CN108485656B - X-ray imaging material - Google Patents

X-ray imaging material Download PDF

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CN108485656B
CN108485656B CN201810203831.7A CN201810203831A CN108485656B CN 108485656 B CN108485656 B CN 108485656B CN 201810203831 A CN201810203831 A CN 201810203831A CN 108485656 B CN108485656 B CN 108485656B
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ray imaging
reaction
cosolvent
matrix material
reaction kettle
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CN108485656A (en
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郭素文
陈磊
郑岩
姚静
侯成义
刘洁
何文
张瑞君
宋长波
戚佳斌
范宏伟
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Shanghai Keyan Phosphor Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/779—Halogenides
    • C09K11/7791—Halogenides with alkali or alkaline earth metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Biophysics (AREA)
  • Optics & Photonics (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention relates to a high-precision X-ray imaging material, which comprises a matrix material BaFCl, a main activator containing Eu, a co-activator containing Ce, Sm, Gd, Dy and Tb, and K+And NH4 +The cosolvent of halogen compound of (1), characterized by taking NH as the raw material4And F is used as a complexing agent, a precursor BaFCl matrix material is prepared by adopting a coprecipitation method, then the activating agent, the cosolvent and the matrix material are uniformly mixed, sodium borohydride is used as a reducing agent to be stirred in a reaction kettle at a constant temperature, the reaction kettle is placed in a microwave reactor after being uniformly stirred, oxidized substances on the surface are removed under an ultraviolet lamp after the reaction is finished, and then the white material is obtained after water washing treatment, wherein the particle size distribution is 50-100 nm.

Description

X-ray imaging material
Technical Field
The invention belongs to a luminescent material preparation technology in the field of light excitation luminescence.
Background
Eu, an important light-excited luminescent material and X-ray image storage material, has received high attention at home and abroad due to its broad prospects in the fields of medical treatment, industrial flaw detection and the like. The so-called Photo2stimulated Luminescence (PSL) is that when X-ray is irradiated, a large amount of free electrons are generated in the material, and part of the electrons are captured by traps in the material to form color centers, so that irradiated energy is stored, when another light is irradiated, the electrons in the color centers are stimulated to be compounded with the Luminescence centers to generate light-stimulated Luminescence, so that the previously stored energy is released, and meanwhile, the rare earth doped barium chlorofluoride has important application value in the fields of optical storage, biological characterization, X-ray intensifying screen, quantum cutting and the like.
Chinese patent CN102260497A (application number: 201110122978.1) discloses a water-soluble rare earth doped barium chlorofluoride nano luminescent material with functionalized surface carboxylic acid and a preparation method thereof, relating to the preparation of the water-soluble nano luminescent material with functionalized surface. PAA is used as a surfactant, and the water-soluble rare earth doped barium chlorofluoride nano luminescent material with functionalized surface carboxylic acid is prepared by one-step reaction. The method prepares the barium chlorofluoride material with uniformly distributed particles, but the intermediate product is more complex due to the use of a large amount of organic solvent in the synthesis process, and the surface performance of the obtained barium chlorofluoride nano material is unstable. Chinese patent CN101747898B (application No. 200810072287.3) discloses a preparation method of trivalent europium doped barium chlorofluoride nano luminescent material, which comprises the steps of forming suspension of europium chloride and barium chloride in ethanol; dissolving ammonium fluoride in a small amount of water, adding a large amount of ethanol to obtain a transparent ammonium fluoride aqueous alcohol solution, and reacting in an autoclave to obtain white powder, namely the Eu: BaFCl nanocrystal. The material obtained by the method has small granularity and uniform distribution, but a large amount of ethanol solvent is used in the synthesis process, so that the potential safety hazard is large, and the luminous efficiency of the obtained material is low.
The invention discloses an X-ray imaging material, which is characterized in that a precursor is prepared by adding an activating agent and a cosolvent into a matrix material, sodium borohydride is used as a reducing agent to be stirred in a reaction kettle at a constant temperature, the reaction kettle is placed in a microwave reactor after being stirred uniformly, and barium fluochloride nano-particles with uniform particle size distribution are prepared; the material prepared by the invention has high luminous efficiency and stable performance, and is not easy to age in the using process.
