CN105385445A - Method for co-doping ions in yttrium tungstate base to obtain white light-emitting fluorescent powder - Google Patents
Method for co-doping ions in yttrium tungstate base to obtain white light-emitting fluorescent powder Download PDFInfo
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- CN105385445A CN105385445A CN201510727601.7A CN201510727601A CN105385445A CN 105385445 A CN105385445 A CN 105385445A CN 201510727601 A CN201510727601 A CN 201510727601A CN 105385445 A CN105385445 A CN 105385445A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—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
- C09K11/7794—Vanadates; Chromates; Molybdates; Tungstates
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Abstract
A method for co-doping ions in a yttrium tungstate base to obtain white light-emitting fluorescent powder includes the five steps that firstly, according to the mole ratio of the chemical formula of Y2-x-yWO6: xMn4+yEu3+, tungsten trioxide, yttrium oxide and europium oxide are respectively weighed and serve as raw materials; secondly, the raw materials are poured in an agate mortar, 1 mL of alcohol is dropwise added for helping grinding, and grinding is performed for 30 min; thirdly, the mixtures are poured into a 10 mL alumina crucible to be heated in a muffle furnace, heating is performed for raising the temperature to 1250 DEG C at the temperature raising speed of 3 DEG C/min, and constant-temperature sintering is performed for 5 h; fourthly, after the temperature is lowered below 200 DEG C, power supply of the muffle furnace stops, and the environment in the furnace is naturally cooled to room temperature; fifthly, calcined samples are taken out and placed in the agate mortar again and are ground into fine and small powder, then the samples are placed into a 200-mesh screen to be screened, and samples where different ions are doped with yttrium tungstate at different concentrations are obtained.
Description
Technical field
The invention provides a kind of in Yttrium Tungstate base co-dopant ions obtain the method for white luminous fluorescent material, it is the method for other elements of codoped in the europium doping Yttrium Tungstate material of emitting red light.The method can change the glow color of europium doping Yttrium Tungstate material, regulates and controls its color from ruddiness to white light.Belong to luminescent material technical field.
Background technology
Also environmental pollution has been there is, a series of significant problem such as energy shortage, ecological damage in 20th century mankind while economy and scientific and technological high speed development.Wherein, energy problem is the task of top priority of the mankind.According to statistics, in China, resident's electric consumption on lighting occupies about 13% of China's generating total amount.The novel illumination apparatus of exploitation energy-conserving and environment-protective is a great problems that the mankind need solution badly.White light-emitting diode, because its efficiency is high, the life-span is long, and response is fast, and safety, the advantages such as environmental protection, are described as after incandescent light, luminescent lamp and high-intensity gas discharge lamp, " forth generation lighting source ".Its core is fluorescent material wherein, so, find there is high conversion efficiency, a study hotspot that high color rendering index (CRI) and the new phosphors with a series of premium properties of safety non-toxic just become field of semiconductor illumination.
Tungstate is a kind of self activation material, and the participation namely not needing sensitizing agent or activator just can be luminous.Under near ultraviolet, X-ray and cathode-ray exciting, they can present efficient luminescence, wave band very wide in the luminous covering visible light region of intrinsic, and luminescent spectrum is stablized, and is well suited for the substrate material as fluorescent material.This seminar has utilized high temperature solid-state method to prepare monoclinic phase Yttrium Tungstate (Y
2wO
6) sample, find that it can launch yellow-green light under near ultraviolet excitation, its excitation spectrum has three absorption peaks, and respectively at 280nm, 310nm and 340nm, the charge transfer transition of light sources between W-O is Y
2wO
6intrinsic luminous.
Doping refers to introduces external impurity in matrix, has a wide range of applications in illumination field.By the different element that adulterates in the substrate, relative to unadulterated phase pure material, we can improve a lot of character of luminescent material, and such as, the glow color of controlled material, improves its luminous intensity etc.Europium element (Eu) is a kind of doped element that semiconductor light emitting field is commonly used, and exists, in a lot of matrix, can obtain new emission peak in a lot of matrix as the form of activator.In Yttrium Tungstate matrix, europium (Eu) also act as the role of activator, and the Yttrium Tungstate being doped with europium ion shows typical emitting red light, is a kind of up-and-coming red fluorescence powder.The present invention is by the sample of europium doping, and codoped enters mn ion, and mn ion is not luminous wherein, as sensitizing agent, improve the ratio of the short-and-medium wavelength emission of sample in entirety is launched, make sample blue shift, thus it is white luminous that sample is converted to from emitting red light.The present invention has widened and obtained white luminous method in Yttrium Tungstate base, is of great importance for instructing the research and development of novel white fluorescent powder.
Summary of the invention
1, the object of the present invention is to provide a kind of in Yttrium Tungstate base co-dopant ions obtain the method for white luminous fluorescent material.This method is easy, feasible, and it significantly can change the color of the luminescence of Yttrium Tungstate material, obtains the sample of transmitting white.
