CN101508894B - Alkaline earth metal borate fluorinate, preparation and uses thereof - Google Patents

Alkaline earth metal borate fluorinate, preparation and uses thereof Download PDF

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CN101508894B
CN101508894B CN200910010805A CN200910010805A CN101508894B CN 101508894 B CN101508894 B CN 101508894B CN 200910010805 A CN200910010805 A CN 200910010805A CN 200910010805 A CN200910010805 A CN 200910010805A CN 101508894 B CN101508894 B CN 101508894B
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earth metal
metal borate
alkaline earth
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fluorophor
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CN101508894A (en
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孙德春
王君
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    • C—CHEMISTRY; METALLURGY
    • 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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7709—Phosphates
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
    • C09K11/7485—Borates
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/778—Borates
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7797—Borates

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  • Inorganic Chemistry (AREA)
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Abstract

The invention relates to an alkaline-earth metal borate fluorophor and a preparation method and the application thereof, wherein a chemical expression formula of the fluorophor is M (1-x-y).B2O7:PbxRy, wherein, M is one element or the combination of a plurality of elements of Mg, Ca, Sr, Ba and Zn, and R is one element or the combination of a plurality of elements of Bi, Sc, Yt, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tu, Yb and Lu. The preparation method comprises the following steps: oxides or corresponding salts of the elements in the expression formula are fed according to mol ratio, added with 0.02-3 percent of fluxing agent according to the weight of the materials and burnt at the high temperature (500-1000 DEG C for 1-10 hours) after being evenly mixed, and the fluorophor material is obtained after post treatment. The alkaline-earth metal borate fluorophor emits UV-B spectrum and has the characteristics of high luminous efficiency, little light decay, good chemical stability, simple manufacturing method, low cost, and the like. A fluorescent lamp produced by the alkaline-earth metal borate fluorophor can be applied to human health protection and the field of livestock breeding.

