CN103614139B - Reverse co-precipitation is adopted to prepare Gd 2ti 2o 7: the method for Ce nano-luminescent powder body - Google Patents
Reverse co-precipitation is adopted to prepare Gd 2ti 2o 7: the method for Ce nano-luminescent powder body Download PDFInfo
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Abstract
Reverse co-precipitation is adopted to prepare Gd
2ti
2o
7: the method for Ce nano-luminescent powder body, relates to a kind of preparation method preparing nano-luminescent powder body, adopts high-purity Gd
2o
3with the relatively inexpensive and Ti (SO of easy handling
4)
2as reaction raw materials, with Ce (NO
3)
3as activator, adopt ammoniacal liquor as precipitation agent, using Sodium dodecylbenzene sulfonate (SDBS) as dispersion agent.Preparation process comprises the preparation of female salts solution, titration precipitation, timeliness, washing, filtration, drying, calcining, process of grinding and to sieve etc.Gd
2ti
2o
7: in Ce nano-luminescent powder body, the content of Ce is in 0.3-2.0%(molar fraction) between.Present invention process is simple, reaction conditions controllable precise, and the less and good dispersity of powder particle size, is suitable for suitability for industrialized production.As nano-powder raw material, have wide practical use in coating or ceramic field.
Description
Technical field
The present invention relates to a kind of preparation method of nano-luminescent powder body, particularly relate to the reverse co-precipitation of a kind of employing and prepare Gd
2ti
2o
7: the method for Ce nano-luminescent powder body.
Background technology
Gd
2ti
2o
7be a kind of have pyrochlore type structure containing oxygen rare earth compound, there is the performance of uniqueness in electricity, magnetic, luminescence and catalysis etc.Gd
2ti
2o
7there is high-melting-point, the features such as higher chemical stability and ionic conductivity, in fields such as ionophore, catalyzer, luminous host material and solidification of radwastes, there is very high scientific research value and application prospect.At present, about Gd
2ti
2o
7research mainly concentrate on the aspects such as microtexture, magnetic property and electrical properties.Research shows the Gd with pyrochlore constitution
2ti
2o
7be a kind of excellent rare earth luminous substrate material, there is lower phonon energy.Therefore, by selecting suitable rare earth ion and doping content, efficient luminescent properties can be obtained within this material.Select Ce
3+due to Ce as activator
3+only have a 4f electronics, there is the simplest 4f-5d Ground-state Structures, Ce
3+the f-d transition that ion parity allows has important using value.In powder sintering field, the luminescent properties of powder significantly strengthens along with the reduction of particle size; In addition, the reduction of grain size can improve sintering activity and the sintered density of powder, and reduces sintering temperature.Therefore, prepare good dispersity, the less and Gd be evenly distributed of particle diameter
2ti
2o
7: Ce nano-luminescent powder body has Important Economic to commercialization demand and is worth.
The method that routine prepares nano-luminescent powder body has high temperature solid-state method, hydrothermal method, sol-gel method, microemulsion method, self-propagating synthesis and coprecipitation method etc.In above-mentioned preparation method, high temperature solid-state method sintering temperature is higher and particle size skewness, purity are low; Hydrothermal method is high to equipment requirements, and cost is high, yields poorly; The powder granule of sol-gel method synthesis is comparatively large and reunion is serious; Microemulsion method preparation technology relative complex, yields poorly; The particle size that self-propagating synthesis obtains is uneven.By contrast, the reaction product of coprecipitation method reaches nano level, can realize that ion doping is even, product purity is high, uniform particle sizes; It is the synthetic method that a kind of component with low cost, each accurately can control, be easy to realize industrialization.Coprecipitation method is adopted to prepare Gd
2ti
2o
7: Ce nano-powder, using Sodium dodecylbenzene sulfonate (SDBS) as dispersion agent, improves dispersed and improves morphology microstructure.By changing processing condition, control Gd
2ti
2o
7: the size of Ce nano-powder and size-grade distribution, thus the Gd obtaining that morphology microstructure is controlled, luminescent properties is excellent
2ti
2o
7: Ce nano-powder.
