CN111057535A - Mn (manganese)4+Preparation method of doped fluoride homogeneous-coated red luminescent crystal - Google Patents
Mn (manganese)4+Preparation method of doped fluoride homogeneous-coated red luminescent crystal Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 70
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000011572 manganese Substances 0.000 title description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title description 2
- 229910052748 manganese Inorganic materials 0.000 title description 2
- 239000011159 matrix material Substances 0.000 claims abstract description 13
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 5
- 229910052701 rubidium Inorganic materials 0.000 claims abstract description 4
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 claims description 14
- AHLATJUETSFVIM-UHFFFAOYSA-M rubidium fluoride Chemical compound [F-].[Rb+] AHLATJUETSFVIM-UHFFFAOYSA-M 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 11
- 239000012452 mother liquor Substances 0.000 claims description 10
- OJOWXSLGSMTXEO-UHFFFAOYSA-H [Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[K+].[K+].[K+].[K+].[K+].[K+] Chemical compound [Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[K+].[K+].[K+].[K+].[K+].[K+] OJOWXSLGSMTXEO-UHFFFAOYSA-H 0.000 claims description 9
- 229940119177 germanium dioxide Drugs 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims 1
- -1 hexafluoromanganic acid Potassium Chemical compound 0.000 claims 1
- 230000005284 excitation Effects 0.000 abstract description 10
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 239000008204 material by function Substances 0.000 abstract 1
- 229910004074 SiF6 Inorganic materials 0.000 description 23
- 239000000463 material Substances 0.000 description 9
- 230000001376 precipitating effect Effects 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 238000000295 emission spectrum Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 238000000695 excitation spectrum Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000002109 crystal growth method Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
- C09K11/615—Halogenides
- C09K11/616—Halogenides with alkali or alkaline earth metals
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/664—Halogenides
- C09K11/665—Halogenides with alkali or alkaline earth metals
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/674—Halogenides
- C09K11/675—Halogenides with alkali or alkaline earth metals
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Abstract
The invention relates to the field of inorganic functional materials, and discloses Mn4+A preparation method of doped fluoride homogeneous-coated luminescent crystal. Mn according to the invention4+The chemical composition of the doped fluoride homogeneous coated luminescent crystal is A2MF6@A2MF6:Mn4+；A2MF6:Mn4+Is an outer layer of matrix crystals, A2MF6:Mn4+Is an inner layer luminescent crystal; a is Cs or Rb, M is one of Si, Ge and Ti; x is the corresponding doping Mn4+Ion relative M4+Molar percentage coefficient of ion, 0<x is less than or equal to 0.10. The invention relates toThe fluoride luminescent crystal has good light transmission, shows a series of narrow-band emission under the excitation of blue light, and has high luminescent efficiency.
Description
Technical Field
The invention relates to Mn4+A preparation method of doped fluoride homogeneous-wrapped luminescent crystal, in particular to Mn for a blue light-emitting diode4+A method for growing same substrate crystal on the surface of doped fluoride red luminescent crystal belongs to the field of inorganic functional material preparation.
Background
White light semiconductor (LED) solid state lighting has been widely used in the fields of lighting, decoration, etc. due to its numerous advantages. However, such lighting has some obvious disadvantages, the efficiency of the phosphor greatly affects the luminous efficiency of the white LED, and the phosphor is not suitable for application to high-power white LED devices due to its poor heat dissipation. Compared with powder materials, the same crystal material has better light transmittance and lower refraction and diffuse reflection performance compared with the powder material, so that the utilization rate of incident light is higher. In addition, the crystal has better heat dissipation performance, so that the luminescent crystal material has more important application front coating on semiconductor solid-state lighting.