Description

A kind of alkaline earth metal borate fluorinate
Technical field
The invention belongs to the phosphor technology field, relate to alkaline earth metal borate fluorinate, use this fluor and can prepare fluorescent-lamp-use in human body and animal health field.
Background technology
The still general lighting that adopts at lighting field is at present used lamp; Such as incandescent light, electricity-saving lamp, mercury lamp, sodium vapor lamp, Metal-halogen lamp etc.; These light emitted visible spectrums; Only possess illumination functions, in fact lighting source is except having illumination functions, to human and other animals have and important effect.The visible fluorescence body that is used to prepare lighting source is existing a lot, and the light fixture of wherein using UV-B section emmission spectrum phosphor preparation beneficial effect also has some reports.Like application number is that 96116266.X has used (Ca 0.94Zn 0.06) 3(PO 4) 2: Tl 0.16Fluor, well-known thallium is a highly toxic substance, so this fluor will bring immense pressure to environment in preparation and use, and this fluor light decay is bigger.ZL02246501.4 provides his Environmental protection lamp of a kind of dimension, and the opticglass inside pipe wall has fluor, can produce the healthy beta radiation of the UV-B that contains minimal erythema dose, and have high-color rendering.This invention used (Ca, Zn) 3-x(PO 4) 2.14: Gd xFluor, (Ca 0.94Zn 0.06) 3(PO 4) 2: Tl 0.16Fluor has very much progress, but still has the big problem of light decay, causes light fixture useful life to shorten, and brings high use cost.
Summary of the invention:
An object of the present invention is to provide a kind of alkaline earth metal borate fluorinate, this fluor has the quantum yield height, the characteristics that light decay is little; A kind of preparation method and application of alkaline earth metal borate fluorinate are provided simultaneously, particularly the preparation luminescent lamp.
The main chemical constitution of alkaline earth metal borate fluorescent material provided by the invention can be represented with chemical formula: M 1-x-yB 2O 7: Pb xR y, wherein: M is selected from Sr, Ca, Ba, Mg, one or more element combinations among the Zn; R is one or more element combinations that are selected from bismuth (Bi) scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), the lutetium (Lu); X, y are mole coefficient, 0.001≤x≤0.2,0.001≤y≤0.2.
The preparation method of above-mentioned alkaline earth metal borate fluorescent material provided by the invention may further comprise the steps:
(1) presses chemical formula M 1-x-yB 2O 7: Pb xR y, 0.001≤x≤0.2,0.01≤y≤0.2 wherein.Accurately take by weighing the oxide compound or the other forms of salt of each element in the said structure formula, take by weighing 0.02～3% fusing assistant and these component co-precipitation or solid phase mixing are even again.Described solubility promoter is NH 4HF 2, NH 4F, BaF 2, SrF 2, BaCl 2, SrCl 2, NH 4One or more combinations among the Cl.
(2) the above-mentioned raw material that mixes is packed in the crucible, place High Temperature Furnaces Heating Apparatus, sintering in air, temperature is 500～1000 ℃, sintering time is 1～10h.
(3) will burn till material and be crushed to and need particle diameter, and wash, sieve, dry, promptly get desired product.This fluor is at the ultraviolet ray excited emission down of 254nm UV-B section UV-light, and the emmission spectrum peak value is in 310 ± 5nm scope.
Because the 7-hydrogen SUV phototransformation in the skin of UV-B section ultraviolet luminous energy promotion humans and animals becomes vitamins D 3, promote metabolism to calcium phosphorus, thus effectively preventing rickets, osteomalacia and osteoporosis.And then help growing and improving immunizing power.Utilize fluor of the present invention to make luminescent lamp, not only can be used for illumination, also can be applicable to human health care and livestock and poultry cultivation field.
The outstanding feature that the present invention compared with prior art has: have characteristics such as luminous efficiency height, light decay is little, chemicalstability is good, and method of manufacture is simple, cost is low.
Description of drawings:
Fig. 1 is alkaline earth metal borate fluorinate emmission spectrum figure provided by the invention.
Fig. 2 is rare earth ion of the present invention and the ion-activated coactivated middle long wave UVF body (A) and single activator fluor (B) emmission spectrum power distribution comparison diagram of transition element.
