CN102206092A - Preparation method and preparation materials of Er-doped lithium niobate porous material - Google Patents
Preparation method and preparation materials of Er-doped lithium niobate porous material Download PDFInfo
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- CN102206092A CN102206092A CN2011100641581A CN201110064158A CN102206092A CN 102206092 A CN102206092 A CN 102206092A CN 2011100641581 A CN2011100641581 A CN 2011100641581A CN 201110064158 A CN201110064158 A CN 201110064158A CN 102206092 A CN102206092 A CN 102206092A
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Abstract
The invention discloses a preparation method and preparation materials of an Er-doped lithium niobate porous material. The preparation method comprises the following steps: preparing an Er-doped lithium niobate crystal material and deionized water which are utilized as raw materials into Er-doped lithium niobate minicrystals by using artificial and mechanical lapping methods; selecting the minicrystals with a proper grain size by utilizing a filtration method; and finally, preparing the Er-doped lithium niobate porous material through utilizing a drying and hardening or sintering method, wherein the size of an Er-doped lithium niobate particle in the porous material is between 100nm and 2mu m, the luminous wave length of the Er-doped lithium niobate porous material is located at multiple wavebands ranging from 400nm-1600nm, the selectable excitation wavelength is located at multiple wavebands ranging from 380nm-1500nm, and the Er-doped lithium niobate porous material has a down-conversion luminescence characteristic and an up-conversion luminescence characteristic. According to the invention, the problems that the existing luminous porous material is lack in luminous wavebands, the selectable pumping light wavelength range is narrow and the porous material capable of being applied to up-conversion luminescence is extremely less are solved.
Description
Technical field:
The invention belongs to the photonics material preparation field, the er-doped Lithium niobium trioxide porous material that relates to a kind of er-doped Lithium niobium trioxide porous material preparation method and use this method to prepare, this porous material can be used for inorganic porous material, fluorescent material and display material.
Background technology:
At present, porous material is used widely in many aspects such as molecular sieve, light-emitting display device, Random Laser gain media, filtration unit, biomimetic material preparations, and the porous material with characteristics of luminescence has irreplaceable effect aspect optoelectronic areas research and the industrial application especially.In addition, because luminous porous material has the wide-angle characteristics of luminescence, make it can be used as the base mateiral of laser display.1999, people such as Cao H. utilized the ZnO porous material to realize relevant Random Laser output.In addition, because of employed porous material in the accidental laser little more a lot of than conventional laser volume, be generally below several millimeters, this just makes that the porous material with characteristics of luminescence can be applied to the manufacturing of micron, nano laser, and can be applied to the preparation of micron, nano photoelectronic devices.Therefore, the porous material with characteristics of luminescence can be widely used in numerous key areas such as micro-nano photonics device, laser paint, laser display, biological tissue's detection, has huge potential prospect.
The at present prepared common light emitting region of luminous porous material that goes out is wide inadequately, for example, similar techniques is disclosed in Chinese patent application CN200910009135.3, but the prepared luminous porous material that goes out of prior art can't be contained the spectral range from 400nm to 1600nm, and its operable excitation wavelength is also less relatively, and 1-2 suitable excitation wavelength only arranged usually.In addition, the porous material that has the characteristics of luminescence at present is in the majority with down-conversion luminescence, be the emergent light that the long pump light of radiothermy excites the long wavelength, excite its application of the photoemissive occasion of short wavelength to be restricted and need do pumping source with long wavelength's light source at some.That is, be subjected to the restriction of excitation light source and spectral range, use face narrower in actual applications thereby cause.
Because the needs of scientific research and production are badly in need of the broad luminous porous material of a kind of adaptive surface and are put in the practical application.
Summary of the invention:
In order to solve the problem that exists in the top background technology, the present invention proposes a kind of er-doped Lithium niobium trioxide porous material preparation method and uses the er-doped Lithium niobium trioxide porous material of this method preparation.Use the prepared er-doped Lithium niobium trioxide porous material of this preparation method to overcome the existing luminous wavelength band deficiency of luminous porous material, can select problems such as the pump light wavelength region is little for use, and can be applied to up-conversion luminescence.
