CN101555405A - Adjustable photochromic phosphor powder, phosphor thin film, preparation method and application thereof - Google Patents
Adjustable photochromic phosphor powder, phosphor thin film, preparation method and application thereof Download PDFInfo
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- CN101555405A CN101555405A CNA200910046433XA CN200910046433A CN101555405A CN 101555405 A CN101555405 A CN 101555405A CN A200910046433X A CNA200910046433X A CN A200910046433XA CN 200910046433 A CN200910046433 A CN 200910046433A CN 101555405 A CN101555405 A CN 101555405A
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Abstract
The invention discloses an adjustable photochromic phosphor powder, a phosphor thin film, and the preparing method and the application thereof. The composition general formula of the phosphor powder is ZnCd<x>O< (1+x)>: S<y>, wherein, x and y are mole number, x is equal to 0.01-1, and y is equal to 0.001-0.01. The phosphor can be excited by broadband ultraviolet or blue/violet laser. In the preparing method, 1) a cadmium source and a zinc source are grinded to obtain a precursor, wherein, the molar ratio of zinc element in the zinc source to cadmium element in the cadmium source is 1 to (0.01-1); 2) the precursor is sintered for 1-4 hours under 650-850 DEG C. Methyl methacrylate polymer is used as a matrix and the adjustable photochromic phosphor powder is used as a luminophor to obtain the adjustable photochromic phosphor thin film. The phosphor powder and the phosphor thin film have the characteristics of high luminescence color purity and stable chemical and light-heat properties, can be applied to the manufacturing of LEDs light-emitting devices and realize the controllable adjustment of the excitation and the emission wavelength of LED-luminescent materials.
Description
Technical field
The present invention relates to field of light emitting materials, specifically disclose a kind of can be by broadband ultraviolet or royal purple optical excitation and photochromic fluorescent material with adjustable and preparation method.
Background technology
In recent years, a revolution of have swepting the globe is just being experienced in white light LEDs s illumination.The semiconductor LED illumination is as third generation light source, and luminous efficiency is 10 times of incandescent light, and the life-span is 100 times of incandescent light., high reliability energy-conservation with it, no mercury etc. are difficult displaced advantage, have penetrated into our life, and will become the main flow of illumination in long period.
The implementation of white light LEDs s is mainly the chip and the combination of gold-tinted fluor of blue light or royal purple light at present, the parameter and the luminescent spectrum of typical products are as follows: electric current 20mA, voltage 3.0～3.5V, brightness～1500mcd, colour temperature 6400K～10000K, chromaticity coordinates x=0.298～0.315, y=0.294～0.330, colour rendering index Ra=50～65.Red part is less in the emmission spectrum of its combination, so the colour rendering index of product is low, can not realize warm white.High-end white light LEDs s will possess three primary colours at least, just can make emmission spectrum realize all standing that the visible region scope is interior.Because white light LEDs s light efficiency and color developing, present application concentrates on mainly that LCD is backlight, portable lighting, information show.So white light LEDs s has very big development space, also face severe technological challenge.
ZnO is important semiconductor material, in atmosphere, be not easy oxidized, have very high chemistry and thermostability, exciton bind energy big (exciton bind energy is 60meV, is ZnSe and GaN sill 3 times), energy gap is about 3.36eV, be difficult under the room temperature by thermal excitation, realize stimulated emission easily, compound under the permission exciton high temperature, be to make most promising material in the optics relevant with exciton.Simultaneously, the lattice imperfection of ZnO crystal inside or adulterated impurity produce tremendous influence to its electricity and optical property.Lattice imperfection in the ZnO crystal for example oxygen defect, zinc defective, zinc gap, the anti-displacement of oxygen etc. can cause the visible emissivity of 400～730nm.Therefore, ZnO doping prepares white light LEDs has caused scientific circles with the research of luminescent material great attention.
