CN108640505A - Europium adulterates the preparation method of fluorophosphate red fluorescence glass - Google Patents

Europium adulterates the preparation method of fluorophosphate red fluorescence glass Download PDF

Info

Publication number
CN108640505A
CN108640505A CN201810958444.4A CN201810958444A CN108640505A CN 108640505 A CN108640505 A CN 108640505A CN 201810958444 A CN201810958444 A CN 201810958444A CN 108640505 A CN108640505 A CN 108640505A
Authority
CN
China
Prior art keywords
glass
red fluorescence
fluorophosphate
europium
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810958444.4A
Other languages
Chinese (zh)
Inventor
李德胜
王波
林海
赵昕
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dalian Polytechnic University
Original Assignee
Dalian Polytechnic University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dalian Polytechnic University filed Critical Dalian Polytechnic University
Priority to CN201810958444.4A priority Critical patent/CN108640505A/en
Publication of CN108640505A publication Critical patent/CN108640505A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/12Silica-free oxide glass compositions
    • C03C3/23Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
    • C03C3/247Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron containing fluorine and phosphorus
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00Compositions for glass with special properties
    • C03C4/12Compositions for glass with special properties for luminescent glass; for fluorescent glass

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The present invention provides a kind of preparation method of the fluorophosphate red fluorescence glass of rare-earth europium doping, a kind of high efficiency red fluorescence is provided for plant growth lighting, the red fluorescence glass is prepared by metaphosphate and alkali metal fluoride and europium oxide, and the component of raw material is by 35~40mol%P2O5, 35~40mol%Na2O, 0~30mol%BaF2, 0~30mol%CaF2, 4wt%EuO compositions, preparation flow includes:Dispensing, grinding, removes water, shakes up, pour, and anneals.There is the fluorophosphate red fluorescence glass of the present invention good chemical stability and mechanical strength, efficient fluorescent emission to be suitable for the illumination of growth and development of plants.

