CN101704635B - Method for preparing aluminum-doped zinc oxide film on optical solar reflector - Google Patents
Method for preparing aluminum-doped zinc oxide film on optical solar reflector Download PDFInfo
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- CN101704635B CN101704635B CN2009103111081A CN200910311108A CN101704635B CN 101704635 B CN101704635 B CN 101704635B CN 2009103111081 A CN2009103111081 A CN 2009103111081A CN 200910311108 A CN200910311108 A CN 200910311108A CN 101704635 B CN101704635 B CN 101704635B
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Abstract
The invention relates to a method for preparing aluminum-doped zinc oxide film on an optical solar reflector and relates to a method for preparing a film. The method solves the problems of high cost, complex phase composition and complex operation of a preparation method of the traditional indium tin oxide film on a surface of a conductive optical solar reflector. The method comprises the following steps: 1, soaking and cleaning the optical solar reflector in lotion; 2, adding zinc acetate, a stabilizer and a doping agent into a solvent to prepare collosol; 3, soaking the optical solar reflector in the collosol to form a film by dip-coating; and 4, sintering the film obtained in the step 3 to obtain an aluminum-doped zinc oxide film prepared on the optical solar reflector. The optical transmittance of the film prepared by the method is more than or equal to 90 percent, the surface resistance of the film is between 8*103 omega/cm2 to 2*104 omega/cm2, and the film can be applied to the temperature control of large and medium-sized satellites. The film prepared by the method is low in cost and simple in preparation method.
Description
Technical field
The present invention relates to a kind of film and preparation method thereof.
Background technology
Optical solar reflector is the passive thermal control coating element of a kind of fine; Be widely used in large and medium-sized temperature control of satellites; It is by transparent to solar spectrum and form by the first surface of high emissivity with to the second surface that solar spectrum has a high-reflectivity; First surface is an emittance greater than 0.8 silica glass, and second surface is a silver layer, and resist behind is the high-temperature nickel-base alloy film; Existing conductivity type optical solar reflector is that the upper surface at silica glass has plated one deck optical transmittance and is higher than 90% indium tin oxide films; Its objective is that in order to prevent satellite when the spaceflight optical solar reflector and space plasma coupling and cause discharge and recharge effect are when being applied to indium tin oxide films the discharge of optical solar reflector surface anti-static; For the solar spectrum specific absorption of avoiding optical solar reflector increases the face resistance R of indium tin oxide films
Optimum range be 5 * 10
3Ω/～1.06 * 10
5Ω/.But the raw material indium of preparation indium tin oxide films is very rare; Cause the cost of film high, the preparation method generally adopts vaccum gas phase sedimentation method, magnetron sputtering method and spray pyrolysis, but these methods exist apparatus expensive, complicated operation; Film surface has the impurity deposition, and phase composite is complicated.
Summary of the invention
The present invention is a problem complicated for the indium tin oxide films cost height, the phase composite that solve existing conductivity type optical solar reflector surface, preparing method's complicated operation, and a kind of method that on optical solar reflector, prepares Al-Doped ZnO film is provided.
A kind of method that on optical solar reflector, prepares Al-Doped ZnO film of the present invention; Carry out according to the following steps: one, earlier optical solar reflector is soaked 3h～5h with washing lotion; And then put into deionized water, absolute ethyl alcohol and acetone successively, ultrasonic cleaning twice, each 5min～15min; Put into 100 ℃ the dry 10min～20min of baking oven at last, obtain clean optical solar reflector; Two, analytically pure zinc acetate, stablizer, doping agent are joined be mixed with the solution that the acetate zinc concentration is 0.5mol/L-2mol/L in the solvent; Wherein the mol ratio of zinc acetate and stablizer is 1: 0.5～2.5; The mol ratio of zinc acetate and doping agent is 100: 0.1～5; Then solution is stirred 4h～12h under 50 ℃～65 ℃ water bath condition, ageing 24h～72h forms vitreosol again; Three, will be immersed in through the optical solar reflector of the cleaning that step 1 obtains in the colloidal sol of step 2 preparation; After soaking 1min～15min; Speed with 1cm/min～10cm/min lifts out, under 50 ℃～150 ℃ conditions, keeps 10min～20min then; Four, will put into sintering oven through the optical solar reflector that step 3 is handled; In air atmosphere, sintering oven is warmed up to 200 ℃～400 ℃ and keep 0.5h～2h with the speed of 1 ℃/min～10 ℃/min; And then continue to be warming up to 500 ℃～650 ℃ and keep 0.5h～3h with the speed of 1 ℃/min～5 ℃/min; Naturally cool to room temperature at last, promptly obtain the Al-Doped ZnO film that on optical solar reflector, prepares.
