CN1994897A - Method for preparing calcium tungstate europium-doped nano material using sodium tungstate - Google Patents
Method for preparing calcium tungstate europium-doped nano material using sodium tungstate Download PDFInfo
- Publication number
- CN1994897A CN1994897A CN 200610169550 CN200610169550A CN1994897A CN 1994897 A CN1994897 A CN 1994897A CN 200610169550 CN200610169550 CN 200610169550 CN 200610169550 A CN200610169550 A CN 200610169550A CN 1994897 A CN1994897 A CN 1994897A
- Authority
- CN
- China
- Prior art keywords
- europium
- solution
- beaker
- calcium
- nano 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.)
- Granted
Links
Images
Abstract
The invention discloses a making method of calcium tungstate with doped europium nanometer material through sodium tungstate in the inorganic chemical technical domain, which is characterized by the following: weighing 25-35ml 0.4-0.5mol/l sodium tungstate solution, 25-35ml 9%-11% ammonium citrate solution and 2. 5-3. 5g hexadecyl trimethyl-ammonium bromide as surface activator to add in the beaker sequently; stirring evenly; blending 25-30ml 0.4-0.5mol/l calcium chloride solution and 5. 5-6. 5ml 0.9-1. 1mol/l europium chloride solution; pouring compound in the separatory funnel; dripping composite solution of calcium chloride and europium chloride into beaker through separatory funnel; stirring through magnetic force; generating white sediment; fetching suspension; placing the suspension in the centrifuger; putting in the toaster to do heat disposal at 100-120 deg. c; placing the solid in the electric furnace to do heat disposal at 550-650 deg. c; grinding solid for 30-40 min to obtain the product.
Description
Technical field
The invention belongs to the inorganic chemical technology technical field, a kind of method of utilizing sodium wolframate to prepare the calcium wolframate europium-doped nano material particularly is provided, utilize pharmaceutical chemicals to prepare the calcium wolframate europium-doped nano material.
Background technology
CaWO with scheelite-type structure
4Fluor be that found in 1896 and very fast first as X ray luminous material, still using so far after experiencing a nearly century.CaWO
4Be typical self activation fluor, under X ray, electron beam and UV optical excitation, produce efficient blue light.In 70～eighties of last century, people such as Powell are once to CaWO
4And Eu
3+Adulterated CaWO
4Luminous and the transmission ofenergy of system is furtherd investigate.The most over the past two years, it is found that at some and mix Eu
3+Tungsten (molybdenum) hydrochlorate in, under nearly UV optical excitation, can produce red fluorescence efficiently, they can be as the red-emitting phosphors of white light LEDs.The happiness of little field the people such as is exerted oneself and is reported LiEuW
2O
8In mix a small amount of Sm
3+After, when the optical excitation of 400nm royal purple, efficiency of conversion is Y
2O
2S:Eu
3+More than 6 times.Wang Jiaguo etc. are to LiEuM
2O
8(M=W, Mo) the system red-emitting phosphors improves, and obtains luminous intensity height under nearly UV optical excitation, and the red-emitting phosphors of high color purity.Some Eu
3+Activated tungsten silicate red phosphor has synthesis temperature low (about 550 °～1300 ℃), the advantage that chemical property is stable.The invention provides a kind of humidifying legal system and be equipped with the method that the nanometer calcium wolframate is mixed the europium fluor.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing sodium wolframate to prepare the calcium wolframate europium-doped nano material, solved the problem of reuniting easily in the nano material preparation.
The present invention utilizes the surfactant micelle method, forms the mode of template with surfactant-dispersed in the aqueous solution, has prepared CaWO
4: Eu
3+Nano material, and inquired into the relation of its luminosity and crystalline network, finally obtain spherulitic calcium wolframate europium-doped nano particle.Concrete technology is:
1. get 25～35ml, 0.4～0.5mol/L sodium tungstate solution, the citric acid ammonia solution of 25～35ml massfraction 9%～11% and 2.5～3.5g Surfactant CTAB (cetyl trimethylammonium bromide) add in the beaker successively, mix.
2. get 25～30ml, 0.4～0.5mol/L calcium chloride solution and 5.5～6.5ml, 0.9～1.1mol/L Europium trichloride solution and mix, pour in the separating funnel.
3. calcium chloride Europium trichloride mixing solutions is slowly splashed in the beaker by the first step gained mixing solutions by separating funnel, simultaneously solution in the beaker is carried out magnetic agitation, the adularescent precipitation generates.
