CN101538705A - Preparation method of rare earth doped SiO*substrate luminescent film - Google Patents
Preparation method of rare earth doped SiO*substrate luminescent film Download PDFInfo
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- CN101538705A CN101538705A CN200910022294A CN200910022294A CN101538705A CN 101538705 A CN101538705 A CN 101538705A CN 200910022294 A CN200910022294 A CN 200910022294A CN 200910022294 A CN200910022294 A CN 200910022294A CN 101538705 A CN101538705 A CN 101538705A
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Abstract
The invention discloses a preparation method of a rare earth doped SiO*substrate luminescent film, which comprises the following steps: firstly, dissolving ethyl orthosilicate Si(C2H5O)4 into ethanol or propanol; secondly, mixing the solution with ethanol or propanol water solution of boric acid; thirdly, adding hydrochloric acid or glacial acetic acid to adjust the pH value to 2-3; fourthly, adding aluminum soluble salt into the solution; fifthly, adding soluble rare-earth salts; sixthly, ageing to obtain gum, preparing the film, and calcining the film under 500-1500 DEG C to obtain the luminescent film. The luminescent film prepared by the invention has uniform and compact surface without cracking, and controllable thickness; and the size of the film particles is 1-50nm. The preparation method has simple process without vacuum equipment, low cost, and easy material obtaining and innocuity.
Description
Technical field
The present invention relates to the phosphor synthesis technical field, particularly a kind of rear-earth-doped SiO
2The preparation method of substrate luminescent film.
Background technology
Light-emitting film is a kind of important functional material, compare with traditional luminescent powder, light-emitting film contrast gradient, resolving power, thermal conduction, homogeneity, and aspect such as tack of substrate, outgas speed all demonstrate stronger superiority, all be widely used in colour TV, picture tube, graphoscope, illumination, medical science, nuclear physics and fields such as radiation field, military affairs.Therefore the good light-emitting film of processability has crucial meaning.The preparation method of existing light-emitting film comprises magnetron sputtering, chemical vapour deposition, excimer laser deposition etc., and all there is relatively limitation such as costliness of technology more complicated, equipment in these methods except its distinct advantages.And sol-gel method is considered to prepare most economical, most important, the most promising a kind of method of various films.This technology is that reaction forms solution, colloidal sol, gel and solidifies through wet-chemical with the organic or inorganic compound of metal, forms oxide compound or forms the method for other matrix material through doping treatment through thermal treatment again.Mixing by solution molecule level level can obtain super even, hyperpure solid material, and the organic group that some are shown unique characteristics is incorporated into the organically-modified hybrid material of formation in the mineral compound.The luminescent material matrix of having developed has sulfide and oxide compound two big series, but a large amount of research mainly concentrates on ZnS, CaS, SrS sulfides material.Because sulfide self instability, to water vapor sensitive, this has higher requirement to manufacturing process such as the photoetching of device and cleanings, and influences the permanent stability of device.Compare with sulfide, oxide compound has that chemical stability is good, material category is many, obtain advantages such as three primary colours easily, has caused investigator's extensive concern.Up to the present do not find with rear-earth-doped SiO
2Relevant report for the light-emitting film material of matrix body.
Summary of the invention
The purpose of this invention is to provide a kind of preparation condition gentleness, processing unit simply, does not use noxious solvent to prepare rear-earth-doped SiO
2The method of substrate nano light-emitting film, even, the fine and close nothing cracking in prepared light-emitting film surface, controllable thickness can obtain green, redness, blueness or three primary colours white light thin-film light emitting material.
Implementation procedure of the present invention is as follows:
Rear-earth-doped SiO
2The preparation method of substrate luminescent film comprises the steps:
(1) with tetraethoxy Si (C
2H
5O)
4Be dissolved in ethanol or the propyl alcohol;
(2) above-mentioned solution mixes with the ethanol or the aqueous propanol solution of boric acid;
(3) add hydrochloric acid or glacial acetic acid and regulate pH value 2～3;
(4) aluminum soluble salt is added in the above-mentioned solution, aluminum soluble salt is selected from Al (NO
3)
3, AlCl
3, Al
2(SO
4)
3
(5) add soluble ree Eu
3+, Tb
3+Or Dy
3+One or both of salt, soluble rare-earth salt are Eu
3+, Tb
3+Or Dy
3+Nitrate or hydrochloride;
(6) ageing gets colloidal sol, colloidal sol is done substrate with clean glass or silicon chip, take dip-coating method or spin coating method system film, the thickness of film can be controlled with the rotating speed that lifts number of times or sol evenning machine by regulating pull rate, after the wet film oven dry film is got light-emitting film at 500～1500 ℃ of calcining 2～4h;
Tetraethoxy in the above-mentioned steps: boric acid: aluminum soluble salt: the mol ratio of rare earth soluble salt is 1: 0.2～0.8: 0.001～0.005: 0.001～0.016.