Because the electronegativity of cadmium, element sulphur and zinc and oxygen element, crystalline structure etc. are much at one, the doping of cadmium, sulphur causes the lattice imperfection of ZnO probably, causes that the photoelectric property of ZnO system takes place significantly to change.But, there is evident difference between the ionic radius of cadmium, stability and the growth temperature, in the preparation process of ZnO, the doping of cadmium is very difficult.How to use simple preparation method make cadmium element effectively codoped enter the lattice of zinc oxide, obtain the light activated photochromic adjustable fluorescent material/film of broadband ultraviolet or royal purple, the needs that adapt to white light LEDs s illumination and other luminescent device are difficult problems that present scientific and technological circle need solution badly.
Purpose of the present invention is exactly the difficult problem that will solve white light LEDs s light efficiency and color developing, has proposed a kind of new white light version: the red greenish-yellow three-color phosphor of royal purple light LED+, emmission spectrum is contained whole visible regions.By the adjustment of fluorescent material ratio, make that the colour temperature of LED is adjustable in 2000～10000 scope, realize high-color rendering.By the coupling of fluorescent powder coated technology and powder-making technique, luminous efficiency is optimized simultaneously, realizes that the high brightness high color rendering index (CRI) is luminous.
Summary of the invention
The present invention aims to provide a kind of photochromic adjustable fluorescent material, can be by broadband ultraviolet or royal purple optical excitation.
Invent second purpose and be to provide the photochromic adjustable fluorescence membrane that utilizes above-mentioned fluorescent material preparation.
The present invention also provides the preparation method of above-mentioned fluorescent material and fluorescence membrane.
The present invention also aims to above-mentioned fluorescent material and fluorescence membrane are applied to white light LEDs s luminescent device.
To achieve the above object of the invention, the present invention is achieved by the following technical programs:
A kind of photochromic adjustable fluorescent material, it forms general formula is ZnCd
xO
(1+x): S
y, wherein x, y and z are mole number, x=0.01～1, y=0.0001～0.01.This fluorescent material can excite under broadband ultraviolet or royal purple light.
The preparation method of above-mentioned broadband ultraviolet or the light activated photochromic adjustable fluorescent material of royal purple may further comprise the steps:
1) cadmium source and zinc source were at room temperature ground 15～30 minutes, promptly get precursor, wherein: in the zinc source in zinc element and the cadmium source mol ratio of cadmium element be 1: (0.01～1);
2) with above-mentioned precursor under conditions of air, in 650～850 ℃ of sintering 1～4 hour.
Resulting sinter is ground, washs, drying.
Described cadmium source is selected from the mixture of mixture, Cadmium oxide and fusing assistant of Cadmium chloride fine powder, Cadmium chloride fine powder, Cadmium Sulfide, Cadmium oxide, Cadmium Sulphate, Cadmium Sulfide and fusing assistant or the mixture of Cadmium Sulphate and fusing assistant; Preferred Cadmium chloride fine powder.Wherein, the preferred ammonium chloride of fusing assistant, the mol ratio of ammonium chloride and Cadmium Sulfide, Cadmium oxide or Cadmium Sulphate is (1～3): 1.
Described zinc source can be selected zinc sulphide for use, or the mixture of elemental sulfur and zinc oxide, or the mixture of elemental sulfur and zinc acetate, and wherein: the mol ratio of elemental sulfur and zinc oxide or zinc acetate is 1: 0.8～1.2.
The mol ratio of zinc element and cadmium element is determined by cadmium element mol ratio in zinc element in the zinc source and the cadmium source in the products therefrom.
The light activated photochromic adjustable fluorescence membrane of a kind of broadband ultraviolet or royal purple is a matrix with the methyl methacrylate polymer, is twinkler with above-mentioned photochromic adjustable fluorescent material.
The preparation method of above-mentioned photochromic adjustable fluorescence membrane comprises the steps:
1) photochromic adjustable fluorescent material, tensio-active agent and water are carried out ultra-sonic dispersion, under 60～70 ℃ of conditions, stir and obtain precursor;
2) in above-mentioned precursor, add methyl methacrylate (MMA) monomer and initiator, under 70～80 ℃ of water bath condition, stirred 5～8 hours, promptly get the film precursor; Wherein: the monomeric mass ratio of fluorescent material and MMA is 1: (10～100);
3) above-mentioned film precursor is smeared made film.