Washing lotion described in the step 1 is that mass concentration is the mixing solutions of 98% the vitriol oil, water and SRM 935a, and wherein the volume ratio of the vitriol oil and water is 8～10: 1, and water and SRM 935a mass ratio are 1～3: 1.
Solvent described in the step 2 is analytically pure methyl alcohol, analytically pure absolute ethyl alcohol, analytically pure propyl alcohol, analytically pure Virahol, analytically pure propyl carbinol, the analytically pure trimethyl carbinol or analytically pure EGME, analytically pure Ucar 35 and analytically pure terepthaloyl moietie.
Stablizer described in the step 2 is analytically pure monoethanolamine, diethylolamine, quadrol, formyl ammonia or ammoniacal liquor.
Doping agent described in the step 2 is analytically pure aluminum chloride, aluminum nitrate, phosphagel phosphaljel, Tiorco 677.
Optical transmittance>=90% of the film that a kind of method that on optical solar reflector, prepares Al-Doped ZnO film of the present invention prepares, the face resistance of film is 8 * 10
3Ω/～2 * 10
4Zinc that Ω/ is easy to get with raw material and aluminium element substitute indium and tin element and prepare and can satisfy that optical sun mirror surface anti-static discharges and the film of the requirement of transparency; This method is handled optical sun mirror with the strong washing lotion of oxidisability; Remove optical sun mirror surperficial greasy dirt and impurity and make substrate cleaning, the film of assurance preparation can directedly evenly be grown, again the concentration of process control colloidal sol; The pull rate of film and agglomerating temperature are regulated the size and the crystalline state of crystal grain on the optical sun mirror; Make the phase composite of film simple, prepare Al-Doped ZnO film, its optical transmittance and electrical property are improved with (002) face preferred orientation.Present method has replaced rare phosphide element and tin element with cost low zinc element and aluminium element; The cost of film is reduced, and present method adopts sol-gel method on optical solar reflector, to prepare Al-Doped ZnO film, and method is simple; Do not need expensive equipment, cost is low.
Description of drawings
Fig. 1 is the X-ray diffractogram of the film of embodiment 20 preparations; Fig. 2 is the AFM figure of the film of embodiment 20 preparations; Fig. 3 is the transmittance curve of the film of embodiment 20 preparations.
Embodiment
Embodiment one: a kind of method that on optical solar reflector, prepares Al-Doped ZnO film of this embodiment is carried out according to the following steps: one, earlier optical solar reflector is soaked 3h～5h with washing lotion; And then put into deionized water, absolute ethyl alcohol and acetone successively; Twice of ultrasonic cleaning; Each 5min～15min puts into 100 ℃ the dry 10min～20min of baking oven at last, obtains clean optical solar reflector; Two, analytically pure zinc acetate, stablizer, doping agent are joined be mixed with the solution that the acetate zinc concentration is 0.5mol/L-2mol/L in the solvent; Wherein the mol ratio of zinc acetate and stablizer is 1: 0.5～2.5; The mol ratio of zinc acetate and doping agent is 100: 0.1～5; Then solution is stirred 4h～12h under 50 ℃～65 ℃ water bath condition, ageing 24h～72h forms vitreosol again; Three, will be immersed in through the optical solar reflector of the cleaning that step 1 obtains in the colloidal sol of step 2 preparation; After soaking 1min～15min; Speed with 1cm/min～10cm/min lifts out, under 50 ℃～150 ℃ conditions, keeps 10min～20min then; Four, will put into sintering oven through the optical solar reflector that step 3 is handled; In air atmosphere, sintering oven is warmed up to 200 ℃～400 ℃ and keep 0.5h～2h with the speed of 1 ℃/min～10 ℃/min; And then continue to be warming up to 500 ℃～650 ℃ and keep 0.5h～3h with the speed of 1 ℃/min～5 ℃/min; Naturally cool to room temperature at last, promptly obtain the Al-Doped ZnO film that on optical solar reflector, prepares.
