CN105567233A - Preparation method of fluorescent powder for optical fiber temperature sensor - Google Patents
Preparation method of fluorescent powder for optical fiber temperature sensor Download PDFInfo
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- CN105567233A CN105567233A CN201610029892.7A CN201610029892A CN105567233A CN 105567233 A CN105567233 A CN 105567233A CN 201610029892 A CN201610029892 A CN 201610029892A CN 105567233 A CN105567233 A CN 105567233A
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- temperature sensor
- fluorescent material
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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
- C09K11/7783—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
- C09K11/7784—Chalcogenides
- C09K11/7787—Oxides
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention belongs to the technical field of transformer fluorescence fiber temperature measurement, and particularly relates to a preparation method of fluorescent powder for an optical fiber temperature sensor. The preparation method comprises the steps that 1, Eu2O3, Yb2O3 and Y2O3 are dissolved in concentrated nitric acid to prepare a solution; 2, the pH value of the solution is regulated to be slightly acidic; 3, the solution is dried and then calcined; 4, a product obtained in the step 3 is ground and then calcined again; 5 the product is naturally cooled to be at room temperature and ground to obtain the fluorescent powder. The prepared fluorescent powder is uniform in particle size and dispersion, regular in particle shape, good in particle uniformity, high in fluorescence conversion efficiency and temperature measurement precision and wide in temperature measurement range.
Description
Technical field
The invention belongs to transformer fluorescence fiber temperature measurement technical field, be specifically related to a kind of preparation method of fibre optic temperature sensor fluorescent material.
Background technology
Fibre optic temperature sensor is high with its precision, sensing scope is wide, not by advantages such as electromagnetic interference, be widely used in the fields such as intelligent grid, biologic medical, petrochemical complex, industrial microwave, power management and military and national defense.The fluorescent optical fiber temperature sensor utilizing pure optical principle to carry out measuring has the incomparable advantage of traditional sensing technology and receives increasing concern.Although some fluorescent optical fiber temperature sensor realize small serial production on market, along with the continuous expansion of Application Areas, the fluorescent material of superior performance is faced with new opportunities and challenges.
The life-span of transformer winding temperature to the aging of insulating material and transformer of power domain plays a decisive role, and Measurement accuracy transformer winding temperature is considered all to seem particularly important from security and economy.At present, business-like most of manufacturer does not also work out the fluorescent material of this field for fluorescent optical fiber temperature sensor, and the main impact by phosphor material powder performance, exists the problem that temperature-measuring range is narrow, temperature measurement accuracy is low; In addition, the granularity of fluorescent material and each distribution of material inequality result also in the poor problem of thermometric consistence.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of fibre optic temperature sensor fluorescent material, and the fluorescent material that the method prepares can improve the temperature-measuring range of fibre optic temperature sensor, temperature measurement accuracy and thermometric consistence.
Technical solution of the present invention is: the preparation method of the fibre optic temperature sensor fluorescent material provided comprises the following steps:
1] by Eu
2o
3, Yb
2o
3and Y
2o
3be dissolved in concentrated nitric acid, be mixed with solution;
2] regulate the potential of hydrogen of described solution to slightly acidic;
3] calcine after described solution being dried;
4] by step 3] products therefrom grinding after again calcine;
5] naturally cool to room temperature, grinding obtains fluorescent powder product.
Beneficial effect of the present invention is: the present invention first prepares mixture by the precipitator method, low temperature calcination is carried out after grinding, carry out regrind after calcining, and then carry out high temperature secondary calcining, finally obtain fluorescent material through high pressure abrasive, the fluorescent material powder globule size prepared evenly, be uniformly dispersed, particle shape rule, particle identity is good, and fluorescence conversion efficiency is high, temperature measurement accuracy is high, and temperature-measuring range is wide.
Embodiment
Preparation method of the present invention comprises the following steps:
(1) Eu
2o
3, Yb
2o
3and Y
2o
3proportionally be dissolved in concentrated nitric acid, be mixed with solution, in solution.
(2) add citric acid, ammoniacal liquor is adjusted to the neutral meta-acid (pH value 5.5-6.5) of solution pH value.
(3) solution carries out calcined crystalline after drying in an oven and becomes single-phase powder.
(4) grinding after calcining, again calcines after grinding,
(5) fluorescent material is obtained through grinding after cooling.