Described tensio-active agent is selected from benzene sulfonic acid sodium salt or sodium laurylsulfonate, and the mass volume ratio of photochromic adjustable fluorescent material water is 1: (50～500) g/L; Surfactant concentrations is 0.05～0.15g/L.
Initiator can be selected Potassium Persulphate for use, and this is 1 for the monomeric quality of initiator and MMA: (100～300)
The performance test results shows, the excitation wavelength of broadband of the present invention ultraviolet or the light activated photochromic adjustable fluorescent material/film of royal purple can be at 250nm to selecting arbitrarily between the 450nm, emission wavelength can be from the 520nm red shift to 620nm, and therefore luminescent material of the present invention can be used for white light LEDs s illumination and other luminescent device etc.
Compared with prior art, the present invention has following beneficial effect:
1) the present invention has realized transition metal Cd doping is entered the lattice of zinc oxide, in the luminescent material that obtains, ZnO is as matrix, and the lattice imperfection that Cd caused is a luminescence center, the compound excitation spectrum generation broadening that makes of transition metal Cd, red shift is to the long wave ultraviolet light district.
2) photochromic adjustable fluorescent material/film of the present invention can excite under broadband ultraviolet or royal purple light, has characteristics such as chemistry and optical property are stable, and luminous efficiency is higher than present commercial fluorescent material.
2) preparation technology of the present invention is simple to operation, and raw material is cheap and easy to get, is fit to suitability for industrialized production, and reaction process does not have three industrial wastes substantially, has environmental protection, less energy-consumption, high benefit characteristics.
The method that we adopt thermooxidizing to decompose ZnS has prepared a small amount of S adulterated broadband ultraviolet or royal purple light activated ZnCdO semiconductor nano luminescent material and light-emitting film, can realize that by this method the LED-luminescent material excites the controllable adjustment with emission wavelength.By regulating the composite concentration of Cd, excitation wavelength can be regulated between the 450nm at 250nm, and emission wavelength can be from the 520nm red shift to 620nm.Grain diameter is less than 1 μ m.After PMMA hydridization, can be made into uniform and stable light-emitting film.This fluorescent material and film have illuminant colour purity height, chemistry and the stable characteristics of light thermal property, and luminous efficiency is higher than present commercial fluorescent material, can be used for white light LEDs s illumination and other luminescent device.In addition, preparation technology of the present invention is simple to operation, and raw material is cheap and easy to get, is fit to suitability for industrialized production, and reaction process does not have three industrial wastes substantially, has environmental protection, less energy-consumption, high benefit characteristics.
Description of drawings
The fluorescence spectrum figure of photochromic adjustable fluorescent material of Fig. 1, Fig. 2 and film.
Fig. 3 is the XRD figure of photochromic adjustable fluorescent material.
Fig. 4 is the SEM figure of photochromic adjustable fluorescent material.
Embodiment
The invention will be further described below by embodiment, and its purpose only is better to understand content of the present invention and unrestricted protection scope of the present invention.
1) with 0.001mol CdCl
2At room temperature ground 15～30 minutes with 0.02mol ZnS, promptly get precursor;
2) above-mentioned precursor is inserted in the crucible of 50ml, seal with lid; Put into retort furnace in 700 ℃ of sintering 3 hours;
3) after the cooling, take out sinter and ground 5～10 minutes, use the washing of deionized water and alcohol, oven dry promptly gets photochromic adjustable fluorescent material, and it is ZnCd that the energy dispersive X-ray spectrum is measured its composition general formula
0.05O
1.05: S
y, y=0.0001～0.01 wherein.Its particle size range is at 100nm～2um, and SEM schemes as shown in Figure 4.
4) get the above-mentioned photochromic adjustable fluorescent material that obtains of 0.5 gram, mix, carry out ultra-sonic dispersion, under 65 ℃ of water bath condition, stirred 60 minutes, promptly get precursor with 200ml 0.15g/L benzene sulfonate aqueous solution;
5) in above-mentioned precursor, add 6 gram MMA monomers and 0.05 gram Potassium Persulphate initiator, under 75 ℃ of water bath condition, stirred 7 hours, promptly get the film precursor;
6) above-mentioned film precursor is smeared instrument with rotation and be coated onto on the quartz plate, promptly get photochromic adjustable fluorescence membrane.