Fig. 3 is rare earth ion of the present invention and the ion-activated coactivated middle long wave UVF body (A) and single activator fluor (B) emmission spectrum power distribution comparison diagram behind aging 1000h under the 185nm ultraviolet ray of transition element.
Fig. 4 is for using the emmission spectrum figure of this bright phosphor preparation luminescent lamp.
Embodiment:
Embodiment of the present invention is following:
The structural formula of fluor of the present invention is: M 1-x-yB 2O 7: Pb xR y, 0.001≤x≤0.2,0.001≤y≤0.2 wherein; Wherein M is selected from Sr, Ca; Ba; Mg; One or more element combinations among the Zn, wherein R is one or more element combinations that are selected from bismuth (Bi) scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), the lutetium (Lu).Accurately take by weighing the oxide compound of each element in the said structure formula or contain the salt of above-mentioned element, as: Strontium carbonate powder (SrCO 3), Natural manganese dioxide (MgO), lime carbonate (CaCO 3), barium carbonate (BaCO 3), zinc oxide (ZnO), gadolinium sesquioxide (Gd 2O 3), cerium oxide (CeO), plumbous oxide (PbO) etc., take by weighing the fusing assistant of raw material weight 0.02～3% again and these components mixed.Then the raw material of mixing is packed in the crucible, place High Temperature Furnaces Heating Apparatus, sintering in air, temperature is 500～1000 ℃, sintering time is 1～10h.Treat the High Temperature Furnaces Heating Apparatus cool to room temperature, will expect to take out to be crushed to needs particle diameter, deionized water wash, wetly sieves, promptly gets fluorescent material of the present invention in 100～120 ℃ of oven dry.
Described solubility promoter is NH 4HF 2, NH 4F, BaF 2, SrF 2, BaCl 2, SrCl 2, NH 4One or more combinations among the Cl.
Embodiment 1: the preparation of fluor.Raw materials used kind and proportioning:
SrCO 3：0.700mol
MgO：0.10mol
Gd 2O 3：0.10mol
CeO：0.05mol
PbO：0.02mol
B 2O 3：2.0mol
Preparing method: accurately take by weighing above-mentioned raw materials, take by weighing the SrF of 7.7g again 2As solubility promoter, and these components are mixed.Then the raw material of mixing is packed in the crucible, place High Temperature Furnaces Heating Apparatus, sintering temperature is 500～1000 ℃ in air, and sintering time is 1～10h.Treat the High Temperature Furnaces Heating Apparatus cool to room temperature, will expect to take out to be crushed to needs particle diameter, 80 ℃ of left and right sides deionized water wash, wetly sieves, promptly gets fluorescent material of the present invention in 100～120 ℃ of oven dry.This fluor is at the ultraviolet ray excited emission down of 254nm UV-B section UV-light, and the emmission spectrum peak value is in 310 ± 5nm scope.The emmission spectrum peak value of this fluor under 254nm is ultraviolet ray excited is as shown in Figure 1 at the excitation spectrum of 305nm.
Press the method for the foregoing description 1, carry out the preparation of the fluor of 2～20 embodiment, resulting fluor is formed and the spectral power data of contrast phosphate fluophor see the following form:
Sequence number Chemical constitution Relative spectral power distributes
Comparative Examples (Ca，Zn) 3-x(PO 4) 2.14:Gd x 35％
Example 2 Sr 0.76Mg 0.2·B 2O7:Pb 0.03Gd 0.005Ce 0.005 120％
Example 3 Sr 0.95·B 2O 7:Pb 0.04Gd 0.01 100％
Example 4 Sr 0.75Mg 0.2·B 2O 7:Pb 0.02Gd 0.01Ce 0.02 102％
Example 5 Sr 0.85Mg 0.1·B 2O 7:Pb 0.02Gd 0.02Ce 0.01 105％
Example 6 Sr 0.85Zn 0.1·B 2O 7:Pb 0.02Gd 0.02Ce 0.01 90％
Example 7 Sr 0.6Mg 0.2Ca 0.05Ba 0.05Zn 0.05·B 2O 7:Pb 0.01Ce 0.03Gd 0.01 88％
Example 8 Sr 0.85Mg 0.1·B 2O 7:Pb 0.02Bi 0.02Dy 0.01 96％
Example 9 Sr 0.85Mg 0.1·B 2O 7:Pb 0.02Bi 0.02Sc 0.01 95％
Example 10 Sr 0.85Mg 0.1·B 2O 7:Pb 0.02Y 0.02La 0.01 97％
Example 11 Nb 0.005Pm 0.005Sr 0.85Mg 0.1·B 2O 7:Pb 0.03Tm 0.001Lu 0.005Gd 0.014 90％
Example 12 Sr 0.85Mg 0.1·B 2O 7:Pb 0.04Sm 0.005Eu 0.005 80％
Example 13 Sr 0.85Mg 0.1·B 2O 7:Pb 0.04Tb 0.005Ho 0.005 81％
Example 14 Sr 0.85Mg 0.1·B 2O 7:Pb 0.04Er 0.005 Yb 0.005 80％
Example 15 Sr 0.85Mg 0.1·B 2O 7:Pb 0.02Pr 0.02 82％
Example 16 Sr 0.85Ca 0.1·B 2O 7:Pb 0.02Gd 0.01Bi 0.001Sc 0.001 81％
Example 17 Sr 0.85Mg 0.1·B 2O 7:Pb 0.02Gd 0.02Ce 0.01 84％
Example 18 Sr 0.6Ba 0.19·B 2O 7:Pb 0.009Gd 0.001Ce 0.2 60％
Example 19 Sr 0.6Mg 0.19·B 2O 7:Pb 0.001Gd 0.2Ce 0.009 58％
Example 20 Sr 0.6Mg 0.19·B 2O 7:Pb 0.2Gd 0.001Ce 0.009 55％
Prepared fluor is at the ultraviolet ray excited emission down of 254nm UV-B section UV-light, and the emmission spectrum peak value is in 310 ± 5nm scope.Utilize fluor of the present invention, process luminescent lamp according to conventional luminescent lamp manufacture craft, the healthy line of emission UV-B section is applied to illumination and human body and animal health field of light fittings.

