CN111025375B - Imaging plate for high-energy neutron photography and preparation method thereof - Google Patents
Imaging plate for high-energy neutron photography and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an imaging plate for high-energy neutron photography and a preparation method thereof. The scheme utilizes the nuclear reaction of neutrons and hydrogen atoms in a hydrogen-containing material to generate recoil protons, the recoil protons react with a fluorescent storage material in an imaging plate to form a latent image with neutron beam space distribution, and the latent image can be read out by a special imaging plate laser scanning device, so that high-energy neutron detection is realized, and the technical blank at home and abroad is filled.
Description
Technical Field
The invention relates to the field of high-energy neutron detectors, in particular to an imaging plate for high-energy neutron photography and a preparation method thereof.
Background
High-energy neutrons can penetrate steel, copper and other heavy metal cladding with the thickness of tens of centimeters and have higher sensitivity to low-Z light materials, so that the 14MeV high-energy neutron photography technology has obvious advantages in the aspects of internal structure and defect detection of large sample parts with the thick and heavy metal cladding, such as the charge quality of conventional weapons such as shells and missiles and the like and the distribution and defect detection of other light nuclides in the large sample parts, compared with other ray nondestructive detection technologies, and the high-energy neutron photography is a technical scheme which has the highest feasibility at present for realizing the nondestructive detection of certain large-size important component parts.
The neutron imaging plate has great potential when being used for high-energy neutron photography, can realize long-time integral imaging, avoids the defect that a digital imaging system cannot be exposed for a long time, solves the problem of low detection efficiency of the high-energy neutron photography to a certain extent, is similar to a film imaging series, has simple and flexible installation conditions and strong environmental adaptability, and has better convenience and usability compared with the digital imaging system when being used for on-site detection of weapon components.
Disclosure of Invention
The invention aims to provide an imaging plate for high-energy neutron photography and a preparation method thereof, which can fill the technical blank at home and abroad that no imaging plate for high-energy neutron photography exists at present.
The imaging plate for high-energy neutron photography has the working principle that neutrons react with hydrogen atoms in a hydrogen-containing material to generate recoil protons, the recoil protons react with a fluorescent storage material in the imaging plate to form a latent image with neutron beam space distribution, and the latent image can be read by a special imaging plate laser scanning device, so that high-energy neutron detection is realized.
The technical scheme adopted by the invention is as follows:
an imaging plate for high-energy neutron photography comprises a gamma filtering layer, a fluorescent layer, a supporting layer and a ferromagnetic layer which are sequentially overlapped from top to bottom; the fluorescent layer is made of polyvinyl butyral and BaFBr Eu2+The fluorescent powder is prepared by mixing the components according to the weight ratio of 1: 1.
The scheme is preferably as follows: the supporting layer is a PET material plate.
The scheme is preferably as follows: the ferromagnetic layer being Fe3O4And polyvinyl butyral in a weight ratio of 1: 1.
The scheme is preferably as follows: the gamma filter layer is a lead plate.
A preparation method of an imaging plate for high-energy neutron photography comprises the following steps:
a. preparing fluorescent powder and ferromagnetic powder:
a1, quantitatively weighing the mixture of the raw materials of the fluorescent powder, namely polyvinyl butyral and BaFBr Eu2+Mixing fluorescent powder according to the weight ratio of 1:1, and grinding in a ball mill;
a2, quantitatively weighing the ferromagnetic powder raw material mixture of polyvinyl butyral and Fe3O4Mixing and putting into a ball mill according to the weight ratio of 1:1 for grinding;
a3, putting the ground fluorescent powder raw material into an alumina boat, putting the alumina boat into a quartz tube of a tube furnace, and sintering to obtain a snow white hard solid product;
a4, grinding the solid product obtained in the step a3 through a 40-mesh screen to obtain a powdery product, namely the fluorescent powder;
a5, putting the ground ferromagnetic powder raw material into an alumina boat, putting the alumina boat into a quartz tube of a tube furnace, and sintering to obtain a snow-white hard solid product;
a6, grinding the solid product obtained in the step a5 through a 200-mesh screen to obtain a powdery product, namely ferromagnetic powder;
b. coating:
