CN102031108A - Method for preparing barium zirconate cerium-doped BaZrO3:Ce nano luminescent material by microemulsion method - Google Patents
Method for preparing barium zirconate cerium-doped BaZrO3:Ce nano luminescent material by microemulsion method Download PDFInfo
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- CN102031108A CN102031108A CN2010105554034A CN201010555403A CN102031108A CN 102031108 A CN102031108 A CN 102031108A CN 2010105554034 A CN2010105554034 A CN 2010105554034A CN 201010555403 A CN201010555403 A CN 201010555403A CN 102031108 A CN102031108 A CN 102031108A
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Abstract
The invention discloses a method for preparing a barium zirconate cerium-doped BaZrO3:Ce nano luminescent material by a microemulsion method, relating to a preparing method of fluorescent powder. In the method, cyclohexane is adopted as an oil phase, cetyl trimethyl ammonium bromide (CATB) is adopted as a surfactant, and n-butyl alcohol is adopted as a cosurfactant. The method comprises the following steps of: preparing an initial rare earth solution and a microemulsion, mixing, leaching, washing, drying, calcining a precursor, wherein the initial concentration range of the rare earth solution is 0.2mol/L. In the preparation process, the crystal form, the appearance and the size of the product are controlled by regulating the proportions of the raw materials, or adding an auxiliary dispersant, or changing the concentration of the initial solution. The precursor is thermally preserved for 3h at the lower calcination temperature (900 DEG C) to obtain a BazerO3:Ce sample with approximately spherical appearance and good dispersibility. The material of the invention can be applied to the fields of high-energy physics and nuclear medicine imaging.
Description
Technical field
The present invention relates to a kind of preparation method of fluorescent material, particularly relate to a kind of microemulsion method and prepare barium zirconate and mix BaZrO
3: the method for Ce nano luminescent material.
Background technology
Scintillator is a kind ofly can absorb energetic ray (x ray, gamma-rays) or high energy particle effectively, and the functional materials of emission UV-light or visible light.Scintillator is mainly used in high energy physics and nuclear medicine field.Scintillator material is divided into inorganic and organic two classes.Organic scintillator belongs to the aromatic hydrocarbons of benzene ring structure mostly, and inorganic scintillator is divided into scintillation single crystal, ceramic scintillator and scintillation glass.Cheap, the easy cutting of ceramic scintillator preparation cost, synthetic powder technology is simple relatively, can realize that the even doping of molecular atoms level has been Future Development trend.The metallic compound material system of isometric system obtained the extensive concern of Chinese scholars, (Sr in recent years; Ba; Ca) HfO
3: Ce and (Sr:Ba; Ca) ZrO
3: Ce has different reports as the document of scintillation material, and target is to solve the synthetic problem with technology of preparing of ceramic flashing material, and becomes one of research focus of field of new.
BaZrO
3And rare earth doped BaZrO
3The preparation method comprise: solid phase method, the precipitator method, sol-gel method, hydrothermal method etc.The sintering temperature height (1200-1700 ℃) and the product size distribution is inhomogeneous, purity is low though solid phase method technology is simple; Wet chemistry method (precipitator method, sol-gel method) is though can effectively improve the performance of material, and impurity is easily reunited, easily introduced to product; Though hydrothermal method product good dispersity, purity height are to equipment requirements height, poor stability.Compare with above-mentioned preparation method, microemulsion method has that preparation technology is simple, sample narrow diameter distribution, sample particle size and pattern is controlled, can realize molecular level even doping, introduce unique advantages such as impurity is few, make its synthetic field that huge application potential be arranged in nano material.
Summary of the invention
The object of the present invention is to provide a kind of anti-phase couple of micro-emulsion method for preparing nano BaZrO
3: the method for Ce luminescent material, the employing hexanaphthene is an oil phase, and cetyl trimethylammonium bromide (CTAB) is a tensio-active agent, and propyl carbinol is that cosurfactant is made into microemulsion and prepares BaZrO
3: the Ce luminescent material.The BaZrO of this method preparation
3: Ce sample luminescent properties improves, and good dispersity, particle diameter are even, have realized the particle diameter and the pattern of sample controlled.
The objective of the invention is to be achieved through the following technical solutions:
Microemulsion method prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material, it is oil phase that this method adopts hexanaphthene, and cetyl trimethylammonium bromide (CATB) is a tensio-active agent, and propyl carbinol is a cosurfactant; The process of preparation comprises the calcination process of configuration, mixing, suction filtration, washing, drying and presoma of configuration, the microemulsion of initial earth solution; The starting point concentration scope of earth solution is at 0.2mol/L.
Described microemulsion method prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material, the tensio-active agent of described employing and the mass ratio of oil phase are 1:3, the mass ratio of tensio-active agent and cosurfactant is 2:5.