Optical transmittance>=90% of the Al-Doped ZnO film that on optical solar reflector, prepares of this embodiment, the face resistance of film is 8 * 10
3Ω/～2 * 10
4Ω/; Prepare the film of the requirement that can satisfy discharge of optical sun mirror surface anti-static and transparency with alternative indium of be easy to get inexpensive zinc and aluminium element and tin element, this method is handled optical solar reflector with the strong washing lotion of oxidisability, goes the greasy dirt and the impurity on surface to make substrate cleaning; The film that guarantees preparation can directedly evenly be grown; Through the concentration of control colloidal sol, the pull rate of film and agglomerating temperature are regulated the size and the crystalline state of crystal grain on the optical sun mirror, make the phase composite of film simple again; Prepare Al-Doped ZnO film, its optical transmittance and electrical property are improved with (002) face preferred orientation.Present method adopts sol-gel process to prepare film, and method is simple, does not need expensive equipment, and cost is low.
Embodiment two: what this embodiment and embodiment one were different is: the washing lotion described in the step 1 is that mass concentration is the mixing solutions of 98% the vitriol oil, water and SRM 935a; Wherein the volume ratio of the vitriol oil and water is 8～10: 1, and water and SRM 935a mass ratio are 1～3: 1.Other is identical with embodiment one.
Embodiment three: what this embodiment was different with embodiment one or two is: the volume ratio of the vitriol oil and water is 9: 1 in the washing lotion, and water and SRM 935a mass ratio are 2: 1.Other is identical with embodiment one or two.
Embodiment four: what this embodiment and embodiment one to three were different is: the solvent described in the step 2 is a kind of or wherein several kinds the combination in analytically pure methyl alcohol, analytically pure absolute ethyl alcohol, analytically pure propyl alcohol, analytically pure Virahol, analytically pure propyl carbinol, the analytically pure trimethyl carbinol or analytically pure EGME, analytically pure Ucar 35 and the analytically pure terepthaloyl moietie.Other is identical with embodiment one to three.
When the solvent in this embodiment was compsn, each solvent was pressed arbitrary proportion and is mixed.
Embodiment five: what this embodiment and embodiment one to four were different is: the stablizer described in the step 2 is that analytically pure monoethanolamine, analytically pure diethylolamine, analytical pure quadrol, analytically pure formyl ammonia or mass concentration are a kind of or wherein several kinds the combination in >=25% ammoniacal liquor.Other is identical with embodiment one to four.
When the stablizer in this embodiment was compsn, each stablizer was pressed arbitrary proportion and is mixed.
Embodiment six: what this embodiment and embodiment one to five were different is: the doping agent described in the step 2 is analytically pure aluminum chloride, analytically pure aluminum nitrate, analytically pure phosphagel phosphaljel, analytically pure Tiorco 677.Other is identical with embodiment one to five.
Embodiment seven: what this embodiment and embodiment one to six were different is: earlier optical solar reflector is soaked 3.5h～4.5h with washing lotion in the step 1; And then put into deionized water, absolute ethyl alcohol and acetone successively; Twice of ultrasonic cleaning; Each 8min～12min puts into 100 ℃ the dry 12min～18min of baking oven at last, obtains clean optical solar reflector.Other and embodiment one to six phase are together.