Claims (5)

1. alkaline earth metal borate fluorinate is characterized in that chemical expression is:
M 1-x-y·B 2O 7:Pb x?R y，
Wherein: M is selected from Sr, Ca, Ba, Mg, one or more element combinations among the Zn; R is one or more element combinations in bismuth (Bi), scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), the lutetium (Lu); X, y are mole coefficient, 0.001≤x≤0.2,0.001≤y≤0.2.
2. alkaline earth metal borate fluorinate according to claim 1, it is characterized in that fluor at the emmission spectrum peak value under the 254nm ultraviolet excitation in 310 ± 5nm scope.
3. the preparation method of alkaline earth metal borate fluorinate as claimed in claim 1 is characterized in that concrete steps are:
(1) presses chemical formula M 1-x-yB 2O 7: Pb xR y, the molar ratio of 0.001≤x≤0.2,0.001≤y≤0.2 wherein accurately takes by weighing the oxide compound or its esters of each element in the said structure formula, takes by weighing the fusing assistant of raw material weight 0.02～3% and these components are even with co-precipitation or solid phase mixing again;
(2) the above-mentioned raw material that mixes is packed in the crucible, place the High Temperature Furnaces Heating Apparatus sintering, sintering temperature is 500～1000 ℃, and sintering time is 1～10h;
(3) will burn till material and be crushed to and need particle diameter, washing, drying, sieving promptly gets product.
4. the preparation method of alkaline earth metal borate fluorinate according to claim 3 is characterized in that described fusing assistant is NH 4HF 2, NH 4F, BaF 2, SrF 2, BaCl 2, SrCl 2, NH 4One or more element combinations among the Cl.
5. alkaline earth metal borate fluorinate as claimed in claim 1 is applied to illumination or human body and animal health luminescent lamp.
CN200910010805A 2009-03-20 2009-03-20 Alkaline earth metal borate fluorinate, preparation and uses thereof Expired - Fee Related CN101508894B (en)

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PCT/CN2009/072456 WO2010105456A1 (en) 2009-03-20 2009-06-26 Alkali earth metal borate fluorescent material and its preparation and its use

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CN101717635B (en) * 2009-12-10 2013-07-31 浙江工业大学 Red fluorescent powder for LED and preparation method thereof
CN102115667B (en) * 2009-12-30 2014-01-08 海洋王照明科技股份有限公司 Borate green luminescent material and preparation method thereof
CN102234508A (en) * 2010-04-20 2011-11-09 中国科学院上海硅酸盐研究所 Rare-earth-doped lutetium borate radiation detection material, and preparation and application thereof
CN102154693A (en) * 2011-03-29 2011-08-17 沈阳化工大学 Preparation method of rare earth cerium-doped boric acid potassium calcium optical crystal
CN102533262A (en) * 2011-12-16 2012-07-04 华南理工大学 Divalent-bismuth-ion-doped strontium borate fluorescent material and preparation method thereof
CN103215035A (en) * 2012-12-21 2013-07-24 彩虹集团电子股份有限公司 Europium excited strontium magnesium borate ultraviolet phosphor and preparation method thereof
CN105816962B (en) * 2016-06-03 2019-01-22 孙德春 A kind of diabetes curing instrument and its source material used
CN105907394B (en) * 2016-06-03 2019-01-15 孙德春 A kind of Adjust-blood lipid instrument and its source material used
CN106085418B (en) * 2016-06-03 2019-01-15 孙德春 A kind of gout treatment instrument and its source material used
CN106968016B (en) * 2017-03-10 2020-07-31 河南理工大学 Preparation, performance and application of green luminescent material terbium lead polyborate

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CN1362465A (en) * 2000-12-30 2002-08-07 大连路明发光科技股份有限公司 New type long-persistence material
US20080213152A1 (en) * 2007-03-01 2008-09-04 Osram Sylvania Inc. Method of Producing UV-Emitting Magnesium Pentaborate Phosphors

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CN1749353A (en) * 2005-11-01 2006-03-22 清华大学 Red and green fluorophor of borate and its preparing method

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CN1362465A (en) * 2000-12-30 2002-08-07 大连路明发光科技股份有限公司 New type long-persistence material
US20080213152A1 (en) * 2007-03-01 2008-09-04 Osram Sylvania Inc. Method of Producing UV-Emitting Magnesium Pentaborate Phosphors

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