The XRD figure of gained fluorescent material sample (test condition is: voltage 40kV, and electric current 40mA, 4 ° of sweep velocitys/min) show: the sample principal phase is a zinc oxide, that is, the gained luminescent material is as matrix (as shown in Figure 3) with zinc oxide.
(test condition is the fluorescence spectrum figure of gained fluorescent material sample and fluorescence membrane: λ ex=400nm, λ em=530nm, slit width 5nm, voltage 500V, sweep velocity 600nm/min) show: this luminescent material has very strong absorption in the long wave ultraviolet region of 250～400nm, at 500～600nm very strong emission (as shown in Figure 1) is arranged.
The difference of present embodiment and embodiment 1 is: ZnS and CdCl
2Mol ratio be 1: 0.01, all the other contents are described with embodiment 1, thereby obtain target product, energy dispersive X-ray spectrum is measured it, and to form general formula be ZnCd
0.01O
1.01: S
y, y=0.0001～0.01 wherein.The XRD analysis result of gained sample and fluorescent spectroscopy result are with described in the embodiment 1.
The difference of present embodiment and embodiment 1 is: ZnS and CdCl
2Mol ratio be 1: 0.03, all the other contents are described with embodiment 1, thereby obtain target product, energy dispersive X-ray spectrum is measured it, and to form general formula be ZnCd
0.03O
1.03: S
y, y=0.0001～0.01 wherein.The XRD analysis result of gained sample and fluorescent spectroscopy result are with described in the embodiment 1.
Embodiment 4
The difference of present embodiment and embodiment 1 is: ZnS and CdCl
2Mol ratio be 1: 0.07, all the other contents are described with embodiment 1, thereby obtain target product, energy dispersive X-ray spectrum is measured it, and to form general formula be ZnCd
0.07O
1.07: S
y, y=0.0001～0.01 wherein.The XRD analysis result of gained sample and fluorescent spectroscopy result are with described in the embodiment 1.
The difference of present embodiment and embodiment 1 is: ZnS and CdCl
2Mol ratio be 1: 0.1, all the other contents are described with embodiment 1, thereby obtain target product, energy dispersive X-ray spectrum is measured it, and to form general formula be ZnCd
0.1O
1.1: S
y, y=0.0001～0.01 wherein.The XRD analysis result of gained sample and fluorescent spectroscopy result are with described in the embodiment 1.
Embodiment 6
The difference of present embodiment and embodiment 1 is: ZnS and CdCl
2Mol ratio be 1: 0.5, the fluorescent spectroscopy result is Fig. 2, all the other contents are described with embodiment 1, thereby obtain target product, energy dispersive X-ray spectrum is measured it, and to form general formula be ZnCd
0.5O
1.5: S
y, y=0.0001～0.01 wherein.The XRD analysis result of gained sample is with described in the embodiment 1.
The difference of present embodiment and embodiment 1 is: ZnS and CdCl
2Mol ratio be 1: 0.4, all the other contents are described with embodiment 1, thereby obtain target product, energy dispersive X-ray spectrum is measured it, and to form general formula be ZnCd
0.4O
1.4: S
y, y=0.0001～0.01 wherein.The fluorescent spectroscopy result of gained sample is Fig. 2, and XRD analysis result is with described in the embodiment 1.
Embodiment 8
The difference of present embodiment and embodiment 1 is: ZnS and CdCl
2Mol ratio be 1: 1, all the other contents are described with embodiment 1, thereby obtain target product, energy dispersive X-ray spectrum is measured it, and to form general formula be ZnCdO
2: S
y, y=0.0001～0.01 wherein.Fluorescent spectroscopy result such as Fig. 2 of gained sample, XRD analysis result is with described in the embodiment 1.
