CN102464348A - Hydrothermal preparation method of lutetium oxide nanometer powder - Google Patents
Hydrothermal preparation method of lutetium oxide nanometer powder Download PDFInfo
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- CN102464348A CN102464348A CN2011102426575A CN201110242657A CN102464348A CN 102464348 A CN102464348 A CN 102464348A CN 2011102426575 A CN2011102426575 A CN 2011102426575A CN 201110242657 A CN201110242657 A CN 201110242657A CN 102464348 A CN102464348 A CN 102464348A
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- lutetium
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Abstract
The invention provides a preparation method of lutetium oxide nanometer powder, wherein the preparation method has the advantages of hydrothermal reaction availability, simple process and relatively low cost. According to the invention, ammonia is uniformly released from urea in a hydrothermal condition, to generate a high-quality precursor together with lutetium ions, and the precursor is roasted to obtain the lutetium oxide nanometer powder. The hydrothermal preparation method of the lutetium oxide nanometer powder, provided by the invention, is based on an aqueous-phase reaction; and the prepared lutetium oxide powder with high purity and nano-particle sizes are in a crystalline state.
Description
Technical field
The invention belongs to field of material preparation, relate in particular to a kind of preparation method of lutecium oxide nano-powder.
Background technology
Scintillation material is can absorb high energy particle or ray and the material that sends optical photon; In field extensive application such as high energy physics, nuclear medicine, space physics, geological prospectings, require it that ionizing rays is had high blocking ability (high-density and thick atom ordinal number are arranged).Lutecium oxide has high-density and thick atom ordinal number, and its prevention to all kinds of rays is effective; Band gap wide (6.5eV) can hold many activator ions as the luminescent material matrix between its valence band and conduction band, therefore enjoys people to favor as the scintillator substrate material.It mixes gadolinium sesquioxide and processes the solid solution matrix material simultaneously, can improve the blocking ability of gadolinium sesquioxide to ionizing rays; Improve gadolinium sesquioxide cube transformation temperature, help the transparent scintillating ceramic that sintering prepares high comprehensive performance to monocline.
Rare-earth oxide phosphor is widely used in high energy light photoluminescence and cathode ray luminous plane indicating meter.High resolving power, high-luminous-efficiency flat-panel monitor require high quality fluorescent material (purity is high, composition is even, particle is little, narrow diameter distribution).Yttrium oxide Y
2O
3Base fluorescent powder is common fluorescent material, as the yttrium oxide of mixing europium is a high efficiency red fluorescent material.Lutecium oxide optics with identical isometric system has isotropy, and each is identical to specific refractory power; Band gap is wide, can hold many active ions, like europium, thulium, dysprosium, erbium etc.; Have good physical and chemical stability, the advantage that do not receive that atmospheric constituent influences etc., be a kind of good phosphor material powder.Lutecium oxide also has characteristics such as high heat conductance, low thermal coefficient of expansion, low effective phonon energy, through mixing the ceramic laser material that Nd or Yb can be used as solid statelaser.
Therefore, lutecium oxide is a kind of luminescent material matrix that has application prospect, no matter be the lutecia based transparent ceramics material, or lutecia based fluorescent material, the preparation of high quality lutecium oxide powder all is a key link.The product of different powder compound methods has different granule-morphologies and specific surface area, has determined final material properties.Synthesis by solid state reaction commonly used, its technology is simple, be easy to produce in batches, but needs high-temperature calcination (it is big that the particle easy-sintering becomes), process of lapping (being prone to introduce impurity), is prone to exist second mutually and deficiencies such as unreacted components.The wet-chemical synthesis method comprises the precipitator method, sol-gel method etc., and product has exact chemical and forms and equally distributed component.