Embodiment eight: what this embodiment and embodiment one to seven were different is: earlier optical solar reflector is soaked 4h with washing lotion in the step 1; And then put into deionized water, absolute ethyl alcohol and acetone successively; Twice of ultrasonic cleaning; Each 10min puts into 100 ℃ the dry 15min of baking oven at last, obtains clean optical solar reflector.Other is identical with embodiment one to seven.
Embodiment nine: what this embodiment and embodiment one to eight were different is: the acetate zinc concentration is the solution of 0.8mol/L～1.8mol/L in the step 2; Wherein the mol ratio of zinc acetate and stablizer is 1: 0.8～2.0, and the mol ratio of zinc acetate and doping agent is 100: 0.5～4.5; Other is identical with embodiment one to eight.
Embodiment ten: what this embodiment and embodiment one to nine were different is: the acetate zinc concentration is the solution of 0.9mol/L～1.3mol/L in the step 2; Wherein the mol ratio of zinc acetate and stablizer is 1: 0.9～1.2, and the mol ratio of zinc acetate and doping agent is 100: 0.6～2; Other is identical with embodiment one to nine.
Embodiment 11: what this embodiment and embodiment one to ten were different is: the acetate zinc concentration is the solution of 1.0mol/L in the step 2; Wherein the mol ratio of zinc acetate and stablizer is 1: 1.0, and the mol ratio of zinc acetate and doping agent is 100: 1; Other is identical with embodiment one to nine.
Embodiment 12: what this embodiment and embodiment one to 11 were different is: the acetate zinc concentration is the solution of 1.4mol/L～1.7mol/L in the step 2; Wherein the mol ratio of zinc acetate and stablizer is 1: 1.3～1.9, and the mol ratio of zinc acetate and doping agent is 100: 2～4.2; Other is identical with embodiment one to ten.
Embodiment 13: what this embodiment and embodiment one to 12 were different is: the acetate zinc concentration is the solution of 1.6mol/L in the step 2; Wherein the mol ratio of zinc acetate and stablizer is 1: 1.6, and the mol ratio of zinc acetate and doping agent is 100: 3; Other is identical with embodiment one to ten.
Embodiment 14: what this embodiment and embodiment one to 13 were different is: solution stirs 5h～11h, ageing 36h～60h in the step 2 under 55 ℃～63 ℃ water bath condition.Other is identical with embodiment one to 13.
Embodiment 15: what this embodiment and embodiment one to 14 were different is: solution stirs 10h, ageing 48h in the step 2 under 60 ℃ water bath condition.Other is identical with embodiment one to 14.
Embodiment 16: what this embodiment and embodiment one to 15 were different is: the soak time of optical solar reflector in colloidal sol is 2min～10min, lifts, under 70 ℃～130 ℃ conditions, keeps 12min～18min then with the speed of 2cm/min～9cm/min in the step 3.Other is identical with embodiment one to 15.
Embodiment 17: what this embodiment and embodiment one to 16 were different is: the soak time of optical solar reflector in colloidal sol is 4min, lifts, under 100 ℃ of conditions, keeps 15min then with the speed of 6cm/min in the step 3.Other and embodiment one to ten six phase are together.
Embodiment 18: what this embodiment and embodiment one to 17 were different is: sintering oven is warmed up to 250 ℃～350 ℃ and keep 0.8h～1.8h with the speed of 2 ℃/min～8 ℃/min earlier in the step 4; And then continue to be warming up to 520 ℃～630 ℃ and keep 0.8h～2.8h with the speed of 2 ℃/min～4 ℃/min, naturally cool to room temperature at last.Other is identical with embodiment one to 17.
Embodiment 19: what this embodiment and embodiment one to 18 were different is: sintering oven is warmed up to 300 ℃ and keep 1.5h with the speed of 5 ℃/min earlier in the step 4; And then continue to be warming up to 600 ℃ and keep 2.5h with the speed of 3 ℃/min, naturally cool to room temperature at last.Other is identical with embodiment one to 18.
