CN100556586C - A kind of preparation method of yttrium borate doped nano powder - Google Patents
A kind of preparation method of yttrium borate doped nano powder Download PDFInfo
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- CN100556586C CN100556586C CNB200410092065XA CN200410092065A CN100556586C CN 100556586 C CN100556586 C CN 100556586C CN B200410092065X A CNB200410092065X A CN B200410092065XA CN 200410092065 A CN200410092065 A CN 200410092065A CN 100556586 C CN100556586 C CN 100556586C
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Abstract
A kind of preparation method of yttrium borate doped nano powder belongs to field of fine chemical.Principal character of the present invention is with yttrium, and the aqueous solution of doping with rare-earth ions and boron ion is raw material, is precipitating reagent with the organic base, the precipitation presoma after filtration, drying, calcining between 600-800 ℃, can obtain average grain diameter is the nothing reunion of 50 nanometers, highly purified yttrium borate doped powder.This method outstanding feature is: be raw material with inorganic salts, needn't add surfactant, can make high-quality yttrium borate doped nano powder, technology is simple simultaneously, and production cost is low, is suitable for suitability for industrialized production.
Description
Technical field
The invention belongs to field of fine chemical, especially relate to the preparation method of yttrium borate doped nano powder.
Technical background
Yttrium borate doped (Re:YBO
3, Re can be Eu
3+Deng rare earth ion) be a kind of widely used functional material, as europium-doped yttrium borate (Eu:YBO
3) be a kind of ruddiness fluorescer that is used for plasma panel (PDP).The plasma screen technology is compared with other display mode, aspect structure and composition in the lead.Independently phosphor pixel is luminous comprehensively forms by each for its image, seems bright-coloured, bright, clear; Another characteristics are to accomplish ultra-thinly, can accomplish the plane giant-screen more than 40 inches, and thickness are less than 100 millimeters.In recent years, along with people are more and more higher to the requirement of audio-visual products, PDP display is developed rapidly with the thin external form of its outstanding picture quality peace, has very big market development potentiality.The critical material of PDP display is high-quality fluorescent material, and it requires powder purity height, uniform doping, lattice perfection, like this light-emitting phosphor efficient height, stability is high, color saturation is good.Simultaneously, in order to obtain higher resolution ratio and the brightness of Geng Gao, need the small fluorescer particle of particle diameter, it also brings higher packed density and advantage such as low adhesive consumption more.Therefore prepare doping YBO
3Nano-powder has great economy and is worth and wide market prospects.
The YBO of preparation doping at present
3Mainly contain solid reaction process, the precipitation method, microwave heating method, sol-gel process etc.The solid reaction process temperature height that responds, doping weak effect, shortcoming such as crystal grain is easily reunited in the powder, and particle is big.Microwave heating method is heated evenly, and firing rate is fast, but equipment is had relatively high expectations.Its reactive component of sol-gel process mixes, the product purity height, and synthesis temperature is low, but cost is higher, and the cycle is long.The precipitation method are a kind of nano powder preparation methods that possess the large-scale production ability, and its advantage is that technology is simple, and it is direct, efficient to mix, the reaction condition gentleness.Inorganic bases such as general employing ammoniacal liquor are made precipitating reagent.Do not see the report that adopts organic base to prepare yttrium borate doped nano powder as precipitating reagent.
Summary of the invention
The object of the invention provide a kind of reunion less, the purity height, be suitable for the yttrium borate doped (YBO of suitability for industrialized production
3) method of nano-powder.The present invention is precipitating reagent with the organic base, and reaction precipitation method prepares doping YBO
3Nano-powder.
The technical scheme that realizes the object of the invention is:
1, the selection of inorganic salts: yttrium and doping with rare-earth ions are selected nitrate aqueous solution for use, and the boron ion is selected boric acid aqueous solution for use, and yttrium, concentration rare earth doped and the boron ion are 5.0-0.05mol/L.
2, precipitation process: precipitation process should fully stir, and all homogeneous precipitation is complete to guarantee all ions.This method precipitating reagent adopts organic base solution, and as triethanolamine, triethylamine, diethylamine etc., its concentration is 5.0-0.05mol/L.
3, Chen Dian suction filtration: earlier with the distilled water washing, use organic solvent washing again, in the suction filtration process in order to remove the organic base of inorganic ions and absorption.
