CN102206092B - 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
- Publication number
- CN102206092B CN102206092B CN 201110064158 CN201110064158A CN102206092B CN 102206092 B CN102206092 B CN 102206092B CN 201110064158 CN201110064158 CN 201110064158 CN 201110064158 A CN201110064158 A CN 201110064158A CN 102206092 B CN102206092 B CN 102206092B
- Authority
- CN
- China
- Prior art keywords
- lithium niobate
- doped lithium
- materials
- preparation
- porous material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Luminescent Compositions (AREA)
- Lasers (AREA)
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 materials of Er-doped lithium niobate porous that relates to a kind of materials of Er-doped lithium niobate porous preparation method and use the 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, so that it can be used as the base mateiral of laser display.1999, the 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 is just so that have the manufacturing that the porous material of the characteristics of luminescence can be applied to 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 photonic 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 is wide not, for example, similar technology is disclosed in Chinese patent application CN200910009135.3, but the prepared luminous porous material of prior art can't be contained the spectral range from 400nm to 1600nm, and its operable excitation wavelength is also relatively less, and 1-2 suitable excitation wavelength only arranged usually.In addition, the following conversion luminescence of porous material that has at present the characteristics of luminescence is in the majority, 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 to do pumping source with long wavelength's light source at some.That is, be subject to the restriction of excitation light source and spectral range, use in actual applications face narrower 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 materials of Er-doped lithium niobate porous preparation method and uses the materials of Er-doped lithium niobate porous of the method preparation.Use the prepared materials of Er-doped lithium niobate porous of this preparation method to overcome the luminous wavelength band deficiency of existing luminous porous material, can select the problems such as the pump light wavelength region is little, 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 crystalline material and deionized water to be raw material, utilize the method for craft and mechanical mill to prepare the Er-doped lithium niobate crystallite, the crystallite that the method that recycling is filtered is selected appropriate particle size utilizes the method for dry and hard or sintering to prepare the materials of Er-doped lithium niobate porous with specific standard at last.
According to a first aspect of the present invention, a kind of porous Er-doped lithium niobate material preparation method is provided, may further comprise the steps:
(1) the Er-doped lithium niobate crystalline 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 fully mix the formation suspension liquid with deionized water at vessel by the powder behind the screen cloth;
(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 materials of Er-doped lithium niobate porous.
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 crystal 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 niobate 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; Between 30 degrees centigrade-800 degrees centigrade, the caking process is dry and hard or sintering with the Temperature Setting of constant temperature oven.In addition, select filter membrane according to size and the concrete needs of particle 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 materials of Er-doped lithium niobate porous that uses above-mentioned porous Er-doped lithium niobate material preparation method preparation is provided, the concentration of Er of the materials of Er-doped lithium niobate porous 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 materials of Er-doped lithium niobate porous manufacture craft is simple, and light emitting region is large, 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 larger, is arranged in a plurality of wave bands from 380nm to the 1500nm scope; In addition, this materials of Er-doped lithium niobate porous not only has lower conversion luminescence characteristic but also has Upconversion luminescence.
Embodiment:
Reach technique means and the effect that predetermined goal of the invention is taked for further setting forth the present invention, the materials of Er-doped lithium niobate porous 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.
It is not enough that core purpose of the present invention is to overcome the luminous wavelength band of existing 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, propose a kind of materials of Er-doped lithium niobate porous preparation method and use the prepared material of this preparation method.The present invention utilizes Er-doped lithium niobate body material and deionized water to be starting material, utilize the method for craft and mechanical mill to prepare the Er-doped lithium niobate crystallite, the crystallite that the method that recycling is filtered is selected appropriate particle size utilizes the method for dry and hard or sintering to prepare materials of Er-doped lithium niobate porous at last.