The light-emitting film surface of the present invention preparation evenly, fine and close do not have a cracking, film size of particles is at 1-50nm, controllable thickness.The sol-gel technique that adopts has that synthesis temperature is low, uniform doping, controllable structure, can provide rich and varied coordination environment for light emitting ionic or group by aftertreatment technology, is convenient to modulate the performance of film.The inventive method technology is simple, needing no vacuum equipment, cost is low, raw material is easy to get and nontoxic.
Embodiment
Preparation process of the present invention is under the condition of room temperature or heating, earlier with tetraethoxy (TEOS), dehydrated alcohol or propyl alcohol mix stirring 30 minutes, pressing chemical dose mixes deionized water again with dehydrated alcohol, stirred 30 minutes after equaling in the pH value to add a certain amount of boric acid under the condition of 2-3, at last two solution are mixed and stirred 1 hour, promptly prepare borated solution.Accurately take by weighing a certain amount of Al (NO
3)
3, joining in the above-mentioned solution that has prepared, insulation is 15 minutes behind the heating in water bath to 70 ℃, naturally cools to room temperature, adds a certain amount of soluble rare-earth salt again, makes that the content of rare earth ion is required doping.At last, the solution stirring that mixes more than 4 hours, is packed in the sealing triangular flask, ageing gets colloidal sol.Do substrate with pretreated clean glass or silicon chip, take dip-coating method or spin coating method system film, the thickness of film can be regulated with the rotating speed that lifts number of times or sol evenning machine by regulating pull rate.The wet film 15-30min that at room temperature dries in the air places 100 ℃ of oven dry of loft drier then, naturally cools to room temperature, repeats the film that above process can obtain different thickness.Again film is put into retort furnace and carry out anneal, make the interior temperature of stove slowly be elevated to temperature required (500～1500 ℃) in the certain hour, and under this temperature, be incubated 2～4h, naturally cool to room temperature and promptly receive light-emitting film.
Embodiment 1: preparation Tb
3+: SiO
2The green emitting film
Raw materials used as follows:
Tetraethoxy (TEOS) 15.1ml
Dehydrated alcohol (C
2H
5OH) 32.6ml
Deionized water (H
2O) 2.5ml
Boric acid (H
3BO
3) 0.8657g
Aluminum nitrate (Al (NO
3)
39H
2O) 0.0526g
Terbium trinitrate (Tb (NO
3)
35H
2O) 0.1523g
Preparation process is as follows:
1) with 15.1ml tetraethoxy, 16.3ml dehydrated alcohol, slowly to mix, magnetic agitation is after 30 minutes, the solution A that is uniformly mixed; Accurately measure 16.3ml dehydrated alcohol, 2.5ml deionized water, 0.8657g boric acid mixing stirring 0.5h again, obtain solution B; Then solution A is mixed stirring 1 hour with B, and be 2-3 with concentrated hydrochloric acid adjusting pH value;
2) above-mentioned solution heating is risen to 70 ℃,, in agitator, stir 15min, reduce to room temperature at last, add the 0.1523g Terbium trinitrate and stir more than 4 hours to wherein adding the 0.0526g aluminum nitrate, still aging 48h, thus form colloidal sol;
3) utilize the spin coating method plated film on the clean silicon chip of cleaning, rotating speed is 3kn/min, at 100 ℃ of dry 1h down, then puts into retort furnace annealing 2 hours, and annealing temperature is 750 ℃.Film thickness is about 425nm, and particle size distribution is even, and mainly between 1.30-1.60nm, mean value is 1.490nm, under the ultraviolet excitation, and the film green light.