Embodiment 9
1) with 0.001mol CdS, 0.002molNH
4Cl and 0.02mol ZnS at room temperature ground 15～30 minutes, promptly got precursor;
2) above-mentioned precursor is inserted in the crucible of 50ml, seal with lid; And the crucible of sealing put into retort furnace in 800 ℃ of sintering 3 hours;
3) after the cooling, take out sinter and ground 5～10 minutes, use the washing of deionized water and alcohol repeatedly, oven dry promptly gets photochromic adjustable fluorescent material, and it is ZnCd that the energy dispersive X-ray spectrum is measured its composition general formula
0.05O
1.05Sy, wherein y=0.0001～0.01.
4) get the above-mentioned photochromic adjustable fluorescent material that obtains of 0.5 gram, mix for the 0.05g/L sodium dodecyl sulfate aqueous solution, carry out ultra-sonic dispersion, under 65 ℃ of water bath condition, stirred 30 minutes, promptly get precursor with 50ml concentration;
5) in above-mentioned precursor, add 45 gram MMA monomers and 0.2 gram Potassium Persulphate initiator, under 75 ℃ of water bath condition, stirred 5 hours, promptly get the film precursor;
6) above-mentioned precursor is smeared instrument with rotation and be coated onto on the quartz plate, promptly get photochromic adjustable fluorescence membrane.
The XRD analysis result of gained sample and fluorescent spectroscopy result are with described in the embodiment 1.
1) with 0.001mol CdSO
4, 0.003molNH
4Cl and 0.02mol ZnS at room temperature ground 15～30 minutes, promptly got precursor;
2) above-mentioned precursor is inserted in the crucible of 50ml, seal with lid; The crucible of sealing is put into retort furnace in 650 ℃ of sintering 2 hours;
3) after the cooling, take out sinter and ground 5～10 minutes, use the washing of deionized water and alcohol repeatedly, oven dry promptly gets photochromic adjustable fluorescent material, and it is ZnCd that the energy dispersive X-ray spectrum is measured its composition general formula
0.05O
1.05S
y, y=0.0001～0.01 wherein.
4) be that the benzene sulfonic acid sodium salt solution of 0.1g/L mixes with above-mentioned photochromic adjustable fluorescent material that obtains of above-mentioned 0.5g and 25ml concentration, carry out ultra-sonic dispersion, under 65 ℃ of water bath condition, stirred 90 minutes, promptly get precursor;
5) in above-mentioned precursor, add 20g MMA monomer and 0.1g Potassium Persulphate initiator, under 75 ℃ of water bath condition, stirred 7 hours, promptly get the film precursor; Wherein: the monomeric mass ratio of gold-tinted fluorescent material and MMA is 1: 10;
6) above-mentioned precursor is smeared instrument with rotation and be coated onto on the quartz plate, promptly get film.
The XRD analysis result of gained sample and fluorescent spectroscopy result are with described in the embodiment 1.
Embodiment 11
The difference of present embodiment and embodiment 1 is: the zinc source of selecting for use is 0.02mol ZnO and 0.02mol S, and all the other contents are described with embodiment 1, thereby obtains target product, and it is ZnCd that the energy dispersive X-ray spectrum is measured its composition general formula
0.05O
1.05: S
y, y=0.0001～0.01 wherein.The XRD analysis result of gained sample and fluorescent spectroscopy result are with described in the embodiment 1.
Embodiment 12
The difference of present embodiment and embodiment 1 is: the zinc source of selecting for use is 0.02mol Zn (Ac)
2With 0.02mol S, the cadmium source of selecting for use is 0.05mol CdO and 0.1mol NH
4Cl, all the other contents are described with embodiment 1, thereby obtain target product, and it is ZnCd that the energy dispersive X-ray spectrum is measured its composition general formula
0.05O
1.05S
y, y=0.0001～0.01 wherein.The XRD analysis result of gained sample and fluorescent spectroscopy result are with described in the embodiment 1.
Claims (10)
1, a kind of photochromic adjustable fluorescent material is characterized in that, the composition general formula is ZnCd
xO
(1+x): S
y, x and y are mole number, x=0.01～1, y=0.0001～0.01.
2, the described a kind of photochromic adjustable fluorescent material of claim 1 is characterized in that particle size range is 300nm～500nm.