Materials of Er-doped lithium niobate porous is prepared by following steps:
(1) Er-doped lithium niobate crystal 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 the abundant mix and blend of ultrasonic agitation machine to form 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 through the suspension liquid behind the filter membrane silica glass vessel, and put it in the constant temperature oven that temperature setting is set to 60 degrees centigrade to dry and hard and be block porous material.
What further specify in addition, is as follows:
The Er-doped lithium niobate material is selected the Lithium niobium trioxide material of concentration of Er 0.01wt.%-0.50wt.% according to concrete needs, and selects hardness to grind greater than the mortar of Er-doped lithium niobate material.The grinding pot of ball mill and mill ball select hardness to grind greater than grinding pot and the mill ball of Er-doped lithium niobate material, and milling time and rotating speed are selected according to the size of the Er-doped lithium niobate 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) and water carry out the vessel of mix and blend and select the vessel that do not react with Er-doped lithium niobate material and deionized water.
Filter membrane in the above-mentioned steps (5), selecting its pore size according to the size of particle in the suspension liquid and concrete needs 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 materials of Er-doped lithium niobate porous that obtains in above-mentioned preparation method not only has lower conversion luminescence characteristic but also has Upconversion luminescence.This materials of Er-doped lithium niobate porous 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.
Er-doped lithium niobate 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 larger, is arranged in a plurality of wave bands from 380nm to the 1500nm scope; In addition, its unique Upconversion luminescence makes it can carry out up-conversion luminescence output simultaneously.These unique character are surveyed in laser display, biological tissue, research and the industry manufacture field of micro-nano photonic device all have huge using value and prospect.
Be summarized as follows: the preparation of the materials of Er-doped lithium niobate porous that the present invention proposes is take Er-doped lithium niobate crystal body material and deionized water as raw material, utilize the method for craft and mechanical mill to prepare the Er-doped lithium niobate crystallite, the method that recycling is filtered is selected the crystallite of appropriate particle size, utilize at last the method for dry and hard or sintering to prepare materials of Er-doped lithium niobate porous, the Er-doped lithium niobate particle size in its porous material is between 100nm-2 μ m; The emission wavelength of materials of Er-doped lithium niobate porous 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; Materials of Er-doped lithium niobate porous not only has lower conversion luminescence characteristic but also has Upconversion luminescence.It is not enough to the invention solves the luminous wavelength band of existing 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.
As above-mentioned, the materials of Er-doped lithium niobate porous preparation method who has described the present invention's proposition in detail and the material that uses its method preparation have been known.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, in 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 (5)
1. materials of Er-doped lithium niobate porous preparation method, it may further comprise the steps:
(1) the Er-doped lithium niobate crystal 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 in vessel, fully mix the formation suspension liquid by the 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 materials of Er-doped lithium niobate porous;
Wherein, the pore size of screen cloth is 15 microns-200 microns, the pore size of filter membrane is 100 nanometers to 2 micron, and the concentration of Er of materials of Er-doped lithium niobate porous is between 0.01wt.%-0.50wt.%, and the Temperature Setting of constant temperature oven is between 30 degrees centigrade-800 degrees centigrade.
2. materials of Er-doped lithium niobate porous preparation method according to claim 1, wherein employed water is deionized water.
3. materials of Er-doped lithium niobate porous 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 crystal 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 niobate small pieces of material that obtains in the step (1).