Embodiment 2: preparation Eu
3+: SiO
2The emitting red light film
Raw materials used as follows:
Tetraethoxy (TEOS) 13.4ml
Dehydrated alcohol (C
2H
5OH) 14.0ml
Deionized water (H
2O) 2.2ml
Boric acid (H
3BO
3) 0.7420g
Aluminum nitrate (Al (NO
3)
39H
2O) 0.0450g
Europium nitrate (Eu (NO
3)
35H
2O) 0.1284g
Preparation process is as follows:
1) with 13.4ml tetraethoxy, 7.0ml dehydrated alcohol, slowly to mix, magnetic agitation is after 30 minutes, the solution A that is uniformly mixed; Accurately measure 7.0ml dehydrated alcohol, 2.2ml deionized water, 0.7420g boric acid mixing stirring 0.5h again, obtain solution B; Then solution A is mixed stirring 1 hour with B, and be 2-3 with concentrated hydrochloric acid adjusting pH value;
2) above-mentioned solution heating is risen 70 ℃,, in agitator, stir 15min, reduce to room temperature at last, add the 0.1284g europium nitrate and stir more than 4 hours, more than the still aging 48h, thereby form colloidal sol to wherein adding the 0.0450g aluminum nitrate;
3) utilize the dip-coating method plated film on the clean silicon chip of cleaning, pull rate is 8cm/min, and lifting the number of plies is 9 layers, at 100 ℃ of dry 1h down, then puts into retort furnace annealing 2 hours, and annealing temperature is 600 ℃.Particle size distribution is even, and mainly near 1.50-2.30nm, mean value is 1.81nm, and under the ultraviolet excitation, film glows.
Embodiment 3: preparation Eu
2+: SiO
2The blue-light-emitting film
Raw materials used as follows:
Tetraethoxy (TEOS) 13.4ml
Dehydrated alcohol (C
2H
5OH) 21.0ml
Deionized water (H
2O) 2.2ml
Boric acid (H
3BO
3) 0.7420g
Aluminum nitrate (Al (NO
3)
39H
2O) 0.0450g
Europium nitrate (Eu (NO
3)
35H
2O) 0.1284g
Preparation process is as follows:
1) at first with 13.4ml tetraethoxy, 10.5ml dehydrated alcohol, slowly to mix, magnetic agitation is after 30 minutes, the solution A that is uniformly mixed; Accurately measure 10.5ml dehydrated alcohol, 2.2ml deionized water, 0.7420g boric acid mixing stirring 0.5h again, obtain solution B; Then solution A is mixed stirring 1 hour with B, and be 2-3 with concentrated hydrochloric acid adjusting pH value;
2) above-mentioned solution heating is risen to 70 ℃,, in agitator, stir 15min, reduce to room temperature at last, add the 0.1284g europium nitrate and stir more than 4 hours, more than the still aging 48h, thereby form colloidal sol to wherein adding the 0.0450g aluminum nitrate;
3) utilize the spin-coating method plated film on the clean silicon chip of cleaning, spin speed is 3kn/min, 30 seconds spin coating time, at 100 ℃ of dry 15min down, then put into retort furnace annealing 2 hours, and annealing temperature is 750 ℃.Film thickness is about 450nm, under the ultraviolet excitation, and the film blue light-emitting.
Embodiment 4: preparation Eu, Dy mixes SiO altogether
2The blue-light-emitting film
Raw materials used as follows:
Tetraethoxy (TEOS) 13.4ml
Dehydrated alcohol (C
2H
5OH) 21.0ml
Deionized water (H
2O) 2.2ml
Boric acid (H
3BO
3) 0.7420g
Aluminum nitrate (Al (NO
3)
39H
2O) 0.0450g
Europium nitrate (Eu (NO
3)
35H
2O) 0.1284g
Dysprosium trinitrate (Dy (NO
3)
35H
2O) 0.0131g
Preparation process is as follows:
1) at first with 13.4ml tetraethoxy, 10.5ml dehydrated alcohol, slowly to mix, magnetic agitation is after 30 minutes, the solution A that is uniformly mixed; Accurately measure 10.5ml dehydrated alcohol, 2.2ml deionized water, 0.7420g boric acid mixing stirring 0.5h again, obtain solution B; Then solution A is mixed stirring 1 hour with B, and be 2-3 with concentrated hydrochloric acid adjusting pH value;
2) above-mentioned solution heating is risen to 70 ℃,, in agitator, stir 15min, reduce to room temperature at last, add 0.1284g europium nitrate and 0.0131g Dysprosium trinitrate and stir more than 4 hours, more than the still aging 48h, thereby form colloidal sol to wherein adding the 0.0450g aluminum nitrate;
3) utilize the dip-coating method plated film on the clean silicon chip of cleaning, pull rate is 8cm/min, and lifting the number of plies is 4 layers, at 100 ℃ of dry 15min down, then puts into retort furnace annealing 2 hours, and annealing temperature is 850 ℃.Under the ultraviolet excitation, the film blue light-emitting.