For achieving the above object, technical scheme of the present invention is to utilize er-doped lithium niobate crystals material and deionized water to be raw material, utilize the method for craft and mechanical mill to prepare er-doped Lithium niobium trioxide crystallite, utilize filtering method to select the crystallite of appropriate particle size again, utilize dry and hard at last or the agglomerating method is prepared the er-doped Lithium niobium trioxide porous material with specific standard.
According to a first aspect of the present invention, a kind of porous er-doped Lithium niobium trioxide preparation methods is provided, may further comprise the steps:
(1) er-doped lithium niobate crystals material is ground into small pieces of material with mortar;
(2) place ball mill to carry out mechanical mill these small pieces of material, make it become powder;
(3) powder is passed through screen cloth, thus the elimination macrobead;
(4) will form suspension liquid at the vessel thorough mixing by powder behind the screen cloth and deionized water;
(5) suspension liquid is passed through filter membrane, thus further elimination larger particles;
(6) suspension liquid is placed constant temperature oven to becoming block porous material, be er-doped Lithium niobium trioxide porous material.
Preferably, employed water is deionized water; The hardness of employed grinding pot and mill ball is greater than the hardness of er-doped lithium niobate crystals in the ball mill, and the rotating speed of milling time and ball mill is selected according to the size of the er-doped Lithium niobium trioxide small pieces of material that obtains in the step (1).
More preferably, milling time is 6 hours-12 hours, and rotating speed is 600 rev/mins-1000 rev/mins.
Preferably, selecting the pore size of screen cloth according to the size of powder is 15 μ m-200 μ m; The temperature of constant temperature oven is set between 30 degrees centigrade-800 degrees centigrade, and the caking process is dry and hard or sintering.In addition, select filter membrane according to particulate size and concrete needs in the suspension liquid.Further, the pore size of filter membrane is 100 nanometers (nm)-2 micron (μ m).
According to a second aspect of the present invention, a kind of er-doped Lithium niobium trioxide porous material that uses above-mentioned porous er-doped Lithium niobium trioxide preparation methods preparation is provided, the concentration of Er of the er-doped Lithium niobium trioxide porous material of its preparation is between 0.01wt.%-0.50wt.%, the crystal fine particle size is 100nm-2 μ m, and pore size is 100nm-2 μ m.
Advantage of the present invention and useful result are: this er-doped Lithium niobium trioxide porous material manufacture craft is simple, and light emitting region is big, and its emission wavelength is arranged in a plurality of wave bands from 400nm to the 1600nm scope; And the scope of its optional excitation wavelength is also bigger, is arranged in a plurality of wave bands from 380nm to the 1500nm scope; In addition, this er-doped Lithium niobium trioxide porous material not only has the down-conversion luminescence characteristic but also have the up-conversion luminescence characteristic.
Embodiment:
Reach technique means and the effect that predetermined goal of the invention is taked for further setting forth the present invention, the er-doped Lithium niobium trioxide porous material preparation method who the present invention is proposed below in conjunction with example and use the prepared material of this preparation method to be elaborated.
Core purpose of the present invention is to overcome the existing luminous wavelength band deficiency of luminous porous material, can select the few problem of porous material that the pump light wavelength region is little and can be applied to up-conversion luminescence for use, propose a kind of er-doped Lithium niobium trioxide porous material preparation method and use the prepared material of this preparation method.The present invention utilizes er-doped Lithium niobium trioxide body material and deionized water to be starting material, utilize the method for craft and mechanical mill to prepare er-doped Lithium niobium trioxide crystallite, utilize filtering method to select the crystallite of appropriate particle size again, utilize dry and hard at last or the agglomerating method is prepared er-doped Lithium niobium trioxide porous material.
Er-doped Lithium niobium trioxide porous material is prepared by following steps:
(1) er-doped lithium niobate crystals body material is manually ground into small pieces of material below the 3mm with mortar.
(2) place planetary ball mill to carry out abundant mechanical mill these small pieces of material, thereby make it become powder.