The X-ray imaging material has the characteristics of high efficiency, stability, no toxicity, environmental protection, low cost, simple synthesis process and the like. The method can be widely applied to the fields of biological characterization, X-ray image materials, optical information storage materials and quantum cutting.
Disclosure of Invention
The invention relates to an X-ray imaging material, which comprises a matrix material BaFCl, a main activator containing Eu, a coactivator containing Ce, Sm, Gd, Dy and Tb, and a coactivator containing K+And NH4 +The cosolvent of halogen compound of (1), characterized by taking NH as the raw material4And F is used as a complexing agent, a precursor BaFCl matrix material is prepared by adopting a coprecipitation method, then the activating agent, the cosolvent and the matrix material are uniformly mixed, sodium borohydride is used as a reducing agent to be stirred in a reaction kettle at a constant temperature, the reaction kettle is placed in a microwave reactor after being uniformly stirred, oxidized substances on the surface are removed under an ultraviolet lamp after the reaction is finished, and then the white material is obtained after water washing treatment, wherein the particle size distribution is 50-100 nm.
The BaFCl as the matrix material is prepared by dissolving barium chloride containing crystal water in deionized water to prepare 10-15% concentration water solution and adding NH4F is used as a complexing agent and is dissolved in deionized water to prepare a 3-5% aqueous solution; according to the metering ratio of 10:1, dropwise adding a complexing agent into the barium chloride aqueous solution at the speed of 50-100ml/min, stirring for reaction, and drying to obtain the matrix material.
The main activator Eu in the invention is EuCl3，EuF3,Eu2O3And Eu (NO)3）30.5-1% by mass of one or more of the above-mentioned components. The coactivator in the invention is CeO2，Sm2O3GdO and Dy2O3Is added into the matrix material according to the mass ratio of 0.1-0.3%. The cosolvent in the invention is KCl, K2CO3，(NH4)2CO3，NH4F and NH4And one or more of Cl is added into the matrix material according to the mass ratio of 5-10%.
In the invention, the matrix material, the activating agent and the cosolvent are uniformly mixed according to a proportion and then are added into a reaction kettle, sodium borohydride is added as a reducing agent after uniform stirring, the reaction kettle is placed into a microwave reactor after uniform stirring, synthesis is carried out at the temperature of 100 ℃ and 300 ℃, and the reaction time is 3-5 hours.
According to the invention, oxidized materials on the surface of the materials obtained by reaction are removed by an ultraviolet lamp, then the powder materials obtained by grinding are dispersed in an ethanol solution, ball milling and dispersion are carried out, and after dispersion is finished, the target materials are obtained by drying after centrifugal water washing, so that the luminous efficiency of the materials is improved by 2-3 times.
The matrix material BaFCl in the invention is BaCl2 。2H2Dissolving O in deionized water, filtering, purifying to obtain water solution containing NH4F is taken as a complexing agent, and is dissolved in deionized water and then is filtered to prepare a complexing agent solution with a certain concentration; mixing complexing agent and BaCl according to a certain mass ratio2 。2H2Stirring the O aqueous solution for reaction to obtain a white precipitate after the reaction is finished, and then centrifuging and washing with water. Drying to obtain the matrix material.
Firstly, weighing a cosolvent according to a certain proportion, placing the weighed cosolvent into a watch glass, adding deionized water to dissolve the cosolvent to form a water solution, then adding a matrix material, and uniformly stirring; and then dissolving, filtering and purifying the main activator and the co-activator to prepare a water solution with a certain concentration, adding the activators into a watch glass according to a certain proportion, uniformly mixing, and placing in an oven for drying to form the precursor material.
The preparation method comprises the steps of grinding a dried precursor uniformly, then putting the precursor into a reaction kettle, adding a certain amount of deionized water to disperse the precursor into a uniform solution, then adding a certain proportion of sodium borohydride serving as a reducing agent, stirring the solution uniformly after dissolution, putting the solution into a microwave reactor, quickly cooling the solution at room temperature after reaction, pouring out supernatant after cooling and standing the solution, then carrying out powder selection treatment under an ultraviolet lamp, removing oxidized substances on the surface of the material, dispersing the material into an ethanol solution for ball milling and dispersion, obtaining a solid material in a centrifugal mode after dispersion is finished, and drying the centrifuged material in an oven to obtain the required material.
