CN104445392B - A kind of hydro-thermal solvent method prepares BaZrO3: the method for (Ce, Pr) nano-powder - Google Patents
A kind of hydro-thermal solvent method prepares BaZrO3: the method for (Ce, Pr) nano-powder Download PDFInfo
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- CN104445392B CN104445392B CN201410607343.4A CN201410607343A CN104445392B CN 104445392 B CN104445392 B CN 104445392B CN 201410607343 A CN201410607343 A CN 201410607343A CN 104445392 B CN104445392 B CN 104445392B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
A kind of hydro-thermal solvent method prepares BaZrO3: the method for (Ce, Pr) nano-powder, relate to a kind of method preparing nano-powder, the method step is: weigh a certain amount of Ba (NO by accurate stoichiometric proportion3)2、ZrOCl2·8H2O、Ce(NO3)3、Pr(NO3)3It is dissolved in alcohol-water solution (ratio of second alcohol and water is 1:1 ~ 4:1), is configured to the metal salt solution that concentration is 0.01 ~ 1mol/L；Using concentration is that the KOH of 2mol/L is as mineralizer；After being added drop-wise to mineralizer in metal salt solution stir 1h, it is loaded in reactor, then still is put in microwave oven, react under suitable conditions, be precipitated thing.Through timeliness, precipitate is filtered, washing, grind, sieve and obtain sample.The BaZrO that the present invention obtains3: (Ce, Pr) powder dispersity is good, uniform particle sizes, and technique is simple, and the cycle is short, low cost, is suitable to batch production.
Description
Technical field
The present invention relates to a kind of method preparing nano-powder, particularly relate to a kind of hydro-thermal solvent method and prepare BaZrO3: the method for (Ce, Pr) nano-powder.
Background technology
Scintillator is important optical function material, is mainly used in the field such as high-energy physics and nuclear medicine, including inorganic scintillation crystal and Inorganic scintillation pottery.The metal compound material system of perovskite structure obtained the extensive concern of Chinese scholars, (Sr in recent years;Ba;Ca)HfO3: Ce and (Sr:Ba;Ca)ZrO3: Ce has different report as the document of scintillation material.One of the problem aiming at solution ceramic scintillation materials synthesis and technology of preparing, and the study hotspot becoming field of new.Alkaline earth BaZrO3As the compound of a kind of perovskite structure, high (the 5.42g/ cm of density3), atomic number is big, has excellent electrically and thermally performance, and adulterate Pr3+、Ce3 +BaZrO3Material has higher absorbability, simultaneously Pr to high-energy ray or high energy particle3+、Ce3+(4f1) optics electronegativity is little, can realize the complete transition of 5d-4f, < feature request of 100ns is the candidate material preparing scintillating ceramic to meet scintillator decay of luminescence.
Prepare BaZrO both at home and abroad at present3And rare earth doped BaZrO3Preparation method include solid phase method, sol-gal process, coprecipitation etc..In above-mentioned synthesis method, solid phase method technique is simple but sintering temperature high and particle size skewness, purity are low.The powder granule of sol-gal process synthesis is big, it is serious to reunite.Hydro-thermal method product good dispersion, purity are high, but high to equipment requirements, and cost is high, yields poorly, is not suitable for industrialized production.Compared to the above, hydro-thermal method is prepared powder body and is had plurality of advantages, the reactive component mixing of hydro-thermal method is molecule, atom level, product reaches nanoscale, can realize ion doping uniformly, doping scope is wide, product purity is high, uniform particle sizes, technique is simple, is a kind of component with low cost, each synthetic method of being accurately controlled, being easily achieved industrialization.
Summary of the invention
It is an object of the invention to provide a kind of hydro-thermal solvent method and prepare BaZrO3: the method for (Ce, Pr) nano-powder, the method forms pure crystalline phase BaZrO3: (Ce, Pr), crystallization temperature is low, without dephasign, better crystallinity degree, cost of material is low, preparation technology is simple, the cycle is short, is suitable for batch production.
It is an object of the invention to be achieved through the following technical solutions:
A kind of hydro-thermal solvent method prepares BaZrO3: the method for (Ce, Pr) nano-powder, described method includes following preparation process:
1), the configuration of solution: weigh Ba (NO by accurate stoichiometric proportion3)2、ZrOCl2·8H2O、Ce(NO3)3、Pr(NO3)3And be dissolved in alcohol-water solution, it is configured to metal salt solution；KOH is diluted to mineralizer；
2), the preparation of presoma: above-mentioned mineralizer is added drop-wise in the metal salt solution configured, after stirring, reactant is loaded in reactor, then reactor is put in microwave oven and react；The precursor precipitate obtained, through timeliness, cleans, sucking filtration, dries and obtains powder sample.
Described a kind of hydro-thermal solvent method prepares BaZrO3: the method for (Ce, Pr) nano-powder, described Ce3+Doping content 0.2mol% ~ 1.0mol%, Ce3+、Pr3+Mole doping content than for 1:0 ~ 1:7.
Described a kind of hydro-thermal solvent method prepares BaZrO3: the method for (Ce, Pr) nano-powder, described alcohol-water is than for 1:1 ~ 4:1, and the initial concentration of metal salt solution is 0.01 ~ 1mol/L.