3, the preparation method of the described a kind of photochromic adjustable fluorescent material of claim 1 is characterized in that, comprises the steps:
1) cadmium source and zinc source ground obtain precursor, wherein: in the zinc source in zinc element and the cadmium source mol ratio of cadmium element be 1: (0.01～1);
Described zinc source is a zinc sulphide, or the mixture of elemental sulfur and zinc oxide, or the mixture of elemental sulfur and zinc acetate; Wherein the mol ratio of elemental sulfur and zinc oxide or zinc acetate is (0.8～1.2): 1.
Described cadmium source is selected from the mixture of mixture, Cadmium oxide and fusing assistant of Cadmium chloride fine powder, Cadmium Sulfide, Cadmium oxide, Cadmium Sulphate, Cadmium Sulfide and fusing assistant or the mixture of Cadmium Sulphate and fusing assistant;
2) with above-mentioned precursor 650～850 ℃ of following sintering 1～4 hour.
4, the preparation method of the described a kind of photochromic adjustable fluorescent material of claim 3 is characterized in that, described fusing assistant is an ammonium chloride, and the mol ratio of ammonium chloride and Cadmium Sulfide, Cadmium oxide or Cadmium Sulphate is (1～3): 1.
5, a kind of photochromic adjustable fluorescence membrane, comprise matrix and twinkler, it is characterized in that described matrix comprises polymethylmethacrylate, twinkler is the described photochromic adjustable fluorescent material of claim 1, and the mass ratio of photochromic adjustable fluorescent material and methyl methacrylate monomer is 1: (10～100).
6, the preparation method of the described a kind of photochromic adjustable fluorescence membrane of claim 5 is characterized in that, comprises the steps:
1) photochromic adjustable fluorescent material and tensio-active agent and water are carried out ultra-sonic dispersion, under 60～70 ℃ of conditions, stirred 30～90 minutes, promptly get precursor; The mass volume ratio of tensio-active agent and water is 0.05～0.15g/L; The mass volume ratio of photochromic adjustable fluorescent material and water is 1: (50～500) g/L.
2) in above-mentioned precursor, add methyl methacrylate monomer and initiator, under 70～80 ℃ of water bath condition, stirred 5～8 hours, promptly get the film precursor; Wherein: the mass ratio of fluorescent material and methyl methacrylate monomer is 1: (10～100);
3) above-mentioned film precursor is smeared into film.
7, the preparation method of the described a kind of photochromic adjustable fluorescence membrane of claim 5 is characterized in that, described tensio-active agent is benzene sulfonic acid sodium salt or sodium laurylsulfonate;
8, the preparation method of the described a kind of photochromic adjustable fluorescence membrane of claim 5 is characterized in that, described initiator is a Potassium Persulphate; And the mass ratio of Potassium Persulphate and methyl methacrylate monomer is 1: (100～300).
9, the application of the described a kind of photochromic adjustable fluorescent material of claim 1 aspect preparation LEDs luminescent device.
10, the application of the described a kind of photochromic adjustable fluorescence membrane of claim 4 aspect preparation LEDs luminescent device.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102251298A (en) * | 2011-06-03 | 2011-11-23 | 大连交通大学 | Preparation method of composite luminescent fiber nanomaterial |
| CN105315695A (en) * | 2015-10-29 | 2016-02-10 | 严梅霞 | Agricultural thin film and production method thereof |
| RU2610614C2 (en) * | 2015-04-13 | 2017-02-14 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Алтайский государственный университет" | Light-converting metal-containing polymerisable compositions and method for production thereof |
-
2009
- 2009-02-20 CN CN200910046433XA patent/CN101555405B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102251298A (en) * | 2011-06-03 | 2011-11-23 | 大连交通大学 | Preparation method of composite luminescent fiber nanomaterial |
| CN102251298B (en) * | 2011-06-03 | 2012-11-14 | 大连交通大学 | Preparation method of composite luminescent fiber nanomaterial |
| RU2610614C2 (en) * | 2015-04-13 | 2017-02-14 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Алтайский государственный университет" | Light-converting metal-containing polymerisable compositions and method for production thereof |
| CN105315695A (en) * | 2015-10-29 | 2016-02-10 | 严梅霞 | Agricultural thin film and production method thereof |
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