In recent years, Mn4+Doped fluoride red phosphors have attracted a great deal of attention. Such as Mn4+Doped A2BF6The luminescence properties of red-emitting powder materials (A is Na, K, Rb, etc.; B is Ti, Si, Sn, Ge, etc.) have been widely reported. In addition, a few fluoride luminescent crystal materials have been reported. Such Mn4+Doped fluoride phosphors have very good luminescent properties, but they also suffer from a serious disadvantage in that they are very weak against water and are very susceptible to hydrolysis by water, thereby affecting their luminous efficiency. In order to solve the problem, organic or inorganic materials are often used to coat the surfaces of the materials, but the organic or inorganic materials have different structures from fluoride, so that the coating performance is not good.
In the present invention, we studied at A2MF6:Mn4+(A is CsOr Rb; m is one of Si, Ge and Ti) luminescent crystal surface growth same A2MF6The method of the substrate crystal greatly improves the application prospect of the luminescence property of the fluoride crystal.
Disclosure of Invention
The invention aims to provide Mn4+Doped fluoride homogeneously wrapped luminescent crystals.
Another object of the present invention is to provide a method for preparing the above homogeneously wrapped luminescent crystal.
In order to achieve the above object, Mn according to the present invention4+A doped fluoride homogeneous-coated luminescent crystal, the chemical composition of which is: a. the2MF6@A2MF6:Mn4+；A2MF6:Mn4+Is an outer layer of matrix crystals, A2MF6:Mn4+Is an inner layer luminescent crystal; a is Cs or Rb, M is one of Si, Ge and Ti; x is the corresponding doping Mn4+Ion relative M4+Molar percentage coefficient of ion, 0<x is less than or equal to 0.10. The raw materials used by the invention are as follows: cesium fluoride or rubidium fluoride, potassium hexafluoro-manganate, silicon dioxide, germanium dioxide or titanium dioxide, hydrofluoric acid.
Mn as described above4+The preparation method of the doped fluoride homogeneous-coated luminescent crystal adopts a two-step liquid phase crystal growth method, and specifically comprises the following steps: firstly, adding silicon dioxide, germanium dioxide or titanium dioxide into hydrofluoric acid, vigorously stirring for 60-120 minutes, then adding cesium fluoride or rubidium fluoride, continuously stirring for 30-90 minutes to form clear and transparent matrix mother liquor, then adding potassium hexafluoromanganate, continuously stirring for 30-60 minutes, slowly volatilizing the obtained solution at normal temperature for 3-10 days, and washing the precipitated crystals with ethanol; secondly, placing the obtained luminescent crystal into fresh matrix mother liquor prepared in the first step, growing for 3-10 days at normal temperature again, and finally precipitating crystal, namely required Mn4+Doped fluoride homogeneously wrapped luminescent crystals.
The luminescent crystal coated with the same material of fluoride has high light transmittance and strong excitation in blue lightThe luminous band is luminous, and the luminous band shows strong red light emission and high luminous efficiency. The CIE value of the emission spectrum of the sample is close to the Standard value of red NTSC (national Television Standard Committee) ((R))x= 0.67,y= 0.33)。
Drawings
FIG. 1 shows Cs in example 12SiF6:Mn4+And Cs2SiF6@Cs2SiF6:Mn4+A photograph of the luminescent crystal under natural light;
FIG. 2 shows Cs in example 12SiF6@Cs2SiF6:Mn4+Room temperature excitation spectrum (monitoring wavelength is 630 nm) and emission spectrum (excitation wavelength is 460 nm) of luminescent crystal;
FIG. 3 shows Cs in example 12SiF6:Mn4+Luminescent crystal and commercial yellow phosphor Y3Al5O12:Ce3+A luminescence spectrum of the warm white LED device manufactured by the blue LED chip under the excitation of 20 mA current;
FIG. 4 is Rb for example 22GeF6:Mn4+And Rb2GeF6@Rb2GeF6:Mn4+A photograph of the luminescent crystal under natural light;
FIG. 5 is Rb for example 22GeF6@Rb2GeF6:Mn4+Room-temperature excitation spectrum (monitoring wavelength of 632 nm) and emission spectrum (excitation wavelength of 455 nm) of luminescent crystal;
FIG. 6 is Rb for example 22GeF6@Rb2GeF6:Mn4+Luminescent crystal and commercial yellow phosphor Y3Al5O12:Ce3+And the light-emitting spectrum of the warm white LED device manufactured by the blue LED chip under the excitation of 20 mA current.