4. titration is finished, and continues magnetic agitation 20～40min, takes out suspension liquid then, puts into whizzer and carries out centrifugation.
5. take out centrifugal precipitation of coming out, put into 100～120 ℃ of thermal treatments of baking oven 3～5 hours, then the gained solid is put into 550～650 ℃ of thermal treatments of electric furnace 1.5～2.5 hours.
To above step gained solid abrasive 30～40min get final product the calcium wolframate europium-doped nano material.
The invention has the advantages that: method is simple, is easy to control, material settling out, and Application Areas is extensive.
Description of drawings
Fig. 1 is a spherulitic calcium wolframate europium-doped nano particulate electron micrograph of the present invention, can see less than the calcium wolframate of 100 nanometers in the photo and mix the europium particle.
Fig. 2 is the present invention
Embodiment
1. get 30ml 0.5mol/L sodium tungstate solution, the citric acid ammonia solution of 30ml massfraction 10% and 3.0g tensio-active agent (CTAB) add in the beaker successively, fully mix.
2. get 30ml 0.5mol/L calcium chloride solution and 6.0ml 0.1mol/L Europium trichloride solution and mix, pour in the separating funnel.
3. calcium chloride Europium trichloride mixing solutions is slowly splashed in the beaker by the first step gained mixing solutions by separating funnel, simultaneously solution in the beaker is carried out magnetic agitation, the adularescent precipitation generates.
4. titration is finished, and continues magnetic agitation 30min, takes out suspension liquid then, puts into whizzer and carries out centrifugation.
5. take out centrifugal precipitation of coming out, put into 110 ℃ of thermal treatments of baking oven 4 hours, then the gained solid is put into 600 ℃ of thermal treatments of electric furnace 2 hours.
To above step gained solid abrasive 30～40min get final product the calcium wolframate europium-doped nano material.
Claims (1)
1, a kind of method of utilizing sodium wolframate to prepare the calcium wolframate europium-doped nano material, it is characterized in that: technology is:
(1) get 25～35ml, 0.4～0.5mol/L sodium tungstate solution, the citric acid ammonia solution of 25～30ml massfraction 9%～11% and 2.5～3.5g tensio-active agent cetyl trimethylammonium bromide add in the beaker successively, mix;
(2) get 25～30ml, 0.4～0.5mol/L calcium chloride solution and 5.5～6.5ml, 0.9～1.1mol/L Europium trichloride solution and mix, pour in the separating funnel;
(3) calcium chloride Europium trichloride mixing solutions is slowly splashed in the beaker by the first step gained mixing solutions by separating funnel, simultaneously solution in the beaker is carried out magnetic agitation, the adularescent precipitation generates;
(4) titration is finished, and continues magnetic agitation 20～40min, takes out suspension liquid then, puts into whizzer and carries out centrifugation;
(5) take out centrifugal precipitation of coming out, put into 100～120 ℃ of thermal treatments of baking oven 3～5 hours, then the gained solid is put into 550～650 ℃ of thermal treatments of electric furnace 1.5～2.5 hours;
(6) can obtain the calcium wolframate europium-doped nano material to gained solid abrasive 30～40min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101695501A CN100418889C (en) | 2006-12-22 | 2006-12-22 | Method for preparing calcium tungstate europium-doped nano material using sodium tungstate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101695501A CN100418889C (en) | 2006-12-22 | 2006-12-22 | Method for preparing calcium tungstate europium-doped nano material using sodium tungstate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1994897A true CN1994897A (en) | 2007-07-11 |
| CN100418889C CN100418889C (en) | 2008-09-17 |
Family
ID=38250118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101695501A Expired - Fee Related CN100418889C (en) | 2006-12-22 | 2006-12-22 | Method for preparing calcium tungstate europium-doped nano material using sodium tungstate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100418889C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701282A (en) * | 2012-05-14 | 2012-10-03 | 无锡润鹏复合新材料有限公司 | Preparation method of CaWO4 hollow spheres |
| CN103318905A (en) * | 2013-07-03 | 2013-09-25 | 北京科技大学 | Method for preparing granular chambersite nanometer material by using sodium borate |
| CN113201392A (en) * | 2021-04-30 | 2021-08-03 | 南京工程学院 | Functional lubricant for surface processing of steel plate strip, preparation method and online detection system |