4, drying: in a conventional oven between 100-120 ℃ dry 2-6 hour, in order to remove the moisture and the organic solvent of the absorption of precipitation presoma.
5, calcining: calcining is that heat treatment temperature is low excessively, YBO for a precipitation presoma is transformed into oxide
3Change mutually not exclusively, produce dephasign, heat treatment temperature is too high, the YAB grain growth, and it is big that diameter of particle becomes, so heat treatment temperature is controlled at 600-800 ℃, and the time was controlled at 2-6 hour.
6, use method provided by the invention, the average grain diameter of the yttrium borate doped nano powder of preparation is the 50-100 nanometer.Powder x-ray diffraction the analysis showed that all characteristic peaks of europium-doped yttrium borate powder are the YAB phase, other impurity peaks do not occur; Transmission electron microscopy the analysis showed that the average grain diameter of same europium-doped yttrium borate powder is 50 nanometers, narrow diameter distribution, and particle agglomeration is few; The EDS energy spectrum analysis shows the Y of same europium-doped yttrium borate nano-powder: the Eu mol ratio is about 9: 1.
Compared with prior art, advantage of the present invention is: preparation technology is simple, and equipment requires low, easily realizes large-scale production; Compare with solid reaction process, yttrium borate doped diameter of particle reaches nanoscale, and synthesis temperature is low, and manufacturing cycle is short; The purity height of powder, it is few to reunite, narrow diameter distribution; Mix mutually between corresponding solion, for the molecular level level is mixed.
Specific embodiments
Example 1:
Y (NO
3)
3, Eu (NO
3)
3And H
3BO
3Be dissolved in the distilled water respectively, the concentration of yttrium, europium and boron ion is respectively 0.5mol/L, 1.0mol/L and 1.0mol/L, is these three kinds of solution mixing in 0.8: 0.2: 1 in molar ratio, under the vigorous stirring, drip an amount of triethanolamine solution (triethanolamine: water=1: 1), obtain white gelatinous precipitate, distillation washing 2 times, absolute ethyl alcohol is washed 2 times, 100 ℃ of dryings 6 hours, grinding is sieved, and is placed in the high temperature furnace 800 ℃ of calcinings 2 hours then, and obtaining highly purified average grain diameter is the europium-doped yttrium borate powder of 80 nanometers.
Example 2:
Y (NO
3)
3, Eu (NO
3)
3And H
3BO
3Be dissolved in the distilled water respectively, the concentration of yttrium, europium and boron ion is respectively 0.05mol/L, 5.0mol/L and 5.0mol/L, is these three kinds of solution mixing in 0.9: 0.1: 1 in molar ratio, under the vigorous stirring, drip an amount of triethanolamine solution (triethanolamine: water=1: 1), obtain white gelatinous precipitate, distillation washing 2 times, absolute ethyl alcohol is washed 2 times, 120 ℃ of dryings 2 hours, grinding is sieved, and is placed in the high temperature furnace 600 ℃ of calcinings 2 hours then, and obtaining highly purified average grain diameter is the europium-doped yttrium borate powder of 100 nanometers.
Example 3:
Y (NO
3)
3, Eu (NO
3)
3And H
3BO
3Be dissolved in the distilled water respectively, the concentration of yttrium, europium and boron ion is respectively 0.5mol/L, 1.0mol/L and 1.0mol/L, is these three kinds of solution mixing in 0.9: 0.1: 1 in molar ratio, under the vigorous stirring, drip an amount of triethylamine solution (triethylamine: ethanol=1: 1), obtain white gelatinous precipitate, distillation washing 2 times, absolute ethyl alcohol is washed 2 times, 110 ℃ of dryings 4 hours, grinding is sieved, and is placed in the high temperature furnace 700 ℃ of calcinings 4 hours then, and obtaining highly purified average grain diameter is the europium-doped yttrium borate powder of 50 nanometers.
Example 4:
Y (NO
3)
3, Eu (NO
3)
3And H
3BO
3Be dissolved in the distilled water respectively, the concentration of yttrium, europium and boron ion is respectively 0.5mol/L, 5.0mol/L and 1.0mol/L, is these three kinds of solution mixing in 0.8: 0.2: 1 in molar ratio, under the vigorous stirring, drip an amount of triethylamine solution (triethylamine: ethanol=1: 1), obtain white gelatinous precipitate, distillation washing 2 times, absolute ethyl alcohol is washed 2 times, 100 ℃ of dryings 4 hours, grinding is sieved, and is placed in the high temperature furnace 800 ℃ of calcinings 3 hours then, and obtaining highly purified average grain diameter is the europium-doped yttrium borate powder of 70 nanometers.