Summary of the invention
The reverse co-precipitation of a kind of employing is the object of the present invention is to provide to prepare Gd
2ti
2o
7: the method for Ce nano-luminescent powder body, the method using ammoniacal liquor as precipitation agent, using Sodium dodecylbenzene sulfonate (SDBS) as dispersion agent; By back titration legal system for Gd
2ti
2o
7: Ce nano-luminescent powder body.The method technique is simple, reaction conditions controllable precise; Preparation Gd
2ti
2o
7: Ce particle diameter of nanometer powder is less, is evenly distributed, approximate sphericity.
The object of the invention is to be achieved through the following technical solutions:
Reverse co-precipitation is adopted to prepare Gd
2ti
2o
7: the method for Ce nano-luminescent powder body, the method adopts high-purity Gd
2o
3with relatively inexpensive and easy handling Ti (SO
4)
2as reaction raw materials, with Ce (NO
3)
3as activator, using ammoniacal liquor as precipitation agent, adopt Sodium dodecylbenzene sulfonate (SDBS) as dispersion agent; Preparation process comprises the preparation of female salts solution, titration precipitation, timeliness, washing, filtration, drying, calcining, process of grinding and sieve.
Described one adopts reverse co-precipitation to prepare Gd
2ti
2o
7: the method for Ce nano-luminescent powder body, Ce
3+doping content between 0.3-2.0% molar fraction.
Described one adopts reverse co-precipitation to prepare Gd
2ti
2o
7: the method for Ce nano-luminescent powder body, the starting point concentration of female salts solution is 0.06 ~ 0.10mol/L; Precipitation agent ammonia concn is 1 ~ 2mol/L; Dispersion agent Sodium dodecylbenzene sulfonate (SDBS) consumption is 1wt% ~ 2wt%.
Described one adopts reverse co-precipitation to prepare Gd
2ti
2o
7: the method for Ce nano-luminescent powder body, precipitation agent is titrated in female salts solution, back titration method, titration speed is 1 ~ 4ml/min, temperature of reaction system is 0 ~ 20 DEG C, the pH value adjusting titration end point reaction system with ammoniacal liquor is 10 ~ 12, timeliness 12h, and the temperature and time of presoma drying is respectively 80 ~ 100 DEG C and 12 ~ 24 h.
Described one adopts reverse co-precipitation to prepare Gd
2ti
2o
7: the method for Ce nano-luminescent powder body, calcining temperature and soaking time are respectively 800 ~ 1100 DEG C and 1 ~ 3h.
Advantage of the present invention and effect are:
Chemical feedstocks that the present invention adopts is with low cost, and technique is simple, reaction conditions controllable precise, and preparation cycle is short, is applicable to batch production.In preparation process, by controlling female salts solution starting point concentration, the pH value of titration end point reaction system, titration speed, dispersant dosage, the condition such as calcining temperature and calcination time, reach the pattern and grain size that control powder product.Presoma is incubated 1h and obtains the Gd of size at about 50nm under lower calcining temperature (900 DEG C)
2ti
2o
7: Ce nano-powder, pattern is spherical substantially, better dispersed.As nano-powder raw material, have wide practical use in coating or ceramic field.
Accompanying drawing explanation
Fig. 1 is Gd
2ti
2o
7: the XRD figure spectrum of Ce powder;
Fig. 2 is female concentration of salt solution is that 0.08mol/L obtains presoma, the Gd obtained after 900 DEG C of calcining 1h
2ti
2o
7: the SEM shape appearance figure of Ce powder;
Fig. 3 is female concentration of salt solution is that 0.06mol/L obtains presoma, the Gd obtained after 900 DEG C of calcining 1h
2ti
2o
7: the SEM shape appearance figure of Ce powder;
Fig. 4 is female concentration of salt solution is that 0.10mol/L obtains presoma, the Gd obtained after 900 DEG C of calcining 1h
2ti
2o
7: the SEM shape appearance figure of Ce powder;
Fig. 5 is the Gd of various ce contents 0.3-2.0mol %
2ti
2o
7: the luminescent properties comparison diagram of Ce powder.