The BaFCl as the matrix material is prepared with barium chloride containing crystal water as material and through dissolving in deionized water to prepare 10-15% concentration water solution and adding NH4F is used as a complexing agent and is dissolved in deionized water to prepare a 3-5% aqueous solution; according to the metering ratio of 10:1, dropwise adding a complexing agent into the barium chloride aqueous solution at the speed of 50-100ml/min, stirring for reaction, and drying to obtain the matrix material. The main activator Eu is EuCl3，EuF3,Eu2O3And Eu (NO)3）30.5-1% by mass of one or more of the above-mentioned components. The co-activator is CeO2，Sm2O3GdO and Dy2O3Is added into the matrix material according to the mass ratio of 0.1-0.3%. Cosolvent is KCl, K2CO3，(NH4)2CO3，NH4F and NH4And one or more of Cl is added into the matrix material according to the mass ratio of 5-10%. Uniformly mixing a matrix material, an activating agent and a cosolvent according to a ratio, adding the mixture into a reaction kettle, uniformly stirring, adding sodium borohydride serving as a reducing agent, uniformly stirring, placing the reaction kettle into a microwave reactor, and synthesizing at the temperature of 100-300 ℃ for 3-5 hours. Removing oxidized materials on the surface of the materials obtained by reaction by an ultraviolet lamp, dispersing the powder materials obtained by grinding into an ethanol solution, performing ball milling dispersion, washing by centrifugal water after the dispersion is finished, and drying to obtain the target material, wherein the luminous efficiency of the material is improved by 2-3 times, and the particle size distribution is 50-100 nm.
Detailed Description
The invention relates to an X-ray imaging material, which comprises a precursor matrix material BaFCl synthesized by a hydrothermal coprecipitation method, a main activator containing Eu, a coactivator containing Ce, Sm, Gd, Dy and Tb, and a coactivator containing K+And NH4 +The cosolvent of the halogen compound is NH4F is used as a complexing agent, a precursor BaFCl matrix material is prepared by adopting a coprecipitation method, and then a main activator and a coactivator are dissolved to prepare an ionic solution with a certain concentration;dissolving a cosolvent in deionized water, adding a matrix material and an activator into the cosolvent by adopting a wet-method burdening mode, uniformly mixing, drying, sintering in a reducing atmosphere, removing oxidized substances on the surface under an ultraviolet lamp after sintering, and then washing with water to obtain a white material with the particle size distribution of 50-100 nm.
The Ba source in the BaFCl as the host material in the present invention is derived from BaCl2 。2H2Dissolving O in deionized water, filtering, purifying to obtain 100g/L aqueous solution, and adding NH4F is taken as a complexing agent, dissolved in deionized water and then filtered to prepare a complexing agent solution with the mass fraction of 5%; mixing complexing agent and BaCl according to a certain mass ratio of 1:102 。2H2And (3) carrying out coprecipitation reaction on the O aqueous solution, controlling the titration speed of the complexing agent to be 50-100ml/min in the reaction process, fully stirring for reaction, obtaining white precipitate after the reaction is finished, then centrifuging, washing with water, drying in an oven at 80 ℃ for 8 hours, and drying to obtain the matrix material.
The invention relates to an X-ray imaging material, which is characterized in that firstly, a cosolvent is weighed according to the mass ratio of 5-10% and then placed in a watch glass, deionized water is added to dissolve the cosolvent to form an aqueous solution, then a matrix material is added, and the mixture is uniformly stirred; and then adding the main activator and the co-activator in a mass ratio of 0.5-1% and 0.1-0.3% into a watch glass, uniformly stirring in a wet blending mode, placing in an oven, drying at 120 ℃ for 6 hours, and drying to form a precursor material.
