=0.2 ~ 1.0 2And SiO 2Colloidal sol is stir about 1 hour at room temperature, again with rare earth Eu 3+, according to Eu 3+/ (TiO 2+ SiO 2) mol ratio 1.4% join in the above-mentioned colloidal sol, continue to stir and to obtain Eu in 0.5 ~ 1 hour 3+Adulterated composite oxide semiconductor colloidal sol at room temperature left standstill in the air 24 ~ 48 hours;
Step 3: after the glass substrate oven dry, immerse the Eu that makes 3+In the adulterated composite oxide semiconductor colloidal sol, adopt vertically to lift plating method and slowly lift with the speed of 4 ~ 6cm/min and obtain gel-film; Gel-film is dry under 100 ℃, and 300 ℃ ~ 550 ℃ following pre-burnings are cooled to room temperature again;
Step 4: repeating step 3 plated films are until desired thickness, with the gel film that makes 500 ℃ of annealing 4 ~ 5 hours in air, obtain Eu then 3+Adulterated composite oxide semiconductor film.
2. according to Eu in the said adjusting oxide semiconductor of claim 1 matrix 3+The method of luminous intensity is characterized in that:
Said glass substrate was soaked earlier 1 ~ 2 hour with washing composition, Hydrogen chloride, deionized water, acetone, ethanol successively separately, and ultrasonic cleaning is 10 ~ 15 minutes then, and washed glass substrate is put into ethanol.
CN2012103105928A 2012-08-28 2012-08-28 Method for adjusting Eu<3+> luminous intensity in oxide semiconductor substrate Pending CN102827606A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102154009A (en) * 2011-03-08 2011-08-17 西北大学 SiO2: RE light-emitting film taking TiO2 nanotube array as carrier and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102154009A (en) * 2011-03-08 2011-08-17 西北大学 SiO2: RE light-emitting film taking TiO2 nanotube array as carrier and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王丹红等: "ZnO缓冲层退火温度对TiO2:Eu/ZnO薄膜光致发光性能的影响", 《材料导报B：研究篇》, vol. 25, no. 11, 30 November 2011 (2011-11-30) *
赵建果等: "退火温度对Eu3+掺杂TiO2-SiO2复合薄膜的发光影响", 《功能材料与器件学报》, vol. 17, no. 4, 31 August 2011 (2011-08-31) *

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Application publication date: 20121219