Detailed Description
Example 1:
1.51g of silica is weighed into 40 ml of hydrofluoric acid and stirred vigorously for 60 minutes, then 9.12 g of cesium fluoride is added and stirring is continued for 30 minutes to form clear and transparent Cs2SiF6Adding 0.62 g of potassium hexafluoromanganate into the matrix mother liquor, continuing stirring for 30 minutes, slowly volatilizing the obtained solution at normal temperature for 9 days, and separating out Cs2SiF6:Mn4+Washing the crystal with ethanol; the luminescent crystals obtained are then placed in fresh Cs prepared as in the first step2SiF6Growing in the mother liquid at normal temperature for 9 days, and finally precipitating crystal, namely the required Mn4+Doped fluoride homogeneous-wrapped luminescent crystal Cs2SiF6@Cs2SiF6:Mn4+。
Shown in FIG. 1 is Cs2SiF6:Mn4+And Cs2SiF6@Cs2SiF6:Mn4+The photo of the luminescent crystal under natural light shows that the sample shows regular shape and has good light transmission performance.
FIG. 2 shows Cs2SiF6@Cs2SiF6:Mn4+Room temperature excitation spectrum (monitoring wavelength: 630 nm) and emission spectrum (excitation wavelength: 460 nm). The sample has a strong broadband absorption in the blue region around 460 nm and shows a series of red emission peaks, with the strongest emission peak at 630 nm. These red emission peaks correspond to Mn4+Is/are as follows2Eg-4A2gAnd (4) energy level transition. The spectrum CIE coordinate values are:x= 0.691,y= 0.309. Our sample CIE values are close to the Standard values of Red NTSC (national television Standard Committee) ((R))x= 0.67,y= 0.33)。
FIG. 3 shows Cs2SiF6@Cs2SiF6:Mn4+Luminescent crystal and commercial Y3Al5O12:Ce3+And the light-emitting device coated on the blue LED chip has a light-emitting spectrum under the excitation of 20 mA current. The color temperature of white light emitted by the white light device is 3243K, and the color rendering index reaches 89.
Example 2:
2.62 g of germanium dioxide is weighed and added into 40 ml of hydrofluoric acid to be stirred vigorously for 90 minutes, then 6.27 g of rubidium fluoride is added to be stirred continuously for 40 minutes to form clear and transparent Rb2GeF6Adding 0.62 g potassium hexafluoromanganate into the matrix mother liquor, continuously stirring for 30 minutes, slowly volatilizing the obtained solution at normal temperature for 6 days, and separating out Rb2GeF6:Mn4+Washing the crystal with ethanol; the luminescent crystals obtained are subsequently placed in fresh Rb as prepared in the first step2GeF6Growing in the mother liquid at normal temperature for 6 days, and finally precipitating crystal, namely the required Mn4+Doped fluoride homo-encapsulated luminescent crystals Rb2GeF6@Rb2GeF6:Mn4+。
Shown in FIG. 4 is Rb2GeF6:Mn4+And Rb2GeF6@Rb2GeF6:Mn4+The photos of the luminescent crystal under natural light show that the coated and uncoated crystals show regular shapes and have good light transmission performance.