The invention relates to an X-ray imaging material; grinding the dried precursor into small particles by using a jaw crusher, dispersing the small particles into powder by using a jet mill, putting the uniformly dispersed precursor into a reaction kettle, adding a certain amount of deionized water to disperse the solution into a solution with the mass fraction of 10-25%, adding sodium borohydride serving as a reducing agent according to the proportion of 2-5%, uniformly stirring the solution after the dissolution is finished, putting the solution into a microwave reactor, setting the temperature at 100 ℃ for 300 ℃, reacting at a constant temperature for 3-5 hours, quickly cooling the solution at room temperature after the reaction is finished, pouring out supernatant after the cooling and standing, performing powder selection treatment under an ultraviolet lamp to remove oxidized substances on the surface, grinding the small particles by using the jaw crusher, dispersing the small particles into powder by using the jet mill, dispersing the dispersed powder material into an ethanol solution for ball milling, and grinding the agate balls required in the ball milling process, The mass ratio of the ethanol to the powder material is 1:1: 1; and after the dispersion is finished, obtaining a powder material through centrifugation, washing the powder material with acetone for three times, then placing the centrifuged material in an oven for drying at 80 ℃, and detecting the particle size distribution of the dried material to be 50-100 nanometers.
The invention has the advantages that
1) The X-ray imaging material has the advantages of simple synthesis process, easy control of the process and cost reduction.
2) The X-ray imaging material is non-toxic and harmless, and has the advantages of low cost, long service life and high efficiency.
3) The X-ray imaging material has the advantages of simple production process, suitability for mass production, simple product classification and convenience in use.
Examples
Example 1
Synthesis of matrix material BaFCl: weighing BaCl2 .2H250g of O material is placed in a beaker, 100ml of deionized water is added, the mixture is heated, dissolved and filtered to be constant volume of 500ml, solution with solid content of 10% is prepared, and then 5g of complexing agent NH is weighed4F, adding deionized water for dissolving, filtering and fixing the volume to 100ml to prepare a solution with the solid content of 5%; then, the complexing agent was added dropwise to BaCl at a rate of 50/min using a constant flow peristaltic pump2 。2H2And (3) fully stirring in the O aqueous solution, standing for 1 hour after dropwise addition, pouring out supernatant on the surface, carrying out centrifugal washing, and drying in an oven at 80 ℃ after washing to obtain the matrix material.
Example 2
0.2g of cosolvent KCl powder and 2.0g of cosolvent NH are weighed in sequence4Placing Cl powder in a watch glass, adding deionized water to dissolve, adding 20g of matrix material BaFCl, stirring uniformly for later use, and adding 0.2g of main activator Eu2O30.1g of CeO co-activator2Uniformly stirring, placing in a drying oven for drying at 120 ℃ for 6 hours, and finishing dryingAnd then obtaining the precursor material.
Example 3
Crushing and uniformly grinding the dried material, putting the crushed and uniformly ground material into a high-temperature reaction kettle, adding a certain amount of deionized water to disperse the deionized water into a solution with the mass fraction of 10%, then adding 2% of sodium borohydride serving as a reducing agent in proportion, setting the temperature at 100 ℃, carrying out constant-temperature reaction for 4 hours, quickly cooling the solution at room temperature after the reaction is finished, pouring out supernatant after cooling and standing, carrying out powder selection treatment under an ultraviolet lamp, removing oxidized substances on the surface, drying the materials in an oven, uniformly grinding the materials after drying, dispersing the materials into an ethanol solution to carry out ball milling dispersion, obtaining a powder material through centrifugation after the dispersion is finished, washing the powder material with acetone for three times, placing the centrifuged material in the oven for drying at 80 ℃, and detecting the particle size distribution of 80-120 nanometers after the drying.
Example 4
0.1g of cosolvent K is weighed in turn2CO3Powder, 1.5g cosolvent (NH)4)2CO3Placing the powder in a watch glass, adding deionized water to dissolve, adding 20g of matrix material BaFCl, stirring, and adding 0.15g of main activator Eu (NO)3）30.05g of CeO co-activator20.05g of the coactivator Dy2O3And (4) uniformly stirring, placing in an oven for drying at 120 ℃ for 6 hours, and obtaining a precursor material after drying.