(3) be the screen cloth of 15 μ m with powder by the aperture, thus the elimination macrobead.
(4) in the silica glass vessel, utilize magnetic stirrer and ultrasonic agitation machine thorough mixing to stir the formation suspension liquid gained powder and deionized water.
(5) be the filter membrane of 220nm with suspension liquid by the aperture, thus further elimination larger particles.
(6) will place the silica glass vessel through the suspension liquid behind the filter membrane, and put it into temperature and be set in 60 degrees centigrade the constant temperature oven to be block porous material to dry and hard.
What further specify in addition, is as follows:
Er-doped Lithium niobium trioxide material is selected the Lithium niobium trioxide material of concentration of Er 0.01wt.%-0.50wt.% for use according to concrete needs, and selects for use hardness to grind greater than the mortar of er-doped Lithium niobium trioxide material.The grinding pot of ball mill and mill ball select for use hardness to grind greater than the grinding pot and the mill ball of er-doped Lithium niobium trioxide material, and milling time and rotating speed are selected according to the size of the er-doped Lithium niobium trioxide small pieces of material that obtains in the step (1): milling time is 6 hours-12 hours; Rotating speed is 600 rev/mins-1000 rev/mins.It is 15 μ m-200 μ m that screen cloth described in the above-mentioned steps (3) is selected its pore size according to the size of powder.
Powder in the above-mentioned steps (4) is selected the vessel that do not react with er-doped Lithium niobium trioxide material and deionized water for use with the vessel of water mixing stirring.
Filter membrane in the above-mentioned steps (5), selecting its pore size according to particulate size and concrete needs in the suspension liquid is 100nm-2 μ m.
The thermostat temperature that baking oven in the above-mentioned steps (6) is set is between 30-800 degree centigrade, and the caking process can be dry and hard or sintering.
The er-doped Lithium niobium trioxide porous material that obtains in above-mentioned preparation method not only has the down-conversion luminescence characteristic but also have the up-conversion luminescence characteristic.This er-doped Lithium niobium trioxide porous material can 381nm, 488nm, 660nm, 800nm, 980nm, and a plurality of wavelength exciting lights such as 1480nm under emitting fluorescence, its emitting fluorescence scope is positioned at a plurality of emission bands between 400nm-1600nm, and has a plurality of up-conversion fluorescence emission bands in the 400nm-710nm scope under 800nm and 980nm exciting light.
The er-doped Lithium niobium trioxide is because of its abundant energy level, make its emission wavelength be arranged in a plurality of wave bands from 400nm to the 1600nm scope, and the scope of its optional excitation wavelength is also bigger, is arranged in a plurality of wave bands from 380nm to the 1500nm scope; In addition, its unique up-conversion luminescence characteristic makes it can carry out up-conversion luminescence output simultaneously.These unique character are surveyed in laser display, biological tissue, the research and the industry manufacture field of micro-nano photonics device all have huge using value and prospect.
Be summarized as follows: the preparation of the er-doped Lithium niobium trioxide porous material that the present invention proposes is a raw material with er-doped lithium niobate crystals body material and deionized water, utilize the method for craft and mechanical mill to prepare er-doped Lithium niobium trioxide crystallite, utilize filtering method to select the crystallite of appropriate particle size again, utilize dry and hard at last or the agglomerating method is prepared er-doped Lithium niobium trioxide porous material, the er-doped Lithium niobium trioxide particle size in its porous material is between 100nm-2 μ m; The emission wavelength of er-doped Lithium niobium trioxide porous material is arranged in from a plurality of wave bands of 400nm-1600nm scope and optional excitation wavelength and is arranged in a plurality of wave bands from the 380nm-1500nm scope; Er-doped Lithium niobium trioxide porous material not only has the down-conversion luminescence characteristic but also have the up-conversion luminescence characteristic.The invention solves the existing luminous wavelength band deficiency of luminous porous material, can select the few problem of porous material that the pump light wavelength region is little and can be applied to up-conversion luminescence for use.