Preparation lutecium oxide powder mainly contains at present: the precipitator method, combustion method.The precipitator method are used inorganic amine precipitation agents such as ammoniacal liquor, bicarbonate of ammonia always, slowly add, and technology is complicated; The combustion method raw materials cost is high, and equipment requirements is higher.Is precipitation agent like the Shi Ying of Shanghai university etc. with ammoniacal liquor, bicarbonate of ammonia, has prepared the lutecium oxide presoma, has prepared nano oxidized lutetium powder (Journal of Inorganic Materials, 2008,4,824) through calcining.The Chen Qi of Shanghai Inst. of Silicate, Chinese Academy of Sciences is big, Shi Jianlin etc. adopted combustion synthesis method; Utilize the burn nano fluorophor powder based on lutecium oxide of synthesizing blender of redox thermopositive reaction; Particle diameter is 20-120nm (Chinese patent 200510027207.9); Also adopt ammoniacal liquor to add bicarbonate of ammonia as compound precipitants; Form doping lutecium oxide deposition presoma, obtain the lutecia based base ceramic material of the highly transparent of transmitance more than 80% (Chinese patent 200510027208.3) through pressureless sintering down through ageing, washing, drying, calcining, moulding, hydrogen atmosphere.It is raw material that the red grade of the Yang Qiu of Shanghai University will adopt high purity nanometer rare earth oxide powder, adds the PA sticker granulation of 5wt%, at 200MPa isostatic cool pressing lower sheeting; Under reducing atmosphere, carry out sintering in 1450～1800 ℃, make and mix Ce
3+Lutecium oxide base transparent flickering ceramic material.(Chinese patent 200810032379.9).The hydrothermal method reactive behavior is high, and synthetic particles dispersed degree is good, percent crystallinity is high, is a kind of Perfected process for preparing nano-powder.Hydrothermal method has better reactive behavior because temperature can reach more than 100 degrees centigrade than conventional wet chemistry method simultaneously, is good reaction system.
Therefore, the preparation method who develops a kind of hydro-thermal reaction, simpler, the lower-cost lutecium oxide nano-powder of technology has important use and is worth.The present invention evenly discharges ammonia through urea under hydrothermal condition, generate the high quality presoma with lutetium ion, obtains the lutecium oxide nano-powder through calcining.
Summary of the invention
The method that the purpose of this invention is to provide a kind of Hydrothermal Preparation high quality lutecium oxide nano-powder.
The present invention adopts following technical scheme:
1, a kind of preparation method of lutecium oxide nano-powder is a raw material with inorganic lutetium salt, is the precipitation from homogeneous solution agent with urea, under hydrothermal condition, generates presoma, makes the lutecium oxide nano-powder through calcining.
According to item 1 described preparation method, it is characterized in that 2, inorganic lutetium salt is selected high-purity inorganic salt for use, like lutecium chloride, lutecium nitrate.
According to item 1 described preparation method, it is characterized in that 3, precipitation agent is an analytical pure urea, be about 10:1-5:1 with the mol ratio of lutetium ion, it decomposes under hydrothermal condition, and precipitation from homogeneous solution generates the high quality presoma.
According to item 1 described preparation method, it is characterized in that 4, the temperature of hydro-thermal reaction is controlled in 120-180 degree centigrade, the reaction times was controlled in 5-10 hour.
According to item 1 described preparation method, it is characterized in that 5, the incinerating temperature is controlled in 500-1000 degree centigrade, the reaction times was controlled in 1-20 hour.
Compared with prior art, the present invention has following advantage: water react, technology are simple, cost is lower, and the lutecium oxide nano-powder of preparation is that crystal form, purity are high, particle diameter is about 20-50 nm.
Description of drawings
Fig. 1 is that particle diameter is the transmission electron microscope TEM figure of the lutecium oxide nano-powder of 20-50 nm;
Fig. 2 is that particle diameter is the x-ray diffractogram of powder of the lutecium oxide nano-powder of 20-50 nm.
Embodiment
Instance 1: be dissolved in 8.0 ml deionized waters to 0.5 g urea, add 8.0 ml LuCl again
3The aqueous solution (0.1 M), after stirring, solution is transferred in the withstand voltage reaction kettle of stainless steel of 40ml; After 8 hours, the gained white precipitate washs secondary through spinning respectively with deionized water and absolute ethyl alcohol 150 ℃ of reactions; Through vacuum-drying, calcined 10 hours, and obtained white powder for 800 ℃.Fig. 1 is its transmission electron microscope picture, can know that it is the nano particle of good dispersion degree, and median size is about 20-50 nm; Fig. 2 is its x-ray diffractogram of powder, can know that it is pure lutecium oxide Lu
2O
3
Instance 2: be dissolved in 4.0 ml deionized waters to 0.5 g urea, add 12.0 ml LuCl again