Description

Europium adulterates the preparation method of fluorophosphate red fluorescence glass
Technical field
The present invention relates to a kind of red fluorescence glass, more specifically to a kind of red under ultraviolet and 395nm excitations The preparation method of color fluorescent glass.
Background technology
Just essential in plant growth and development process, plant accumulates nutrient by photosynthesis, but due to season Section property, at the cloudy day, plant can not obtain enough illumination to carry out photosynthesis.Thus to plant by the way of artificial light source It is the excellent means for promoting plant growth to carry out light filling.
The orange light of 600~780nm is that greenery carry out a kind of photosynthetic important band, to the shape of flower and blade There is prodigious effect at the development of, rhizome.Especially to germination, branches and leaves bifurcated, pigment synthesis, bar Stem nematode, bloom and The formation of enzyme etc. is especially important.Therefore a kind of excellent red fluorescence is provided for the growth of plant and its important.Europium of the present invention The fluorphosphate glass of doping can generate the feux rouges fluorescence of higher-strength under ultraviolet and 395nm excitation, can be applied to Growing process illuminates.
Invention content
The object of the present invention is to provide the preparation methods that a kind of europium adulterates fluorophosphate red fluorescence glass, make it have good Good glass forming ability, chemical stability and mechanical strength, lower nonlinear refractive index.
The present invention adopts the following technical scheme that:
A kind of fluorophosphate red fluorescence glass of europium doping, including glass matrix and europium oxide;Wherein, the glass base The group of matter becomes:35~40mol%P2O5, 35~40mol%Na2O, 0~30BaF2, 0~30mol%CaF2;The europium oxide Account for the 4wt% of glass matrix weight.
The preparation method of above-mentioned europium doping fluorophosphate fluorescent glass, includes the following steps:
Step S1, high-purity NaPO is selected3, BaF2, CaF2Glass matrix is introduced, the glass matrix group becomes:70~ 80mol%NaPO3, 0~30mol%BaF2, 0~30mol%CaF2, EuO is weighed by the 4wt% of the glass matrix weight, is ground Grind full and uniform, formation prepares the dispensing of glass;
Step S2, dispensing under 900~950 degrees Celsius is carried out to melting 50~70 minutes, during which shake up glass metal, prevent There is striped in the glass of formation, pour glass metal after homogenizing, annealing obtains fluorophosphate red fluorescence glass;
Wherein, in the step S2, the glass metal after homogenizing is poured on the aluminium sheet of 250~300 degrees Celsius of preheating, waits for glass It is put into 380~410 degrees Celsius of stove and anneals after glass molding, fluorophosphate red is made in the internal stress for eliminating inside glass Fluorescent glass;
After the step S2, further include:By fluorophosphate red fluorescence glass heat-insulating 8~10 hours, then stop protecting Temperature cools to room temperature with the furnace.
Advantages of the present invention:
The fluorophosphate red fluorescence glass of the present invention has good glass forming ability, chemical stability and machinery strong Degree, devitrification resistance can be excellent, have low nonlinear refractive index.Compared with existing fluorophosphate fluorophor, show compared with High rare earth dissolubility, this experiment content of rare earth are total mass fraction 4% still without concentration quenching under high doping.It is relatively strong to possess Fluorescent absorption and red emission ability.And t=102 DEG C of the Δ of glass in present case has good thermal stability.
Description of the drawings
Fig. 1 is the DTA curve of 1 europium of embodiment doping fluorophosphate red fluorescence glass.
Fig. 2 is the spectral radiation curves of 1 europium of embodiment doping fluorophosphate red fluorescence glass.
Specific implementation mode
A kind of fluorophosphate red fluorescence glass of europium doping, the molar constituent of raw material is 35~40mol%P2O5, 35~ 40mol%Na2O, 0~30mol%BaF2, 0~30mol%CaF2, 4wt%EuO.
The preparation that europium adulterates fluorophosphate fluorescent glass includes following link:
Dispensing:According to 70~80mol%NaPO of component3, 0~30mol%BaF2, 0~30mol%CaF2, 4wt%EuO claims Measure high-purity sodium metaphosphate, barium fluoride, calcirm-fluoride, europium oxide, and drug ground uniform, at powdered, formation prepares glass Dispensing.
Remove moisture removal:Load weighted dispensing is fitted into clean alumina crucible, is put into electric furnace and is melted, 300 30 minutes are kept the temperature under degree Celsius, removes moisture removal.
Melting:Above-mentioned batch is melted under 900~950 degrees Celsius, 50 minutes is kept the temperature, and rock crucible, makes Glass metal is uniform, prevents striped from generating.
It pours and anneals:Glass metal after homogenizing is poured on the aluminium sheet of 250 degrees Celsius of preheating, after glass molding at once It is put into 380~410 degrees Celsius of Muffle furnace and anneals, keep the temperature 8~10 hours, then stop heat preservation, cool to room with the furnace Fluorophosphate red fluorescence glass is made in temperature, the internal stress for eliminating inside glass.
Embodiment 1
The molar constituent of glass is 37.5mol%P2O5, 37.5mol%Na2O, 25%molBaF2, 4wt%EuO, according to It is prepared by following steps.
Dispensing:According to the molar constituent ratio of glass, high-purity sodium metaphosphate, barium fluoride, europium oxide are weighed, and drug is ground Mill is uniform.
Remove moisture removal:Load weighted dispensing is fitted into clean alumina crucible, is put into electric furnace and is melted, 300 30 minutes are kept the temperature under degree Celsius, removes moisture removal.
Melting:Above-mentioned batch is kept the temperature 50 minutes under 920 degrees Celsius, crucible is during which rocked twice, keeps glass metal equal It is even, prevent having striped appearance in the glass to be formed.
It pours and anneals:The glass metal melted is poured on the aluminium sheet of 250 degrees Celsius of preheating, after glass molding at once It is put into 390 degrees Celsius of Muffle furnace and anneals, eliminate the internal stress of inside glass.
Embodiment 2
The molar constituent of glass is 36mol%P2O5, 36mol%Na2O, 28mol%CaF2, 4wt%EuO, according to as follows It is prepared by step.
Dispensing:According to the molar constituent ratio of glass, high-purity sodium metaphosphate, calcirm-fluoride, europium oxide are weighed, and drug is ground Mill is uniform, in powdered.
Remove moisture removal:Load weighted dispensing is fitted into clean alumina crucible, is put into electric furnace and is melted, 300 30 minutes are kept the temperature under degree Celsius, removes moisture removal.
Melting:Above-mentioned batch is kept the temperature 60 minutes under 940 degrees Celsius, crucible is during which rocked twice, keeps glass metal equal It is even, prevent striped occur in the glass to be formed.
It pours and anneals:The glass metal melted is poured on the aluminium sheet of 250 degrees Celsius of preheating, after glass molding at once It is put into 400 degrees Celsius of Muffle furnace and anneals, eliminate the internal stress of inside glass.
Embodiment 3
The molar constituent of glass is 38mol%P2O5, 38mol%Na2O, 20mol%BaF2, 4mol%CaF2, 4wt% EuO is prepared in accordance with the following steps.
Dispensing:According to the molar constituent ratio of glass, high-purity sodium metaphosphate is weighed, barium fluoride, calcirm-fluoride, europium oxide, and Drug grinding is uniform, in powdered.
Remove moisture removal:Load weighted dispensing is fitted into clean alumina crucible, is put into electric furnace and is melted, 300 30 minutes are kept the temperature under degree Celsius, removes moisture removal.
Melting:Above-mentioned batch is kept the temperature 60 minutes under 940 degrees Celsius, and rocks crucible, keeps glass metal uniform, is eliminated Striped.
It pours and anneals:The glass metal melted is poured on the aluminium sheet of 250 degrees Celsius of preheating, after glass molding at once It is put into 400 degrees Celsius of Muffle furnace and anneals, eliminate the internal stress of inside glass.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Any one skilled in the art in the technical scope of present disclosure, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (6)