Note: Fig. 1-Fig. 5 of the present invention is analysis schematic diagram or the photo (only for reference) of product state, word or the unintelligible understanding do not affected technical solution of the present invention of image in figure.
Embodiment
Below in conjunction with specific examples, the present invention is further described.
Embodiment 1:
Material selection of the present invention: experimental raw is Gd
2o
3(99.99%), Ce (NO
3)
3(99.9%), Ti (SO
4)
2, ammoniacal liquor, nitric acid, dehydrated alcohol and Sodium dodecylbenzene sulfonate (SDBS) be analytical reagent, distilled water is intermediate water.Above reagent is all without purification process.
Preparation process of the present invention: take Gd according to precise stoichiometry ratio
2o
3, Ti (SO
4)
2with Ce (NO
3)
3.By Gd
2o
3be dissolved in excessive dilute nitric acid solution, obtain Gd (NO
3)
3solution; Again by Ti (SO
4)
2being dissolved in above-mentioned solution preparation after water-soluble becomes metal cation concentration to be female salts solution of 0.08mol/L.Take 0.3%(molar fraction) Ce (NO
3)
3be dissolved in female salts solution being stirred well to and mix.Preparation 1mol/L ammoniacal liquor is precipitation agent, and the dispersion agent SDBS taking 1wt% ~ 2wt% is dissolved in precipitation agent ammoniacal liquor and stirs.Female salts solution is titrated to (back titration) in precipitation agent, magnetic agitation, controlling titration speed with peristaltic pump is 2ml/min, temperature of reaction system is 0 DEG C, the pH value adjusting titration end point reaction system with ammoniacal liquor is 11, namely the pioneer precipitate of white flock is obtained, timeliness 12h, after filtering, clean 4 times with distilled water, then use washes of absolute alcohol 2 times, removing foreign ion, then presoma is placed in vacuum drying oven (80 DEG C) dry 12h, puts into crucible and calcine 1h at 1173K after grinding, product sieves through grinding and namely obtains Gd
2ti
2o
7: Ce nano-powder.The XRD figure spectrum of gained sample as shown in Figure 1, the characteristic peak of products therefrom and Gd as seen from Figure 1
2ti
2o
7standard P DF card No.23-0259 completely the same, sample complete crystallization.Do not observe other impurity peaks, show Ce
3+be incorporated in matrix, there is not the derivative of Ce.As shown in Figure 2, sample topography is spherical to the SEM figure of gained sample, and particle diameter is about 50nm, even particle size distribution, and sample dispersion is good.
Embodiment 2:
Female salt concn is 0.06mol/L, and other conditions are as embodiment 1, and the pattern of gained sample is as shown in SEM in Fig. 3, and sample topography is subsphaeroidal substantially, and particle diameter is about 60nm, and sample dispersion is general, there is agglomeration.
Embodiment 3:
Female salt concn is 0.10mol/L, and other conditions are as embodiment 1, and the pattern of gained sample is as shown in SEM in Fig. 4, and sample topography is subsphaeroidal substantially, and size distribution is uneven, and agglomeration is obvious.
Embodiment 4
Change the content of Ce within the scope of 0.3-2.0mol%, other conditions are as embodiment 1, and the luminescent properties of gained sample as shown in Figure 5.When Ce content is 0.7mol%, sample luminescent properties is best.