Example 5:
Y (NO
3)
3, Eu (NO
3)
3And H
3BO
3Be dissolved in the distilled water respectively, the concentration of yttrium, europium and boron ion is respectively 0.1mol/L, 1.0mol/L and 1.0mol/L, is these three kinds of solution mixing in 0.9: 0.1: 1 in molar ratio, under the vigorous stirring, drip an amount of triethanolamine solution (triethanolamine: water=1: 1), obtain white gelatinous precipitate, distillation washing 2 times, absolute ethyl alcohol is washed 2 times, 120 ℃ of dryings 3 hours, grinding is sieved, and is placed in the high temperature furnace 700 ℃ of calcinings 3 hours then, and obtaining highly purified average grain diameter is the europium-doped yttrium borate powder of 50 nanometers.
Claims (1)
1. the preparation method of a yttrium borate doped nano powder comprises selection, the precipitation process of inorganic salts, suction filtration, drying and the calcination process of precipitation, it is characterized in that:
(1) composition formula of this nano-powder is Y
xL
1-xBO
3, L is a doping with rare-earth ions, and it is raw material that ruthenium ion, doping with rare-earth ions are selected corresponding nitrate for use, and it is raw material that boron is selected boric acid for use, and yttrium, rare earth doped and borate ion concentration all are 5.0-0.05mol/L, 0.8≤X＜1
(2) precipitating reagent adopts triethanolamine or triethylamine or diethylamine solution, and concentration is 5.0-0.05mol/L;
(3) precipitation suction filtration step is: will precipitate earlier with the distilled water washing, and use organic solvent washing again;
(4) drying is removed the moisture and the organic solvent of the absorption of precipitation presoma, and baking temperature is 100-120 ℃, and the time is 2-6 hour;
(5) calcining heat is 600-800 ℃, and the time is 2-6 hour.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1171369A (en) * | 1997-06-26 | 1998-01-28 | 中国科学院固体物理研究所 | Process for preparing nm-class bismuth titanate and its sosoloid |
| CN1297964A (en) * | 1999-11-30 | 2001-06-06 | 上海跃龙有色金属有限公司 | Preparation of red phosphor |
| CN1389540A (en) * | 2002-06-14 | 2003-01-08 | 中国地质大学（武汉） | Prepn. of europium activated yttrium-gadolinium borate phosphor |
-
2004
- 2004-11-01 CN CNB200410092065XA patent/CN100556586C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1171369A (en) * | 1997-06-26 | 1998-01-28 | 中国科学院固体物理研究所 | Process for preparing nm-class bismuth titanate and its sosoloid |
| CN1297964A (en) * | 1999-11-30 | 2001-06-06 | 上海跃龙有色金属有限公司 | Preparation of red phosphor |
| CN1389540A (en) * | 2002-06-14 | 2003-01-08 | 中国地质大学（武汉） | Prepn. of europium activated yttrium-gadolinium borate phosphor |
Non-Patent Citations (5)
| Title |
|---|
| （Y,Gd）BO3:Eu3＋荧光粉的合成及粒度控制. 董岩，蒋建清，肖睿，刘刚，陈会东，于金.中国稀土学报，第22卷第2期. 2004 * |
| 含Tb3+，Eu3+硼酸铝磷光体的制备及荧光特性. 周建国，赵凤英，郭宝生，李五聚，阮慎康，苏勉曾.化学研究与应用，第12卷第4期. 2000 * |
| 喷雾热解法制备YBO3:Eu球形发光粉. 王列松，林君，周永慧.高等学校化学学报，第25卷第1期. 2004 * |
| 溶胶-凝胶法制备小颗粒（Y,Gd）BO3：Eu及其表征. 蒋凯，余兴海，叶明新，黄玮石，黄京根.发光学报，第25卷第1期. 2004 * |
| 纳米材料的制备及在化工中的应用. 朱赛芬，吴周安.上海化工，第8期. 2001 * |
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