1. a kind of europium adulterates fluorophosphate red fluorescence glass, which is characterized in that including glass matrix and europium oxide;
Wherein, the group of the glass matrix becomes:35~40mol%P2O5, 35~40mol%Na2O, 0~30BaF2, 0~ 30mol%CaF2
The europium oxide accounts for the 4wt% of glass matrix weight.
2. europium adulterates fluorophosphate red fluorescence glass according to claim 1, which is characterized in that the group of the glass matrix As 37.5mol%P2O5, 37.5mol%Na2O, 25%molBaF2
3. a kind of preparation method of europium doping fluorophosphate red fluorescence glass, which is characterized in that include the following steps:
Step S1, NaPO is selected3、BaF2、CaF2Glass matrix is introduced, the glass matrix group becomes:70~80mol%NaPO3、 0~30mol%BaF2, 0~30mol%CaF2, EuO is weighed by the 4wt% of the glass matrix weight, grinds full and uniform, shape At the dispensing for preparing glass;
Step S2, dispensing is melted under 900~950 degrees Celsius, pours glass metal after homogenizing, annealing obtains fluorophosphoric acid Salt red fluorescence glass.
4. the preparation method of europium doping fluorophosphate red fluorescence glass according to claim 3, which is characterized in that the step In rapid S2, the glass metal after homogenizing is poured on the aluminium sheet of 250~300 degrees Celsius of preheating, it is put into 380 after glass molding~ It anneals in 410 degrees Celsius of stove, fluorophosphate red fluorescence glass is made in the internal stress for eliminating inside glass.
5. the preparation method of europium doping fluorophosphate red fluorescence glass according to claim 4, which is characterized in that the step After rapid S2, further include:By fluorophosphate red fluorescence glass heat-insulating 8~10 hours, then stops heat preservation, cool to room with the furnace Temperature.
6. adulterating the preparation method of fluorophosphate red fluorescence glass according to any europium of claim 3~5, feature exists In the group of the glass matrix becomes 37.5mol%P2O5, 37.5mol%Na2O, 25%molBaF2
CN201810958444.4A 2018-08-22 2018-08-22 Europium adulterates the preparation method of fluorophosphate red fluorescence glass Pending CN108640505A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810958444.4A CN108640505A (en) 2018-08-22 2018-08-22 Europium adulterates the preparation method of fluorophosphate red fluorescence glass

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810958444.4A CN108640505A (en) 2018-08-22 2018-08-22 Europium adulterates the preparation method of fluorophosphate red fluorescence glass

Publications (1)

Publication Number Publication Date
CN108640505A true CN108640505A (en) 2018-10-12

Family

ID=63761102

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810958444.4A Pending CN108640505A (en) 2018-08-22 2018-08-22 Europium adulterates the preparation method of fluorophosphate red fluorescence glass

Country Status (1)

Country Link
CN (1) CN108640505A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110416387A (en) * 2019-06-28 2019-11-05 苏州紫灿科技有限公司 A kind of high heat dissipation white light laser piece and preparation method
TWI740329B (en) * 2019-12-27 2021-09-21 鑫虹光電有限公司 Fluorescent glass composite material, fluorescent glass substrate including the same, and light conversion device

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3836375A (en) * 1972-04-06 1974-09-17 Leitz Ernst Gmbh TiO{11 {13 P{11 O{11 {13 Na{11 O{13 WO{11 {11 OPTICAL GLASSES AND METHOD
US3847624A (en) * 1972-06-26 1974-11-12 Leitz Ernst Gmbh Fluorophosphate optical glass
JPH07172864A (en) * 1993-12-14 1995-07-11 Nikon Corp Fluorinated phosphate based low dispersing optical glass
CN101024552A (en) * 2007-02-05 2007-08-29 中南大学 YB3+ dopped ion fluophosphate laser glass material containing high-valence cationic exide and its preparing method
CN102211867A (en) * 2011-04-15 2011-10-12 中国科学院上海光学精密机械研究所 Silver-europium co-doped base aluminophosphate glass and preparation method thereof
CN102604638A (en) * 2012-01-19 2012-07-25 苏州大学 Eu<3+>-activated phosphate red phosphor powder as well as preparation method and application thereof
CN103694999A (en) * 2014-01-07 2014-04-02 中国计量学院 Europium ion activated phosphate red fluorescent powder and preparation method thereof
RU2617662C1 (en) * 2015-12-03 2017-04-25 федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский национальный исследовательский университет информационных технологий, механики и оптики" (Университет ИТМО) Luminescent phosphate glass