Example 5
Crushing and uniformly grinding the dried material, putting the crushed and uniformly ground material into a high-temperature reaction kettle, adding a certain amount of deionized water to disperse the deionized water into a solution with the mass fraction of 15%, then adding 5% of sodium borohydride serving as a reducing agent in proportion, setting the temperature at 200 ℃, carrying out constant-temperature reaction for 3 hours, quickly cooling the mixture at room temperature after the reaction is finished, pouring out supernatant after the mixture is cooled and stood, carrying out powder selection treatment under an ultraviolet lamp, removing oxidized substances on the surface of the mixture, drying the mixture in an oven, uniformly grinding the mixture after the drying, dispersing the mixture into an ethanol solution for ball milling and dispersion, centrifuging the mixture after the dispersion is finished to obtain a powder material, washing the powder material with acetone for three times, placing the centrifuged material in an oven for drying at 80 ℃, and detecting the particle size distribution of 100 and 120 nanometers after.
While the foregoing is directed to the preferred embodiment of the present invention, it will be apparent to those skilled in the art that various changes and modifications can be made herein without departing from the spirit and scope of the invention.

Claims (6)

1. An X-ray imaging material comprises a base material BaFCl, a main activator containing Eu is added into the base material, and CeO is added according to the mass ratio of 0.1-0.3%2，Sm2O3GdO and Dy2O3As a co-activator, with NH4F as a complexing agent to contain K+And NH4 +The halogen compound is used as a cosolvent, sodium borohydride is used as a reducing agent, the mixture is stirred in a reaction kettle at a constant temperature, the reaction kettle is placed in a microwave reactor after being uniformly stirred, the temperature is set to be 100 ℃ and 300 ℃, the reaction time is 3-5 hours, and after the reaction is finished, the white material is obtained after water washing treatment, wherein the particle size distribution is 50-100 nm.
2. An X-ray imaging material as defined in claim 1; the substrate material BaFCl is prepared by dissolving barium chloride containing crystal water in deionized water to prepare 10-15% aqueous solution and taking NH as raw material4F is used as a complexing agent and is dissolved in deionized water to prepare a 3-5% aqueous solution; according to the metering ratio of 10:1, dropwise adding a complexing agent into the barium chloride aqueous solution at the speed of 50-100ml/min, stirring for reaction, and drying to obtain the matrix material.
3. An X-ray imaging material as defined in claim 1; the main activator Eu is EuCl3，EuF3,Eu2O3And Eu (NO)3）30.5-1% by mass of one or more of the above-mentioned components.
4. A high brightness X-ray imaging as claimed in claim 1A material; the cosolvent is KCl, K2CO3，(NH4)2CO3，NH4F and NH4And one or more of Cl is added into the matrix material according to the mass ratio of 5-10%.
5. An X-ray imaging material as defined in claim 1; uniformly mixing a matrix material, an activating agent and a cosolvent according to a ratio, adding the mixture into a reaction kettle, uniformly stirring, adding sodium borohydride serving as a reducing agent, uniformly stirring, placing the reaction kettle into a microwave reactor, and synthesizing at the temperature of 100-300 ℃ for 3-5 hours.
6. An X-ray imaging material as defined in claim 1; removing oxidized materials on the surface of the materials obtained by reaction by an ultraviolet lamp, dispersing the powder materials obtained by grinding into an ethanol solution, performing ball milling dispersion, washing by centrifugal water after the dispersion is finished, and drying to obtain the target materials, wherein the luminous efficiency of the materials is improved by 2-3 times.
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CN110699074B (en) * 2019-11-06 2022-09-09 中国科学院理化技术研究所 Divalent europium-doped barium bromofluoride luminescent material and preparation method and application thereof
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CN102517001A (en) * 2010-12-24 2012-06-27 中国科学院福建物质结构研究所 Surface amine functionalized rare earth doped BaFCl nanometer fluorescence labeling material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN102517001A (en) * 2010-12-24 2012-06-27 中国科学院福建物质结构研究所 Surface amine functionalized rare earth doped BaFCl nanometer fluorescence labeling material and preparation method thereof

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