As above-mentioned, the clear material that has described the er-doped Lithium niobium trioxide porous material preparation method of the present invention's proposition in detail and used its method preparation.Although the present invention is described and explained to the preferred embodiments of the present invention in detail, but this area those skilled in the art be appreciated that, under the situation of the spirit and scope of the present invention that do not deviate from the claims definition, can in form and details, make multiple modification.
Claims (9)
1. er-doped Lithium niobium trioxide porous material preparation method, it may further comprise the steps:
(1) er-doped lithium niobate crystal body and function mortar is ground into small pieces of material;
(2) place ball mill to carry out mechanical mill these small pieces of material, make it become powder;
(3) powder is passed through screen cloth, thus the elimination macrobead;
(4) will form suspension liquid by thorough mixing in vessel by powder behind the screen cloth and water;
(5) suspension liquid is passed through filter membrane, thus further elimination larger particles;
(6) suspension liquid is placed constant temperature oven to becoming block porous material, be er-doped Lithium niobium trioxide porous material.
2. er-doped Lithium niobium trioxide porous material preparation method according to claim 1, wherein employed water is deionized water.
3. er-doped Lithium niobium trioxide porous material preparation method according to claim 1, wherein the hardness of employed grinding pot and mill ball is greater than the hardness of er-doped lithium niobate crystals in the ball mill, and the rotating speed of milling time and ball mill is selected according to the size of the er-doped Lithium niobium trioxide small pieces of material that obtains in the step (1).
4. er-doped Lithium niobium trioxide porous material preparation method according to claim 3, wherein milling time is 6 hours to 12 hours, rotating speed is 600 rev/mins-1000 rev/mins.
5. er-doped Lithium niobium trioxide porous material preparation method according to claim 1, wherein selecting the pore size of screen cloth according to the size of powder is 15 μ m-200 μ m (micron).
6. er-doped Lithium niobium trioxide porous material preparation method according to claim 1 wherein selects filter membrane according to particulate size and concrete needs in the suspension liquid.
7. er-doped Lithium niobium trioxide porous material preparation method according to claim 6, wherein the pore size of filter membrane is that 100 nanometers (nm) are to 2 microns (μ m).
8. er-doped Lithium niobium trioxide porous material preparation method according to claim 1, wherein the temperature with constant temperature oven is set between 30 degrees centigrade-800 degrees centigrade, and the caking process is dry and hard or sintering.
9. use aforesaid right to require the er-doped Lithium niobium trioxide porous material of the arbitrary described preparation method's preparation among the 1-8, the concentration of Er that it is characterized in that er-doped Lithium niobium trioxide porous material is between 0.01wt.%-0.50wt.%, the crystal fine particle size is 100nm-2 μ m, and pore size is that 100nm (nanometer) is to 2 μ m.
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Citations (4)
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| JP2000332314A (en) * | 1999-05-25 | 2000-11-30 | Murata Mfg Co Ltd | Production of piezoelectric substrate |
| US20050016274A1 (en) * | 2000-02-18 | 2005-01-27 | Fujitsu Limited | Acceleration sensor |
| CN101050122A (en) * | 2007-05-21 | 2007-10-10 | 北京工业大学 | Method for preparing functional ceramic of lithium niobate |
| CN101575734A (en) * | 2009-04-27 | 2009-11-11 | 哈尔滨工业大学 | Erbium-doped lithium niobate crystal and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000332314A (en) * | 1999-05-25 | 2000-11-30 | Murata Mfg Co Ltd | Production of piezoelectric substrate |
| US20050016274A1 (en) * | 2000-02-18 | 2005-01-27 | Fujitsu Limited | Acceleration sensor |
| CN101050122A (en) * | 2007-05-21 | 2007-10-10 | 北京工业大学 | Method for preparing functional ceramic of lithium niobate |
| CN101575734A (en) * | 2009-04-27 | 2009-11-11 | 哈尔滨工业大学 | Erbium-doped lithium niobate crystal and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李仲秋等: "铒掺杂对铌酸锂晶体光学性质的影响", 《哈尔滨师范大学自然科学学报》 * |
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