Embodiment 20: a kind of method that on optical solar reflector, prepares Al-Doped ZnO film of (referring to accompanying drawing 1, Fig. 2 and Fig. 3) this embodiment is carried out according to the following steps: one, earlier optical solar reflector is soaked 3.5h with washing lotion; And then put into deionized water for ultrasonic and clean twice, each 5min; Put into analytically pure absolute ethyl alcohol ultrasonic cleaning twice again, each 5min; Put into analytically pure acetone again, ultrasonic cleaning twice, each 5min puts into 100 ℃ the dry 15min of baking oven at last, obtains clean optical solar reflector; Two, with analytically pure zinc acetate, analytically pure monoethanolamine; Analytically pure aluminum chloride joins and is mixed with the solution that the acetate zinc concentration is 1.5mol/L in the ethanol; Wherein the mol ratio of zinc acetate and monoethanolamine is 1: 1, and the mol ratio of zinc acetate and aluminum chloride is 100: 1.5, then solution is stirred 9h under 60 ℃ water bath condition; Ageing 48h forms vitreosol again; Three, will be immersed in through the optical solar reflector of the cleaning that step 1 obtains in the colloidal sol of step 2 preparation, soak 1.5min after, lift out with the speed of 6cm/min, be to keep 15min under 100 ℃ of conditions in temperature then; Four, will put into sintering oven through the optical solar reflector that step 3 is handled; In air atmosphere, sintering oven is warmed up to 400 ℃ and keep 1h with the speed of 3 ℃/min; And then continue to be warming up to 550 ℃ and keep 2h with the speed of 1 ℃/min; Naturally cool to room temperature at last, promptly obtain the Al-Doped ZnO film that on optical solar reflector, prepares.
The X-ray diffraction spectrogram of the film of the method preparation of this embodiment is as shown in Figure 1; As can beappreciated from fig. 1; The film that on optical solar reflector, makes has only 1 strong diffraction peak, and corresponding diffraction angle is at 34.42 °, and this shows that the film of preparing is to have (the zinc oxide of the wurtzite structure of 002 preferred orientation; Do not have other any impurity, phase composite is simple; The surface atom of the film of this embodiment preparation is tried hard to as shown in Figure 2, the as can be seen from Figure 2 crystal grain perfect crystalline of film surface, and crystal boundary is clear; The crystal grain marshalling is intensive; This constructional feature of film descends the resistance of film, homogeneous grain size, and diameter is about 30nm; The optical transmittance rate curve of the film of this embodiment preparation is as shown in Figure 3, as can be seen from Figure 3, is higher than 90% at the optical transmittance of visible region film.The face resistance of film is 8.9 * 10
3Ω/.
This embodiment has replaced rare phosphide element and tin element to prepare with low zinc element of cost and aluminium element can satisfy Al-Doped ZnO film that optical solar reflector requires and that have (002) face preferred orientation; The cost of film is reduced; Present method adopts the sol-gel thin films; Method is simple, does not need expensive equipment, and cost is low.
Claims (10)
1. method that on optical solar reflector, prepares Al-Doped ZnO film; It is characterized in that a kind of method that on optical solar reflector, prepares Al-Doped ZnO film carries out according to the following steps: one, earlier optical solar reflector is soaked 3h～5h with washing lotion; And then put into deionized water, absolute ethyl alcohol and acetone ultrasonic cleaning successively twice; Each 5min～15min puts into 100 ℃ the dry 10min～20min of baking oven at last, obtains clean optical solar reflector; Two, analytically pure zinc acetate, stablizer, doping agent are joined be mixed with the solution that the acetate zinc concentration is 0.5mol/L-2mol/L in the solvent; Wherein the mol ratio of zinc acetate and stablizer is 1: 0.5～2.5; The mol ratio of zinc acetate and doping agent is 100: 0.1～5; Then solution is stirred 4h～12h under 50 ℃～65 ℃ water bath condition, ageing 24h～72h forms vitreosol again; Three, will be immersed in through the optical solar reflector of the cleaning that step 1 obtains in the colloidal sol of step 2 preparation; After soaking 1min～15min; Speed with 1cm/min～10cm/min lifts out, under 50 ℃～150 ℃ conditions, keeps 10min～20min then; Four, will put into sintering oven through the optical solar reflector that step 3 is handled; In air atmosphere, sintering oven is warmed up to 200 ℃～400 ℃ and keep 0.5h～2h with the speed of 1 ℃/min～10 ℃/min; And then continue to be warming up to 500 ℃～650 ℃ and keep 0.5h～3h with the speed of 1 ℃/min～5 ℃/min; Naturally cool to room temperature at last, promptly obtain the Al-Doped ZnO film that on optical solar reflector, prepares.