Embodiment 5: preparation Eu, Dy mixes SiO altogether
2The three-color light-emitting film
Raw materials used as follows:
Tetraethoxy (TEOS) 13.4ml
Dehydrated alcohol (C
2H
5OH) 21.0ml
Deionized water (H
2O) 2.2ml
Boric acid (H
3BO
3) 0.7420g
Europium nitrate (Eu (NO
3)
35H
2O) 0.1284g
Dysprosium trinitrate (Dy (NO
3)
35H
2O) 0.0131g
Preparation process is as follows:
1) at first with 13.4ml tetraethoxy, 10.5ml dehydrated alcohol, slowly to mix, magnetic agitation is after 30 minutes, the solution A that is uniformly mixed; Accurately measure 10.5ml dehydrated alcohol, 2.2ml deionized water, 0.7420g boric acid mixing stirring 0.5h again, obtain solution B; Then solution A is mixed stirring 1 hour with B, and be 2-3 with concentrated hydrochloric acid adjusting pH value;
2) above-mentioned solution is added 0.1284g europium nitrate and 0.0131g Dysprosium trinitrate and stir more than 4 hours, more than the still aging 48h, thereby form colloidal sol;
3) utilize the spin-coating method plated film on the clean silicon chip of cleaning, spin speed is 3kn/min, 30 seconds spin coating time, at 100 ℃ of dry 15min down, then put into retort furnace annealing 2 hours, and annealing temperature is 850 ℃.Film thickness is about 450nm, and under the UV-irradiation, film is sent out red, green, blue three primary colours light.
Embodiment 6: preparation Eu, Tb mixes SiO altogether
2Blue light luminescent film
Raw materials used as follows:
Tetraethoxy (TEOS) 22.4ml
Dehydrated alcohol (C
2H
5OH) 23.4ml
Deionized water (H
2O) 7.2ml
Boric acid (H
3BO
3) 1.2368g
Aluminum nitrate (Al (NO
3)
39H
2O) 0.0750g
Terbium trinitrate (Tb (NO
3)
35H
2O) 0.1305g
Europium nitrate (Eu (NO
3)
3.5H
2O) 0.2620g
Preparation process is as follows:
1) at first with 22.4ml tetraethoxy, 11.7ml dehydrated alcohol, slowly to mix, magnetic agitation is after 30 minutes, the solution A that is uniformly mixed; Accurately measure 11.7ml dehydrated alcohol, 22.4ml deionized water, 1.2368g boric acid mixing stirring 0.5h again, obtain solution B; Then solution A is mixed stirring 1 hour with B, and be 2-3 with concentrated hydrochloric acid adjusting pH value;
2) above-mentioned solution heating is risen 70 ℃,, in agitator, stir 15min, reduce to room temperature at last, add 0.1305g Terbium trinitrate and 0.2620g europium nitrate and stir more than 4 hours, more than the still aging 48h, thereby form colloidal sol to wherein adding the 0.0750g aluminum nitrate;
3) utilize the spin-coating method plated film on the clean silicon chip of cleaning, spin speed is 3kn/min, 30 seconds spin coating time, at 100 ℃ of dry 15min down, then put into retort furnace annealing 2 hours, and annealing temperature is 850 ℃.Under the ultraviolet excitation, the sample blue light-emitting.
Claims (6)
1, a kind of rear-earth-doped SiO
2The preparation method of substrate luminescent film comprises the steps:
(1) with tetraethoxy Si (C
2H
5O)
4Be dissolved in ethanol or the propyl alcohol;
(2) above-mentioned solution mixes with the ethanol or the aqueous propanol solution of boric acid;
(3) regulate pH value 2～3;
(4) aluminum soluble salt is added in the above-mentioned solution;
(5) add soluble ree Eu
3+, Tb
3+Or Dy
3+One or both of salt;
(6) ageing gets colloidal sol, the preparation film, with film 500～1500 ℃ calcine light-emitting film;
Tetraethoxy in the above-mentioned steps: boric acid: aluminum soluble salt: the mol ratio of rare earth soluble salt is 1: 0.2～0.8: 0.001～0.005: 0.001～0.016.