3The aqueous solution (0.1 M), after stirring, solution is transferred in the withstand voltage reaction kettle of stainless steel of 40ml; After 10 hours, the gained white precipitate washs secondary through spinning respectively with deionized water and absolute ethyl alcohol 150 ℃ of reactions; Through vacuum-drying, calcined 10 hours, and obtained white powder for 800 ℃.Through transmission electron microscope and powder x-ray diffraction analysis, its median size is about the pure lutecium oxide Lu of 20-60 nm
2O
3
Instance 3: be dissolved in 4.0 ml deionized waters to 0.5 g urea, add 8.0 ml Lu (NO again
3)
3The aqueous solution (0.1 M), after stirring, solution is transferred in the withstand voltage reaction kettle of stainless steel of 40ml; After 8 hours, the gained white precipitate washs secondary through spinning respectively with deionized water and absolute ethyl alcohol 130 ℃ of reactions; Through vacuum-drying, calcined 10 hours, and obtained white powder for 800 ℃.Through transmission electron microscope and powder x-ray diffraction analysis, its median size is about the pure lutecium oxide Lu of 20-50 nm
2O
3
Instance 4: be dissolved in 4.0 ml deionized waters to 0.5 g urea, add 12.0 ml Lu (NO again
3)
3The aqueous solution (0.1 M), after stirring, solution is transferred in the withstand voltage reaction kettle of stainless steel of 40ml; After 8 hours, the gained white precipitate washs secondary through spinning respectively with deionized water and absolute ethyl alcohol 170 ℃ of reactions; Through vacuum-drying, calcined 10 hours, and obtained white powder for 800 ℃.Through transmission electron microscope and powder x-ray diffraction analysis, its median size is about the pure lutecium oxide Lu of 30-70 nm
2O
3
Claims (5)
1. the preparation method of a lutecium oxide nano-powder is a raw material with inorganic lutetium salt, is the precipitation from homogeneous solution agent with urea, under hydrothermal condition, generates presoma, makes the lutecium oxide nano-powder through calcining.
2. preparation method according to claim 1 is characterized in that, inorganic lutetium salt is selected high-purity inorganic salt for use, like lutecium chloride, and lutecium nitrate.
3. preparation method according to claim 1 is characterized in that, precipitation agent is an analytical pure urea, is about 10:1-5:1 with the mol ratio of lutetium ion, and it decomposes under hydrothermal condition, and precipitation from homogeneous solution generates the high quality presoma.
4. preparation method according to claim 1 is characterized in that, the temperature of hydro-thermal reaction is controlled in 120-180 degree centigrade, and the reaction times was controlled in 5-10 hour.
5. preparation method according to claim 1 is characterized in that, the incinerating temperature is controlled in 500-1000 degree centigrade, and the reaction times was controlled in 1-20 hour.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106145959A (en) * | 2016-07-10 | 2016-11-23 | 九江学院 | A kind of preparation method of luteium oxide crystalline ceramics |
| CN107720802A (en) * | 2017-09-28 | 2018-02-23 | 上海应用技术大学 | A kind of preparation method for independently filling monodispersed luteium oxide nanosphere |
| CN114015088A (en) * | 2021-09-18 | 2022-02-08 | 东北师范大学 | Preparation method and application of organic-inorganic nano composite scintillator material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1760327A (en) * | 2005-06-28 | 2006-04-19 | 中国科学院上海硅酸盐研究所 | Nano fluorophor powder based on lutecium oxide and synthetic method of solution burning thereof |
| CN1840480A (en) * | 2005-03-29 | 2006-10-04 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
| CN101648726A (en) * | 2009-06-26 | 2010-02-17 | 上海大学 | Hydrothermal synthesis method of LuO(OH) nanorods and Lu2O3 nanorods luminescent powder |
-
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840480A (en) * | 2005-03-29 | 2006-10-04 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
| CN1760327A (en) * | 2005-06-28 | 2006-04-19 | 中国科学院上海硅酸盐研究所 | Nano fluorophor powder based on lutecium oxide and synthetic method of solution burning thereof |
| CN101648726A (en) * | 2009-06-26 | 2010-02-17 | 上海大学 | Hydrothermal synthesis method of LuO(OH) nanorods and Lu2O3 nanorods luminescent powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106145959A (en) * | 2016-07-10 | 2016-11-23 | 九江学院 | A kind of preparation method of luteium oxide crystalline ceramics |
| CN107720802A (en) * | 2017-09-28 | 2018-02-23 | 上海应用技术大学 | A kind of preparation method for independently filling monodispersed luteium oxide nanosphere |
| CN107720802B (en) * | 2017-09-28 | 2019-11-29 | 上海应用技术大学 | A kind of preparation method independently filling monodispersed luteium oxide nanosphere |
| CN114015088A (en) * | 2021-09-18 | 2022-02-08 | 东北师范大学 | Preparation method and application of organic-inorganic nano composite scintillator material |
| CN114015088B (en) * | 2021-09-18 | 2024-04-16 | 东北师范大学 | Preparation method and application of organic-inorganic nano composite scintillator material |
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Application publication date: 20120523 |