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3836375A (en) * 1972-04-06 1974-09-17 Leitz Ernst Gmbh TiO{11 {13 P{11 O{11 {13 Na{11 O{13 WO{11 {11 OPTICAL GLASSES AND METHOD
US3847624A (en) * 1972-06-26 1974-11-12 Leitz Ernst Gmbh Fluorophosphate optical glass
JPH07172864A (en) * 1993-12-14 1995-07-11 Nikon Corp Fluorinated phosphate based low dispersing optical glass
CN101024552A (en) * 2007-02-05 2007-08-29 中南大学 YB3+ dopped ion fluophosphate laser glass material containing high-valence cationic exide and its preparing method
CN102211867A (en) * 2011-04-15 2011-10-12 中国科学院上海光学精密机械研究所 Silver-europium co-doped base aluminophosphate glass and preparation method thereof
CN102604638A (en) * 2012-01-19 2012-07-25 苏州大学 Eu<3+>-activated phosphate red phosphor powder as well as preparation method and application thereof
CN103694999A (en) * 2014-01-07 2014-04-02 中国计量学院 Europium ion activated phosphate red fluorescent powder and preparation method thereof
RU2617662C1 (en) * 2015-12-03 2017-04-25 федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский национальный исследовательский университет информационных технологий, механики и оптики" (Университет ИТМО) Luminescent phosphate glass

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
R VAN DEUN等: "Optical properties of Eu3+-doped fluorophosphates Glasses", 《JOURNAL OF PHYSICS:CONDENSED MATTER》 *
R. BALAKRISHNAIAH等: "Characterization of Eu3+-doped fluorophosphate glasses for red emission", 《JOURNAL OF NON-CRYSTALLINE SOLIDS》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110416387A (en) * 2019-06-28 2019-11-05 苏州紫灿科技有限公司 A kind of high heat dissipation white light laser piece and preparation method
TWI740329B (en) * 2019-12-27 2021-09-21 鑫虹光電有限公司 Fluorescent glass composite material, fluorescent glass substrate including the same, and light conversion device

Similar Documents

Publication Publication Date Title
CN110194593A (en) A method of full-inorganic perovskite quantum dot crystallization in glass is promoted by addition fluoride
CN108640505A (en) Europium adulterates the preparation method of fluorophosphate red fluorescence glass
CN105254181A (en) Europium-doped tungstate transparent glass ceramic and preparation method thereof
CN102211872A (en) 3 mu m luminous rare earth ion doped fluorophosphates laser glass and preparation method thereof
RU2579056C1 (en) Luminescent nano-glass-ceramic
CN102765883B (en) Preparation method of YAG microcrystalline glass
CN101265026B (en) Microcrystalline glass for precipitating La2O3 nano-crystalline and preparation method thereof
CN101723594A (en) Rare earth iron-doped transparent oxygen fluorine germanate microcrystalline glass and preparation method thereof
CN106927685B (en) It is a kind of with long-persistence luminous microcrystalline glass optical fiber and preparation method thereof
CN106186679A (en) Er ions mid-infrared luminescence fluorine chlorine phosphorus glass and preparation method thereof
CN115504672A (en) Infrared glass ceramic with chromium ions doped in various similar ways and preparation method thereof
CN108892375B (en) Silicon silicate glass and preparation method thereof
CN107586041B (en) Microcrystalline glass for dentistry and preparation method thereof
CN106927681B (en) A kind of gear division devitrified glass that lithium sodium potassium is co-doped with and its preparation and application
JPS63201034A (en) Production of crystallized glass having negative thermal expansion coefficient
CN102390932B (en) Transparent oxyfluoride tellurite glass ceramic of fluoride-containing nanocrystalline
JP2019532009A (en) Mycelite crystallized glass for artificial teeth and coloring method thereof
CN106430951B (en) A kind of tellurium oxide and antimony fluoride system matrix glass and preparation method thereof
CN108996904B (en) Eu and Pr ion co-doped barium silicate luminescent glass and preparation method thereof
CN108975714A (en) A kind of double-energy light-converting glass and preparation method thereof promoting photosynthesis of plant
CN106587635B (en) A kind of Ni2+:Cs2SiF6Devitrified glass and its preparation method and application
CN115504673B (en) CsPbBr 3 Quantum dot glass ceramic and preparation method thereof
CN110723907B (en) Europium-doped zinc molybdate-containing crystalline phase transparent glass ceramic and preparation method thereof
CN108998017A (en) One kind near-infrared long after glow luminous material of matrix containing silicon spinel and preparation method thereof
CN112062472B (en) High-hardness Lu2Si2O7Transparent microcrystalline glass and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20181012

RJ01 Rejection of invention patent application after publication