Described a kind of hydro-thermal solvent method prepares BaZrO3: the method for (Ce, Pr) nano-powder, the PH of the completely rear regulation system of described precipitation is 8 ~ 14, and reaction temperature and time are respectively 120 ~ 240 DEG C and 12 ~ 24 h.
Advantages of the present invention with effect is:
1, the present invention can form pure crystalline phase BaZrO3: (Ce, Pr), crystallization temperature is low, without dephasign, better crystallinity degree.
2, cost of material of the present invention is low, and preparation technology is simple, and the cycle is short, has broad application prospects, and is suitable for batch production.
Accompanying drawing explanation
Fig. 1 is BaZrO3The SEM pattern of powder body.Can be seen that powder dispersity is good, almost spherical；
Fig. 2 Ce3+The doping content impact on powder body luminescent properties, work as Ce3+When doping content is 0.4mol%, the luminescent properties of powder body is the strongest；
Fig. 3 Ce3+、Pr 3+The impact of doping molar concentration comparison powder body luminescent properties, it is seen that add Pr 3+After, powder body luminescent properties strengthens, optimal Ce3+、Pr 3+Doping molar concentration rate is 1:3.
Detailed description of the invention
Illustrated embodiment below in conjunction with the accompanying drawings, the invention will be further described.
Embodiment 1:
Ba (NO3)2、ZrOCl2·8H2O mixes and is dissolved in alcohol-water solution (second alcohol and water ratio is 3:1), is made into 0.2 mol/L metal salt solution.It is the mineralizer of 3mol/L by KOH diluted concentration.Then mineralizer is instilled in the metal salt solution prepared, until pH=14, and by magnetic stirrer, titrate end and be loaded in reactor, then reactor is put in microwave oven, react under suitable condition (temperature, time, pH etc.).After reaction, through timeliness, being cleaned three times by the precipitate distilled water generated, detecting filtrate with silver nitrate, until existing without chloride ion, then washing twice with dehydrated alcohol, being placed in temperature is to be dried 24h in 80 DEG C of drying baker, grinds, obtains good dispersion, subglobose BaZrO3Powder body.
Embodiment 2:
Ba (NO3)2、ZrOCl2·8H2O and different amounts of Ce (NO3)3Mix and be dissolved in alcohol-water solution (second alcohol and water ratio is 3:1), being made into 0.2 mol/L metal salt solution.It is the mineralizer of 3mol/L by KOH diluted concentration.Then mineralizer is instilled in the metal salt solution prepared, until pH=14, and by magnetic stirrer, titrate end and be loaded in reactor, then reactor is put in microwave oven, react under suitable condition (temperature, time, pH etc.).After reaction, through timeliness, the precipitate distilled water generated is cleaned three times, detecting filtrate with silver nitrate, until existing without chloride ion, then washing twice with dehydrated alcohol, being placed in temperature is to be dried 24h in 80 DEG C of drying baker, grinds, obtains good dispersion, subglobose BaZrO3: Ce powder body.
Embodiment 3:
Ba (NO3)2、 ZrOCl2·8H2O and different amounts of Pr (NO3)3、Ce(NO3)3And it is dissolved in alcohol-water solution (second alcohol and water ratio is 3:1), it is made into 0.2 mol/L metal salt solution.It is the mineralizer of 3mol/L by KOH diluted concentration.Then mineralizer is instilled in the metal salt solution that prepared, until PH=14, and by magnetic stirrer, titration end is loaded in reactor,, then reactor is put in microwave oven, reacts under suitable condition (temperature, time, pH etc.).After reaction, after timeliness, it is thus achieved that precipitate clean three times with distilled water, detecting filtrate with silver nitrate, until existing without chloride ion, then washing twice with dehydrated alcohol, being placed in temperature is to be dried 24h in 80 DEG C of drying baker, grinds, obtains good dispersion, subglobose BaZrO3: (Ce, Pr) powder body.
Claims (1)
1. a hydro-thermal solvent method prepares the BaZrO that Ce, Pr adulterate3The method of nano-powder, it is characterised in that described method includes following preparation process:
1), the preparation of solution: weigh Ba (NO by accurate stoichiometric proportion3)2、ZrOCl2·8H2O、Ce(NO3)3、Pr(NO3)3And be dissolved in alcohol-water solution, it is configured to metal salt solution；KOH is diluted to mineralizer；
2), the preparation of presoma: above-mentioned mineralizer is added drop-wise in the metal salt solution prepared, after stirring, reactant is loaded in reactor, then reactor is put in microwave oven and react；The precursor precipitate obtained, through timeliness, cleans, sucking filtration, dries and obtains powder sample；
Wherein Ce3+Doping content 0.2mol% ~ 1.0mol%
, Ce3+、Pr3+Mole doping content than for 1:0 ~ 1:7；Alcohol-water is than for 1:1 ~ 4:1, and the initial concentration of metal salt solution is 0.01 ~ 1mol/L；The pH of the rear regulation system of precipitation is 8 ~ 14, and reaction temperature and time are respectively 120 ~ 240 DEG C and 12 ~ 24 h.
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