4. materials of Er-doped lithium niobate porous 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. materials of Er-doped lithium niobate porous preparation method according to claim 1, wherein the caking process is dry and hard or sintering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110064158 CN102206092B (en) | 2011-03-17 | 2011-03-17 | Preparation method and preparation materials of Er-doped lithium niobate porous material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110064158 CN102206092B (en) | 2011-03-17 | 2011-03-17 | Preparation method and preparation materials of Er-doped lithium niobate porous material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102206092A CN102206092A (en) | 2011-10-05 |
| CN102206092B true CN102206092B (en) | 2013-01-09 |
Family
ID=44695192
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110064158 Expired - Fee Related CN102206092B (en) | 2011-03-17 | 2011-03-17 | Preparation method and preparation materials of Er-doped lithium niobate porous material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102206092B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000332314A (en) * | 1999-05-25 | 2000-11-30 | Murata Mfg Co Ltd | Production of piezoelectric substrate |
| JP2001228168A (en) * | 2000-02-18 | 2001-08-24 | Fujitsu Ltd | Acceleration sensor |
-
2011
- 2011-03-17 CN CN 201110064158 patent/CN102206092B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (3)
| Title |
|---|
| JP特开2000-332314A 2000.11.30 |
| 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》.2009,第25卷(第6期),全文. |
| 铒掺杂对铌酸锂晶体光学性质的影响;李仲秋等;《哈尔滨师范大学自然科学学报》;20091231;第25卷(第6期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102206092A (en) | 2011-10-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Naik et al. | Low temperature synthesis and photoluminescence properties of red emitting Mg2SiO4: Eu3+ nanophosphor for near UV light emitting diodes | |
| Chen et al. | Combinatorial approach to the development of a single mass YVO4: Bi3+, Eu3+ phosphor with red and green dual colors for high color rendering white light-emitting diodes | |
| CN103265954B (en) | Potassium-sodium niobate based oxide up-conversion luminescent material and preparation method thereof | |
| Yu et al. | Fabrication of Nd: YAG transparent ceramics using powders synthesized by citrate sol-gel method | |
| CN102060519A (en) | Method for preparing rare earth doped yttrium aluminum garnet transparent ceramics by utilizing spray granulation modified powder | |
| CN107418580A (en) | A kind of preparation method for improving up-conversion luminescence film | |
| CN102321475A (en) | Oxide compound up-conversion luminescent material of a kind of calcium titanium ore structure and preparation method thereof | |
| Sengthong et al. | A bright yellow light from a Yb 3+, Er 3+-co-doped Y 2 SiO 5 upconversion luminescence material | |
| CN105950146A (en) | Preparation method of hydroxylapatite fluorescent material doped with rare earth samarium | |
| JP2007254723A (en) | Eu-CONTAINING INORGANIC COMPOUND, LUMINESCENT COMPOSITION CONTAINING THE SAME AND ILLUMINANT, SOLID-STATE LASER APPARATUS AND LIGHT EMITTING DEVICE | |
| CN102206092B (en) | Preparation method and preparation materials of Er-doped lithium niobate porous material | |
| CN102373058B (en) | Silicate fluorescent material and preparation method thereof | |
| CN108545950A (en) | A kind of er-doped biological activity glass and preparation method thereof | |
| CN109082272A (en) | A kind of red light fluorescent powder and preparation method thereof | |
| Hirano et al. | Intense up-conversion luminescence of Er3+/Yb3+ co-doped YNbO4 through hydrothermal route | |
| CN102140692B (en) | Holmium-ytterbium-doped lithium potassium niobate monocrystal and preparation method thereof | |
| KR101302417B1 (en) | Preparation method of green-emitting phosphor using mesoporous silica, and the green-emitting phosphor thereby | |
| CN208862021U (en) | A kind of LED coating of multilayer encapsulation quantum dot | |
| CN108512029B (en) | Ultra-wideband random laser scattering material based on amorphous bismuthate, laser device, preparation and application | |
| CN104946253A (en) | Double-rare-earth element doped zirconia luminescent powder | |
| CN102211942A (en) | Preparation method of Er: YAG polycrystal transparent ceramic material | |
| CN110964497B (en) | Optical anti-counterfeiting material and preparation method thereof | |
| CN109825292B (en) | Preparation method and application of inorganic microparticles with photoresponse and green long-afterglow luminescence effects | |
| CN109097043A (en) | A kind of erbium and ytterbium codope sodium niobate up-conversion and its preparation method and application | |
| CN109233829B (en) | Magnesium erbium ytterbium three-doped sodium niobate and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130109 |