Described microemulsion method prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material, the mixed system temperature of reaction of microemulsion is controlled at 0-75 ℃; Drying temperature is controlled at 80-100 ℃.
Described microemulsion method prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material, presoma incinerating temperature range is controlled between 500-1000 ℃.
Described microemulsion method prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material, BaZrO
3: the atom content of Ce is between the 0.1-1.1% molar fraction in the Ce nano-powder.
Advantage of the present invention and effect are:
Raw materials cost of the present invention is low, and waste liquid easily reclaims, and it is few to introduce impurity, and technology is simple, and is easy and simple to handle, and preparation cycle is short.In preparation process, or by the adjusting proportion of raw materials, or add a kind of auxiliary dispersants, or the concentration of change initial soln is controlled crystal formation, pattern and the size of product.Presoma is incubated the BaZrO that 3h obtains down in low calcining temperature (900 ℃)
3: the Ce sample, pattern is subsphaeroidal, and good dispersity, particle diameter evenly are about 20nm.This BaZrO
3: the Ce sample preparation methods holds out broad prospects in actual applications.
Description of drawings
Fig. 1 is for adding polyvinyl alcohol pyridine alkane ketone 0%(massfraction), the SEM figure of the sample that behind 900 ℃ of calcining 3h, obtains;
Fig. 2 is for adding polyvinyl alcohol pyridine alkane ketone 1% (massfraction), the SEM figure of the sample that obtains behind 900 ℃ of calcining 3h;
Fig. 3 is for adding polyvinyl alcohol pyridine alkane ketone 2% (massfraction), the SEM figure of the sample that obtains behind 900 ℃ of calcining 3h;
Fig. 4 is for adding polyvinyl alcohol pyridine alkane ketone 3% (massfraction), the SEM figure of the sample that obtains behind 900 ℃ of calcining 3h;
Fig. 5 is various ce contents (a 0.1-1.1 %(molar fraction)) BaZrO
3: Ce sample luminescent properties is relatively.
Annotate: Fig. 1-Fig. 5 of the present invention is the analysis synoptic diagram or the photo of product state, the unintelligible understanding that does not influence technical solution of the present invention of literal or image among the figure.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
Material selection of the present invention:
Raw material nitrate of baryta, nitric acid oxidation zirconium, cerous nitrate, cetyl trimethylammonium bromide CTAB, polyvinyl alcohol pyridine alkane ketone, oxalic acid, hexanaphthene, propyl carbinol and ethanol etc. are analytical reagent, and distilled water is secondary water.Above reagent does not all pass through purification process.
Preparation process of the present invention:
Raw material nitrate of baryta, nitric acid oxidation zirconium dissolved in distilled water are made into the initial soln that concentration is 0.2mol/L.The hexanaphthene of getting 100ml adds the cetyl trimethylammonium bromide of 7.451g and the propyl carbinol of 22.9ml, adds the earth solution of 8.9ml initial soln and different volumes under the powerful stirring of magnetic stirring apparatus, obtains transparent micro emulsion A behind the 20min.The 2mol/L oxalic acid solution is made into microemulsion B according to aforesaid operations, under the state that stirs, microemulsion A is added drop-wise among the microemulsion B, with splashing into of microemulsion A, constantly generate white gelatinous precipitate in the solution, sustained reaction 60min, forerunner's throw out is through ageing, absolute ethanol washing, suction filtration, dry 24h under 80 ℃ obtains presoma in vacuum drying oven.Precursor powder ground to sieve to be placed in the corundum crucible in retort furnace, in 500-1000 ℃ of scope, obtain BaZrO behind the calcining 3h
3: the Ce sample.
Embodiment 1
According to preparation process, add 100ml hexanaphthene, 7.415g CATB, 22.9ml propyl carbinol in the beaker of 400ml, magnetic stirring apparatus is powerful to be stirred, and adds the earth solution of the 0.2mol/L of 8.9ml simultaneously, solution becomes is transparent behind the 20min, obtains stable microemulsion liquid system (being designated as A).Get the hexanaphthene of same amount, CATB and propyl carbinol add 1.0mol/L oxalic acid solution 4.5ml in the time of stirring in another 400ml beaker, constantly stir and obtain transparent micro emulsion (being designated as B).Constantly under the condition of stirring, A solution is added in the B solution, occur muddy after for some time, behind the reaction 60min, use the vacuum pump suction filtration, absolute ethanol washing repeatedly is placed in the vacuum drying oven through suction filtration again and obtains the presoma powder behind 80 ℃ of dry 24h, obtains sample through 900 ℃ of calcinings again after powder is milled and sieved.The sample that calcining under the differing temps is obtained down carries out XRD analysis, and the TG/DTA heat of comprehensive presoma powder is analyzed, and determines calcining temperature.Pattern to the sample of gained carries out sem analysis, and the sample particle size is obtained by the ImgineJ software analysis.The gained sample shape is irregular, and size is about 30nm, as shown in Figure 1.