2. a kind of method that on optical solar reflector, prepares Al-Doped ZnO film according to claim 1; It is characterized in that the washing lotion described in the step 1 is that mass concentration is the mixing solutions of 98% the vitriol oil, water and SRM 935a; Wherein the volume ratio of the vitriol oil and water is 8～10: 1, and water and SRM 935a mass ratio are 1～3: 1.
3. a kind of method that on optical solar reflector, prepares Al-Doped ZnO film according to claim 1 and 2 is characterized in that the solvent described in the step 2 is analytically pure methyl alcohol, analytically pure absolute ethyl alcohol, analytically pure propyl alcohol, analytically pure Virahol, analytically pure propyl carbinol, the analytically pure trimethyl carbinol or analytically pure EGME, analytically pure Ucar 35 or analytically pure terepthaloyl moietie.
4. a kind of method that on optical solar reflector, prepares Al-Doped ZnO film according to claim 3 is characterized in that the stablizer described in the step 2 is analytically pure monoethanolamine, diethylolamine, quadrol, formyl ammonia or ammoniacal liquor.
5. according to claim 1,2 or 4 described a kind of methods that on optical solar reflector, prepare Al-Doped ZnO film, it is characterized in that the doping agent described in the step 2 is analytically pure aluminum chloride, aluminum nitrate, phosphagel phosphaljel or Tiorco 677.
6. a kind of method that on optical solar reflector, prepares Al-Doped ZnO film according to claim 5; It is characterized in that earlier optical solar reflector being soaked 3.5h～4.5h with washing lotion in the step 1; And then put into deionized water, absolute ethyl alcohol and acetone successively, ultrasonic cleaning twice, each 8min～12min; Put into 100 ℃ the dry 12min～18min of baking oven at last, obtain clean optical solar reflector.
7. according to claim 1,2,4 or 6 described a kind of methods that on optical solar reflector, prepare Al-Doped ZnO film; It is characterized in that the acetate zinc concentration is the solution of 0.8mol/L～1.8mol/L in the step 2; Wherein the mol ratio of zinc acetate and stablizer is 1: 0.8～2.0, and the mol ratio of zinc acetate and doping agent is 100: 0.5～4.5.
8. a kind of method that on optical solar reflector, prepares Al-Doped ZnO film according to claim 7 is characterized in that solution stirs 5h～11h, ageing 36h～60h in the step 2 under 55 ℃～63 ℃ water bath condition.
9. according to claim 1,2,4,6 or 8 described a kind of methods that on optical solar reflector, prepare Al-Doped ZnO film, it is characterized in that the soak time of optical solar reflector in colloidal sol in the step 3 is 2min～10min, lifts, under 70 ℃～130 ℃ conditions, keeps 12min～18min then with the speed of 2cm/min～9cm/min.
10. a kind of method that on optical solar reflector, prepares Al-Doped ZnO film according to claim 9; It is characterized in that sintering oven in the step 4 is warmed up to 250 ℃～350 ℃ and keep 0.8h～1.8h with the speed of 2 ℃/min～8 ℃/min earlier; And then continue to be warming up to 520 ℃～630 ℃ and keep 0.8h～2.8h with the speed of 2 ℃/min～4 ℃/min, naturally cool to room temperature at last.
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