Claims (1)
1. adopt reverse co-precipitation to prepare Gd
2ti
2o
7: the method for Ce nano-luminescent powder body, is characterized in that, the method adopts high-purity Gd
2o
3with relatively inexpensive and easy handling Ti (SO
4)
2as reaction raw materials, with Ce (NO
3)
3as activator, using ammoniacal liquor as precipitation agent, adopt Sodium dodecylbenzene sulfonate (SDBS) as dispersion agent; Preparation process comprises: take Gd according to precise stoichiometry ratio
2o
3, Ti (SO
4)
2with Ce (NO
3)
3, by Gd
2o
3be dissolved in excessive dilute nitric acid solution, obtain Gd (NO
3)
3solution; Again by Ti (SO
4)
2being dissolved in above-mentioned solution preparation after water-soluble becomes metal cation concentration to be female salts solution of 0.06 ~ 0.10mol/L; Take Ce
3+ce (the NO of doping content between 0.3-2.0% molar fraction
3)
3be dissolved in female salts solution being stirred well to and mix; Preparation 1 ~ 2mol/L ammoniacal liquor is precipitation agent, and the dispersion agent SDBS taking 1wt% ~ 2wt% is dissolved in precipitation agent ammoniacal liquor and stirs; Female salts solution is titrated in precipitation agent, magnetic agitation, controlling titration speed with peristaltic pump is 1 ~ 4ml/min, temperature of reaction system is 0 ~ 20 DEG C, the pH value adjusting titration end point reaction system with ammoniacal liquor is 10 ~ 12, namely the pioneer precipitate of white flock is obtained, timeliness 12h, after filtering, clean 4 times with distilled water, then use washes of absolute alcohol 2 times, removing foreign ion, then presoma is placed in dry 12 ~ 24 h of vacuum drying oven of 80 ~ 100 DEG C, put into crucible after grinding at 800 ~ 1100 DEG C of calcining 1 ~ 3h, product sieves through grinding and namely obtains Gd
2ti
2o
7: Ce nano-powder.
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| CN106495500B (en) * | 2016-09-19 | 2019-01-04 | 沈阳理工大学 | A method of preparing hollow metatitanic acid gadolinium tubular material |
| CN107955605B (en) * | 2017-11-21 | 2018-12-18 | 杭州鼎好新材料有限公司 | A kind of Gd2Ti2O7 system phosphor and preparation method thereof |
| CN114958372A (en) * | 2021-12-09 | 2022-08-30 | 营口理工学院 | Preparation of GdAlO by reverse coprecipitation technology 3 Method for preparing Ce luminescent powder |
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| US6139774A (en) * | 1996-10-03 | 2000-10-31 | Hitachi Maxell, Ltd. | Fluorescent substance |
| CN101974329A (en) * | 2010-10-08 | 2011-02-16 | 东华大学 | La2Ti2O7:Sm3+ red phosphor and preparation method thereof |
| CN102502816A (en) * | 2011-10-27 | 2012-06-20 | 沈阳化工大学 | Method for preparing Gd2Zr207 nano-powder through coprecipitation |
-
2013
- 2013-11-27 CN CN201310609795.1A patent/CN103614139B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6139774A (en) * | 1996-10-03 | 2000-10-31 | Hitachi Maxell, Ltd. | Fluorescent substance |
| CN101974329A (en) * | 2010-10-08 | 2011-02-16 | 东华大学 | La2Ti2O7:Sm3+ red phosphor and preparation method thereof |
| CN102502816A (en) * | 2011-10-27 | 2012-06-20 | 沈阳化工大学 | Method for preparing Gd2Zr207 nano-powder through coprecipitation |
Non-Patent Citations (2)
| Title |
|---|
| M.Saif.Luminescence based on energy transfer in silica doped with lanthanide titania (Gd2Ti2O7:Ln3+) [Ln3+=Eu3+ or Dy3+].《Journal of Photochemistry and Photobiology A:Chemistry》.2009,第205卷(第2-3期),第145-150页. * |
| 共沉淀法制备Gd2Zr2O7纳米粒子;李权等;《人工晶体学报》;20130131;第42卷(第1期);第72-77页 * |
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