FIG. 5 is Rb2GeF6@Rb2GeF6:Mn4+Room temperature excitation spectrum (monitoring wavelength of 632 nm) and emission spectrum (excitation wavelength of 455 nm). The sample has a strong broadband absorption in the blue region around 455 nm and exhibits a series of red emission peaks, the strongest of which is at 632 nm. These red emission peaks correspond to Mn4+Is/are as follows2Eg-4A2gAnd (4) energy level transition. The spectrum CIE coordinate values are:x= 0.692,y= 0.308. Our sample CIE values are close to the Standard values of Red NTSC (national television Standard Committee) ((R))x= 0.67,y= 0.33)。
FIG. 6 is Rb2GeF6@Rb2GeF6:Mn4+Luminescent crystal and commercial Y3Al5O12:Ce3+And the light-emitting device coated on the blue LED chip has a light-emitting spectrum under the excitation of 20 mA current. The color temperature of white light emitted by the white light device is 3545K, and the color rendering index reaches 86.
Example 3:
2.62 g of germanium dioxide is weighed into 40 ml of hydrofluoric acid and stirred vigorously for 90 minutes, then 9.12 g of cesium fluoride is added and stirring is continued for 30 minutes to formClear and transparent Cs2GeF6Adding 0.78 g of potassium hexafluoromanganate into the matrix mother liquor, continuously stirring for 60 minutes, slowly volatilizing the obtained solution at normal temperature for 6 days, and separating out Cs2GeF6:Mn4+Washing the crystal with ethanol; the luminescent crystals obtained are then placed in fresh Cs prepared as in the first step2GeF6Growing in the mother liquid at normal temperature for 6 days, and finally precipitating crystal, namely the required Mn4+Doped fluoride homogeneous-wrapped luminescent crystal Cs2GeF6@ Cs2GeF6:Mn4+。
Example 4:
2.01g of titanium dioxide is weighed into 40 ml of hydrofluoric acid and stirred vigorously for 60 minutes, then 9.12 g of cesium fluoride is added and stirring is continued for 30 minutes to form clear and transparent Cs2TiF6Adding 0.62 g of potassium hexafluoromanganate into the matrix mother liquor, continuing stirring for 30 minutes, slowly volatilizing the obtained solution at normal temperature for 9 days, and separating out Cs2TiF6Washing the crystal with ethanol; the luminescent crystals obtained are then placed in fresh Cs prepared as in the first step2TiF6Growing in the mother liquid at normal temperature for 9 days, and finally precipitating crystal, namely the required Mn4+Doped fluoride homogeneous-wrapped luminescent crystal Cs2TiF6@ Cs2TiF6:Mn4+。
Example 5:
2.01g of titanium dioxide is weighed and added into 40 ml of hydrofluoric acid to be stirred vigorously for 120 minutes, then 6.27 g of rubidium fluoride is added to be stirred continuously for 60 minutes to form clear and transparent Rb2TiF6Adding 0.78 g potassium hexafluoromanganate into the matrix mother liquor, continuously stirring for 60 minutes, slowly volatilizing the obtained solution at normal temperature for 3 days, and separating out Rb2TiF6Washing the crystal with ethanol; the luminescent crystals obtained are subsequently placed in fresh Rb as prepared in the first step2TiF6Growing in the mother liquid at normal temperature for 3 days, and finally precipitating crystal, namely the required Mn4+Doped fluoride homo-encapsulated luminescent crystals Rb2TiF6@ Rb2TiF6:Mn4+。
Example 6:
1.51g of silicon dioxide is weighed into 40 ml of hydrofluoric acid and stirred vigorously for 60 minutes, then 6.27 g of rubidium fluoride is added and stirring is continued for 60 minutes, so that clear and transparent Rb is formed2SiF6Adding 0.62 g potassium hexafluoromanganate into the matrix mother liquor, continuing stirring for 30 minutes, slowly volatilizing the obtained solution at normal temperature for 8 days, and separating out Rb2SiF6Washing the crystal with ethanol; the luminescent crystals obtained are subsequently placed in fresh Rb as prepared in the first step2SiF6Growing in the mother liquid at normal temperature for 8 days, and finally precipitating crystal, namely the required Mn4+Doped fluoride homo-encapsulated luminescent crystals Rb2SiF6@ Rb2SiF6:Mn4+。
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