2, technical solution of the present invention: by mn ion (Mn
4+) and europium ion (Eu
3+) codoped enters in Yttrium Tungstate substrate, regulates and controls europium-ion-doped (Eu
3+) glow color of Yttrium Tungstate red fluorescence powder, obtain white luminous fluorescent material.Concrete steps are as follows:
Step one: according to meeting chemical formula: Y
2-x-ywO6:xMn
4+yEu
3+mol ratio take tungstic oxide (WO respectively
3, analytical pure, purity is 99.9%), yttrium oxide (Y
2o
3, analytical pure, purity is 99.9%), manganese oxide (MnO
2, analytical pure, purity 97.5%) and europium sesquioxide (Eu
2o
3, analytical pure, purity 99.9%) and as raw material.
Step 2: the above-mentioned raw material weighed up is put into agate mortar, and instill 1mL alcohol help grinding, grind 30 minutes, ensure the full and uniform mixing of sample.
Step 3: above-mentioned uniform mixture is poured in the alumina crucible of 10mL, and put it in retort furnace and heat in air atmosphere, the temperature program(me) of heating is be heated to 1250 DEG C with the temperature rise rate of about 3 DEG C/min from room temperature, Isothermal sinter 5 hours at this temperature.
Step 4: stop retort furnace powering after being cooled to less than 200 DEG C, after annealing, allow material naturally cool to room temperature in stove.
Step 5: the sample of taking-up after calcining is placed in agate mortar again, grinding makes it become fine powder shape, then sample is put in 200 object sieves carries out process of sieving, and can obtain different ions and to adulterate under different concns the sample of Yttrium Tungstate.
3, advantage of the present invention is: by simply at europium doped ion (Eu
3+) Yttrium Tungstate substrate in codoped enter mn ion (Mn
4+), its glow color is regulated to white light from redness, makes it obtain in LEDphosphor for LED illumination and apply widely.
Accompanying drawing explanation
Fig. 1: the emmission spectrum schematic diagram of europium doping Yttrium Tungstate material.
Fig. 2: europium, manganese mix the emmission spectrum schematic diagram of Yttrium Tungstate material altogether.
Fig. 3: the chromaticity coordinates figure of codoped Yttrium Tungstate material.
Fig. 4: be FB(flow block) of the present invention.
Embodiment
Below in conjunction with embodiment and Fig. 1-Fig. 4, the present invention is described in detail, but protection scope of the present invention is not limited in the following example, should comprise the full content in application for patent.
Embodiment 1
Step one: take 0.46368g tungstic oxide, 0.44258g yttrium oxide, 0.0070g manganese oxide and 0.00323g europium sesquioxide respectively as raw material according to the mol ratio meeting chemical formula 0.02Mn0.02Eu:Y2WO6.
Step 2: the above-mentioned raw material weighed up is put into agate mortar, and instill 1mL essence help grinding, grind 30 minutes, ensure the full and uniform mixing of sample.
Step 3: above-mentioned uniform mixture is poured in the alumina crucible of 10mL, and put it in retort furnace and heat in air atmosphere, the temperature program(me) of heating is be heated to 1250 DEG C with the temperature rise rate of about 3 DEG C/min from room temperature, Isothermal sinter 5 hours at this temperature.
Step 4: stop retort furnace powering after being cooled to less than 200 DEG C, after annealing, allow material naturally cool to room temperature in stove.
Step 5: the sample of taking-up after calcining is placed in agate mortar again, grinding makes it become fine powder shape, then sample is put in 200 object sieves carries out process of sieving, and can obtain different ions and to adulterate under different concns the sample of Yttrium Tungstate.
Embodiment 2
Step one: take 0.46368g tungstic oxide, 0.43807g yttrium oxide, 0.00350g Manganse Dioxide and 0.00323g europium sesquioxide respectively as raw material according to the mol ratio meeting chemical formula 0.01Mn0.02Eu:Y2WO6.
Step 2: the above-mentioned raw material weighed up is put into agate mortar, and instill 1mL alcohol help grinding, grind 30 minutes, ensure the full and uniform mixing of sample.
Step 3: above-mentioned uniform mixture is poured in the alumina crucible of 10mL, and put it in retort furnace and heat in air atmosphere, the temperature program(me) of heating is be heated to 1250 DEG C with the temperature rise rate of about 3 DEG C/min from room temperature, Isothermal sinter 5 hours at this temperature.
Step 4: stop retort furnace powering after being cooled to less than 200 DEG C, after annealing, allow material naturally cool to room temperature in stove.
Step 5: the sample of taking-up after calcining is placed in agate mortar again, grinding makes it become fine powder shape, then sample is put in 200 object sieves carries out process of sieving, and can obtain different ions and to adulterate under different concns the sample of Yttrium Tungstate.