In step (1), the atomic fraction ratio of each element is: Eu≤30%, Yb≤50%, Y
2≤ 40%.In step (2), the pH value of solution is 5.5-6.5.Calcining temperature in step (3) is 650-900 DEG C.Calcining temperature in step (4) is 1200-1650 DEG C.Grinding condition in step (4) and step (5) is: grinding in 5-10Mpa, 3-8 minute.
Embodiment one: element ratio is Eu:Yb:Y
2=25% ︰ 40% ︰ 35%; Solution pH value is 6.4; One time calcining temperature is 850 DEG C; Secondary clacining temperature is 1550 DEG C; Grinding condition is 7.5Mpa, grinding in 6 minutes.Can reach temperature measurement accuracy within the scope of-50 DEG C ~ 400 DEG C through the fluorescent material of which process can reach ± 1 DEG C.
Embodiment two: element ratio is Eu:Yb:Y
2=20% ︰ 45% ︰ 35%; Solution pH value is 6; One time calcining temperature is 750 DEG C; Secondary clacining temperature is 1650 DEG C; Grinding condition is 6.5Mpa, grinding in 4 minutes.Can reach temperature measurement accuracy within the scope of-50 DEG C ~ 250 DEG C through the fluorescent material of which process can reach ± 0.5 DEG C.
Claims (6)
1. a preparation method for fibre optic temperature sensor fluorescent material, is characterized in that: comprise the following steps:
1] by Eu
2o
3, Yb
2o
3and Y
2o
3be dissolved in concentrated nitric acid, be mixed with solution;
2] regulate the potential of hydrogen of described solution to slightly acidic;
3] calcine after described solution being dried;
4] by step 3] products therefrom grinding after again calcine;
5] naturally cool to room temperature, grinding obtains fluorescent powder product.
2. the preparation method of fibre optic temperature sensor fluorescent material according to claim 1, is characterized in that: described step 1] in the molar mass proportionlity of three kinds of elements be: Eu≤30%, Yb≤50%, Y≤40%.
3. the preparation method of fibre optic temperature sensor fluorescent material according to claim 1 and 2, is characterized in that: described step 2] potential of hydrogen to the pH value that uses citric acid and ammoniacal liquor regulator solution is 5.5-6.5.
4. the preparation method of fibre optic temperature sensor fluorescent material according to claim 3, is characterized in that: described step 3] in calcining temperature be 650-900 DEG C, calcination time is 0.5-2 hour.
5. the preparation method of fibre optic temperature sensor fluorescent material according to claim 4, is characterized in that: described step 4] in calcining temperature be 1200-1650 DEG C, calcination time is 0.5-2 hour.
6. the preparation method of fibre optic temperature sensor fluorescent material according to claim 5, is characterized in that: described step 4] and step 5] in grinding condition be: grinding pressure 5-10Mpa, milling time 3-8 minute.
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CN201610029892.7A CN105567233A (en) | 2016-01-15 | 2016-01-15 | Preparation method of fluorescent powder for optical fiber temperature sensor |
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CN201610029892.7A CN105567233A (en) | 2016-01-15 | 2016-01-15 | Preparation method of fluorescent powder for optical fiber temperature sensor |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108976869A (en) * | 2018-08-10 | 2018-12-11 | 安徽信达家居有限公司 | A kind of environmentally friendly luminescent coating suitable for wood finishing |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101838534A (en) * | 2010-06-23 | 2010-09-22 | 哈尔滨工业大学 | Preparation method of single-green up-conversion fluorescent marking material |
-
2016
- 2016-01-15 CN CN201610029892.7A patent/CN105567233A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101838534A (en) * | 2010-06-23 | 2010-09-22 | 哈尔滨工业大学 | Preparation method of single-green up-conversion fluorescent marking material |
Non-Patent Citations (2)
Title |
---|
X. WEI ET AL.,: ""Cooperative energy transfer in Eu3+, Yb3+ codoped Y2O3 phosphor"", 《JOURNAL OF RARE EARTHS》 * |
徐国刚等,: ""沉淀法制备纳米Eu:Y2O3荧光粉"", 《稀有金属材料与工程》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108976869A (en) * | 2018-08-10 | 2018-12-11 | 安徽信达家居有限公司 | A kind of environmentally friendly luminescent coating suitable for wood finishing |
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Application publication date: 20160511 |
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