| CN113713812A (en) * | 2021-08-06 | 2021-11-30 | 中国科学院海洋研究所 | Visible light response Pt/WO3Use of optical materials |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005179498A (en) * | 2003-12-19 | 2005-07-07 | Nec Lighting Ltd | Red phosphor material, white light-emitting diode using the same, and illuminator using the white light-emitting diode |
-
2006
- 2006-12-22 CN CNB2006101695501A patent/CN100418889C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701282A (en) * | 2012-05-14 | 2012-10-03 | 无锡润鹏复合新材料有限公司 | Preparation method of CaWO4 hollow spheres |
| CN102701282B (en) * | 2012-05-14 | 2015-05-20 | 无锡润鹏复合新材料有限公司 | Preparation method of CaWO4 hollow spheres |
| CN103318905A (en) * | 2013-07-03 | 2013-09-25 | 北京科技大学 | Method for preparing granular chambersite nanometer material by using sodium borate |
| CN103318905B (en) * | 2013-07-03 | 2014-12-10 | 北京科技大学 | Method for preparing granular chambersite nanometer material by using sodium borate |
| CN113201392A (en) * | 2021-04-30 | 2021-08-03 | 南京工程学院 | Functional lubricant for surface processing of steel plate strip, preparation method and online detection system |
| CN113713812A (en) * | 2021-08-06 | 2021-11-30 | 中国科学院海洋研究所 | Visible light response Pt/WO3Use of optical materials |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100418889C (en) | 2008-09-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Two-phase solvothermal synthesis of rare-earth doped NaYF4 upconversion fluorescent nanocrystals | |
| Liu et al. | Enhanced photocatalytic mechanism of the Nd-Er co-doped tetragonal BiVO4 photocatalysts | |
| CN105062485B (en) | Nano/micron crystal preparation method is changed on gadolinium ion doping fluorination lutetium sodium | |
| CN100418889C (en) | Method for preparing calcium tungstate europium-doped nano material using sodium tungstate | |
| CN112080278B (en) | Up/down conversion dual-mode luminescent nanocrystal and preparation method and application thereof | |
| WO2019024523A1 (en) | Preparation method for thin film capable of improving up-conversion luminescence | |
| CN112940726B (en) | Blue-violet and near-infrared two-region dual-mode luminescent nanocrystal and preparation method thereof | |
| CN106566536A (en) | Red light-blue light dual-emission composited optical transfer material, and preparation method and application of red light-blue light dual-emission composited optical transfer material | |
| CN109825288A (en) | A kind of red solid fluorescent carbon point and its preparation method and application | |
| CN106350057A (en) | Preparation method of fluorescent hybrid nanoparticles | |
| CN101966978A (en) | Method for preparing multi-metal-oxygen cluster-doped silicon dioxide nanoparticles | |
| CN103468266A (en) | Preparation method of water-soluble upconversion fluorescence nano material | |
| CN103275715B (en) | Preparation method of rare earth molybdate matrix red nanophosphor | |
| CN109504381A (en) | The method of microwave and the double outfield auxiliary liquid phase synthesis bismuth europium codope molybdate red phosphors of ultrasonic wave | |
| CN104610965A (en) | Preparation method of spherical fluorescent powder | |
| Liu et al. | Facile synthesis and multicolor luminescence properties of Gd4O3F6: Ln3+ (Ln= Eu, Tb, Dy, Sm, Ho, Tm, Yb/Er, Yb/Ho) microcrystals | |
| CN104498036B (en) | A kind of one-dimensional rod-like rare-earth-dopping yttrium aluminum garnet luminescent material and its preparation method and application | |
| CN103589418B (en) | A kind of preparation method of water-soluble upconversion fluorescence nano material | |
| CN103599801A (en) | Silver-phosphate-based composite visible light photocatalytic material and preparation method thereof | |
| CN1994898B (en) | Method for preparing linear calcium tungstate europium-doped nano material using ammonium tungstate | |
| CN106010526A (en) | Method for preparing molybdate nanometer microparticles by using different surfactants | |
| CN106590631A (en) | Rare earth doped nanometer calcium citrate fluorescent powder and preparation method thereof | |
| Tang et al. | Improving Upconversion Luminescence by Coating Active Shell: A Case Study on NaYF4: Gd, Yb, Er@ NaYF4: Yb, Pr | |
| CN103409138A (en) | Preparation method of CNTs (Carbon Nano Tubes) used on PDP (Plasma Display Panel) and mixed with fluorescent powder | |
| CN101391795B (en) | Method for preparing down-conversion fluorescent substrate material gadolinium sodium fluoride nanocrystalline |
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 | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080917 Termination date: 20101222 |