Claims (1)
1. in Yttrium Tungstate base, co-dopant ions obtains a method for white luminous fluorescent material, it is characterized in that: the method concrete steps are as follows:
Step one: according to meeting chemical formula: Y
2-x-ywO6:xMn
4+yEu
3+mol ratio take tungstic oxide WO respectively
3analytical pure, purity are 99.9%, yttrium oxide Y
2o
3analytical pure, purity are 99.9%, manganese oxide MnO
2analytical pure, purity 97.5% and europium sesquioxide Eu
2o
3analytical pure, purity 99.9% are as raw material;
Step 2: the above-mentioned raw material weighed up is put into agate mortar, and instill 1mL alcohol help grinding, grind 30 minutes, ensure the full and uniform mixing of sample;
Step 3: above-mentioned uniform mixture is poured in the alumina crucible of 10mL, and put it in retort furnace and heat in air atmosphere, the temperature program(me) of heating is be heated to 1250 DEG C with the temperature rise rate of 3 DEG C/min from room temperature, Isothermal sinter 5 hours at this temperature;
Step 4: stop retort furnace powering after being cooled to less than 200 DEG C, after annealing, allow material naturally cool to room temperature in stove;
Step 5: the sample of taking-up after calcining is placed in agate mortar again, grinding makes it become fine powder shape, then sample is put in 200 object sieves carries out process of sieving, and namely obtains different ions and to adulterate under different concns the sample of Yttrium Tungstate.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1539914A (en) * | 2003-10-23 | 2004-10-27 | 北京有色金属研究总院 | Red luminescent powder in use for LED, preparing method and electric light source produced |
| CN1214471C (en) * | 2000-07-28 | 2005-08-10 | 电灯专利信托有限公司 | Illumination device with at least one LED as light source |
| CN1858150A (en) * | 2006-06-09 | 2006-11-08 | 中国科学院上海硅酸盐研究所 | X-ray excited rare-earth ion blended tungstate flash luminous material and its preparing method |
| CN1938870A (en) * | 2004-03-10 | 2007-03-28 | 吉尔科有限公司 | Phosphor and blends thereof for use in LED |
| CN101157853A (en) * | 2007-11-12 | 2008-04-09 | 中国科学院长春光学精密机械与物理研究所 | Near ultraviolet or blue-light excited red fluorescence powder and preparation method thereof |
| CN101255337A (en) * | 2008-03-13 | 2008-09-03 | 同济大学 | Preparation method of red-light fluorescent powder for LED or PDP display |
| CN102417815A (en) * | 2011-09-01 | 2012-04-18 | 上海师范大学 | Rare earth tungstate phosphor matrix, its preparation method and application |
| CN104085928A (en) * | 2014-07-17 | 2014-10-08 | 中国科学院上海硅酸盐研究所 | Rare-earth-ion-doped tungstate flicker film and preparation method thereof |
| CN104194786A (en) * | 2014-07-29 | 2014-12-10 | 北京航空航天大学 | Method for improving luminous performance of yttrium tungstate material by doping ions |
-
2015
- 2015-10-30 CN CN201510727601.7A patent/CN105385445B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1214471C (en) * | 2000-07-28 | 2005-08-10 | 电灯专利信托有限公司 | Illumination device with at least one LED as light source |
| CN1539914A (en) * | 2003-10-23 | 2004-10-27 | 北京有色金属研究总院 | Red luminescent powder in use for LED, preparing method and electric light source produced |
| CN1938870A (en) * | 2004-03-10 | 2007-03-28 | 吉尔科有限公司 | Phosphor and blends thereof for use in LED |
| CN1858150A (en) * | 2006-06-09 | 2006-11-08 | 中国科学院上海硅酸盐研究所 | X-ray excited rare-earth ion blended tungstate flash luminous material and its preparing method |
| CN101157853A (en) * | 2007-11-12 | 2008-04-09 | 中国科学院长春光学精密机械与物理研究所 | Near ultraviolet or blue-light excited red fluorescence powder and preparation method thereof |
| CN101255337A (en) * | 2008-03-13 | 2008-09-03 | 同济大学 | Preparation method of red-light fluorescent powder for LED or PDP display |
| CN102417815A (en) * | 2011-09-01 | 2012-04-18 | 上海师范大学 | Rare earth tungstate phosphor matrix, its preparation method and application |
| CN104085928A (en) * | 2014-07-17 | 2014-10-08 | 中国科学院上海硅酸盐研究所 | Rare-earth-ion-doped tungstate flicker film and preparation method thereof |
| CN104194786A (en) * | 2014-07-29 | 2014-12-10 | 北京航空航天大学 | Method for improving luminous performance of yttrium tungstate material by doping ions |
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