Add polyvinyl alcohol pyridine 1%(massfraction), other conditions such as embodiment 1, the pattern of gained sample as shown in Figure 2, sample topography is a polyhedron substantially, particle diameter is about 28nm.
Add polyvinyl alcohol pyridine 2% (massfraction), other conditions such as embodiment 1, the pattern of gained sample are shown in SEM among Fig. 3, and sample topography is subsphaeroidal substantially, and particle diameter is about 25nm, and sample dispersion is better.
Add polyvinyl alcohol pyridine 3%(massfraction), other conditions such as embodiment 1, the pattern of gained sample as shown in Figure 4, sample topography be sphere substantially, particle diameter is about 20nm, sample dispersion is good.
Embodiment 5
The content that changes Ce is in the 0.1-1.1%(molar fraction) in the scope, other conditions such as embodiment 1, the luminescent properties of gained sample is as shown in Figure 5.When Ce content is 0.7%, sample luminescent properties the best.
Claims (5)
1. microemulsion method prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material, it is characterized in that it is oil phase that this method adopts hexanaphthene, cetyl trimethylammonium bromide (CATB) is a tensio-active agent, propyl carbinol is a cosurfactant; The process of preparation comprises the calcination process of configuration, mixing, suction filtration, washing, drying and presoma of configuration, the microemulsion of initial earth solution; The starting point concentration scope of earth solution is at 0.2mol/L.
2. microemulsion method according to claim 1 prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material, it is characterized in that the tensio-active agent of described employing and the mass ratio of oil phase are 1:3, the mass ratio of tensio-active agent and cosurfactant is 2:5.
3. microemulsion method according to claim 1 prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material is characterized in that the mixed system temperature of reaction of microemulsion is controlled at 0-75 ℃; Drying temperature is controlled at 80-100 ℃.
4. microemulsion method according to claim 1 prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material is characterized in that presoma incinerating temperature range is controlled between 500-1000 ℃.
5. microemulsion method according to claim 1 prepares barium zirconate and mixes cerium BaZrO
3: the method for Ce nano luminescent material is characterized in that BaZrO
3: the atom content of Ce is between the 0.1-1.1% molar fraction in the Ce nano-powder.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109022837A (en) * | 2018-08-31 | 2018-12-18 | 内蒙古科技大学 | The method for preparing rodlike rare earth oxalate powder based on reverse microemulsion process |
| US10344209B2 (en) * | 2015-08-07 | 2019-07-09 | Boe Technology Group Co., Ltd. | White-light fluorescent material, and manufacturing method and use thereof |
| CN116251562A (en) * | 2023-02-10 | 2023-06-13 | 广州市汉宵科研技术有限公司 | Nanoscale cerium oxide particle material and preparation method thereof |
Citations (3)
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| CN1719641A (en) * | 2005-06-17 | 2006-01-11 | 桂林工学院 | Process for preparing electrochemical active nano-powder material of doped non-crystalline nickel hydroxide |
| CN101077974A (en) * | 2007-07-05 | 2007-11-28 | 清华大学 | Method of preparing nano-level sphere cerium activated yttrium aluminum garnet phosphor powder |
| CN101260299A (en) * | 2008-04-03 | 2008-09-10 | 沈阳化工学院 | Method for preparing yttrium gadolinium oxide and europium nano luminescent powder by micro-emulsion method |
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- 2010-11-23 CN CN2010105554034A patent/CN102031108A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1719641A (en) * | 2005-06-17 | 2006-01-11 | 桂林工学院 | Process for preparing electrochemical active nano-powder material of doped non-crystalline nickel hydroxide |
| CN101077974A (en) * | 2007-07-05 | 2007-11-28 | 清华大学 | Method of preparing nano-level sphere cerium activated yttrium aluminum garnet phosphor powder |
| CN101260299A (en) * | 2008-04-03 | 2008-09-10 | 沈阳化工学院 | Method for preparing yttrium gadolinium oxide and europium nano luminescent powder by micro-emulsion method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10344209B2 (en) * | 2015-08-07 | 2019-07-09 | Boe Technology Group Co., Ltd. | White-light fluorescent material, and manufacturing method and use thereof |
| CN109022837A (en) * | 2018-08-31 | 2018-12-18 | 内蒙古科技大学 | The method for preparing rodlike rare earth oxalate powder based on reverse microemulsion process |
| CN116251562A (en) * | 2023-02-10 | 2023-06-13 | 广州市汉宵科研技术有限公司 | Nanoscale cerium oxide particle material and preparation method thereof |
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Application publication date: 20110427 |