2, rear-earth-doped SiO according to claim 1
2The preparation method of substrate luminescent film is characterized in that: aluminum soluble salt is selected from Al (NO
3)
3, AlCl
3, Al
2(SO
4)
3
3, rear-earth-doped SiO according to claim 1
2The preparation method of substrate luminescent film is characterized in that: soluble rare-earth salt is Eu
3+, Tb
3+Or Dy
3+Nitrate or hydrochloride.
4, rear-earth-doped SiO according to claim 1
2The preparation method of substrate luminescent film is characterized in that: add hydrochloric acid or glacial acetic acid and regulate the pH value.
5, rear-earth-doped SiO according to claim 1
2The preparation method of substrate luminescent film is characterized in that: film is at 500～1500 ℃ of calcining 2～4h.
6, according to one of any described rear-earth-doped SiO of claim 1 to 5
2The preparation method of substrate luminescent film, it is characterized in that: colloidal sol is done substrate with clean glass or silicon chip, take dip-coating method or spin coating method system film, the thickness of film can be controlled with the rotating speed that lifts number of times or sol evenning machine by regulating pull rate, calcines after the wet film oven dry again.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101950786A (en) * | 2010-09-13 | 2011-01-19 | 北京大学 | Method for preparing silicon-based light emitting diode (LED) |
| 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 |
| CN101781559B (en) * | 2010-02-08 | 2013-01-23 | 西北大学 | Metal ion doped nanometer silicon-based luminescent material and preparation method thereof |
| CN105293941A (en) * | 2015-11-16 | 2016-02-03 | 宁波大学 | Preparation method for glass film containing divalent-europium-ion-doped strontium iodide microcrystalline |
| CN105428991A (en) * | 2015-12-16 | 2016-03-23 | 中国科学院西安光学精密机械研究所 | Solid mode-locked laser absorption device and preparation method thereof |
| CN107601516A (en) * | 2017-09-26 | 2018-01-19 | 湖北工程学院 | A kind of carbon coating boron doping silicon dioxide nano material and preparation method thereof |
| CN110143765A (en) * | 2019-05-16 | 2019-08-20 | 辽宁师范大学 | With the fluorescent silicon dioxide film and preparation method of the preparation of amphipathic AIE molecule |
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| US20030024275A1 (en) * | 1999-04-09 | 2003-02-06 | Kanishka Tankala | Method of fabrication of rare earth doped preforms for optical fibers |
Non-Patent Citations (1)
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781559B (en) * | 2010-02-08 | 2013-01-23 | 西北大学 | Metal ion doped nanometer silicon-based luminescent material and preparation method thereof |
| CN101950786A (en) * | 2010-09-13 | 2011-01-19 | 北京大学 | Method for preparing silicon-based light emitting diode (LED) |
| CN101950786B (en) * | 2010-09-13 | 2013-03-27 | 北京大学 | Method for preparing silicon-based light emitting diode (LED) |
| 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 |
| CN102154009B (en) * | 2011-03-08 | 2013-01-23 | 西北大学 | SiO2: RE light-emitting film taking TiO2 nanotube array as carrier and preparation method thereof |
| CN105293941A (en) * | 2015-11-16 | 2016-02-03 | 宁波大学 | Preparation method for glass film containing divalent-europium-ion-doped strontium iodide microcrystalline |
| CN105428991A (en) * | 2015-12-16 | 2016-03-23 | 中国科学院西安光学精密机械研究所 | Solid mode-locked laser absorption device and preparation method thereof |
| CN105428991B (en) * | 2015-12-16 | 2019-06-28 | 中国科学院西安光学精密机械研究所 | Preparation method of solid mode-locked laser absorption device |
| CN107601516A (en) * | 2017-09-26 | 2018-01-19 | 湖北工程学院 | A kind of carbon coating boron doping silicon dioxide nano material and preparation method thereof |
| CN107601516B (en) * | 2017-09-26 | 2019-09-06 | 湖北工程学院 | A kind of carbon coating boron doping silica nano material and preparation method thereof |
| CN110143765A (en) * | 2019-05-16 | 2019-08-20 | 辽宁师范大学 | With the fluorescent silicon dioxide film and preparation method of the preparation of amphipathic AIE molecule |
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