b1, weighing a proper amount of PVB, putting the PVB into a beaker, adding butanone and methyl isobutyl ketone into the beaker respectively, stirring for 2-3 minutes at normal temperature, heating to 60 ℃, stirring while heating, and standing by after the PVB is completely dissolved;
b2, adding the fluorescent powder, dibutyl phthalate and PVB solution into a ball milling tank, and carrying out ball milling for a specified time for later use;
b3, fixing the PET substrate on a stainless steel platform of a coating device, vacuumizing by using a vacuum pump to suck the PET substrate, installing the frame on the PET substrate, adjusting the level of the platform, opening hot water to pass through a pipeline in the stainless steel platform, controlling the temperature of the hot water to be 36 ℃, heating the platform, adding 10-15 ml of butanone into two cups in the coating device respectively, heating to 50 ℃, filling butanone gas into the coating device, and manufacturing a butanone atmosphere;
b4, pouring the mixed liquid reserved in the ball milling tank in the step b2 into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed;
b5, pouring the mixed liquid in the beaker into a frame installed on a PET sheet base through the operation of gloves on a glove box of the coating device, leveling the mixed liquid for 3-5 minutes, closing hot water, turning on ice water, reducing the temperature of a platform, keeping the temperature below 15 ℃ for 5 minutes, opening a valve on the coating device to a half position, continuously introducing the ice water for not less than 4 hours, opening the maximum position of the valve, and volatilizing all the solvent after 40 hours to finish the coating and drying of the fluorescent layer;
b6, adding the ferromagnetic powder and the PVB solution into a ball milling tank, and performing ball milling for a specified time for later use;
b7, pouring the mixed liquid reserved in the ball milling tank in the step b6 into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed;
b8, pouring the mixed liquid in the beaker into a frame arranged on a PET sheet base on the back of the fluorescent layer prepared in the step b5 through the operation of gloves on a glove box of the coating device, leveling the mixed liquid for 10 minutes, closing hot water, opening ice water, reducing the temperature of the platform, keeping the temperature below 15 ℃ for 5 minutes, opening a valve on the coating device to a half position, continuously introducing the ice water for not less than 5 hours, then opening the maximum position of the valve, and after 20 hours, completely volatilizing the solvent to finish the coating and drying of the ferromagnetic layer;
c. molding:
c1, stripping the prepared fluorescent layer and the prepared ferromagnetic layer from the PET film base;
c2, using a printing film laminating machine to smoothly adhere a piece of double-sided adhesive tape on two sides of the clean PET film at room temperature;
c3, respectively sticking the peeled fluorescent layer and ferromagnetic layer on two surfaces of the PET at room temperature by using a printing film covering machine;
c4, compacting the sample prepared in the step c3 at 60 ℃ by using a printing glazing machine, and covering the outer surfaces of the fluorescent layer and the ferromagnetic layer with a BOPP film with the thickness of 12 microns by using a printing film covering machine at 80 ℃;
c5, using a punching machine to cover a lead plate with a matched size above the fluorescent layer after punching and forming.
The scheme is preferably as follows: in the step a1, the phosphor powder comprises the following raw materials in parts by weight: NH (NH)4Br73.74 parts, BaCO370.46 parts of BaF265.76 parts of Eu2O30.645 parts; the raw materials of each component are put into a ball mill and then manually stirred to preliminarily mix the components, then the ball mill is started, the rotating speed of the ball mill is controlled to be 500 r/m, the ball milling time is 10 minutes, the operation is repeated for 3 times, and the ground raw material powder is obtained after sieving.
The scheme is preferably as follows: in step a3, the specific sintering process is as follows: vacuumizing the quartz tube, introducing mixed gas containing 93% of argon and 7% of hydrogen when the negative pressure in the quartz tube reaches 0.08MPa, and enabling the air pressure in the quartz tube to reach 0.02 MPa;
setting a temperature control program of the tube furnace:
a. heating to 380 ℃ from room temperature for 2 hours;
b. keeping the temperature at 380 ℃ for 2 hours;
c. heating from 380 ℃ to 850 ℃ for 2 hours;
d. keeping the temperature at 850 ℃ for 2 hours;
e. cooling to room temperature from 850 deg.C;
synchronously connecting the mixed gas, when the temperature control stage of the tube furnace is in the stages a to d, the gas flow rate is 10-12ml/min, and the gas flow rate is kept at 4-6ml/min in the stage e.
The scheme is preferably as follows: in the step b2, 1.14ml of dibutyl phthalate is added for every 20g of fluorescent powder.
The scheme is preferably as follows: in step b2, the working process of the ball mill is as follows: after ball milling for 5 hours, stopping the machine and placing for not less than 12 hours, then restarting the ball mill and carrying out ball milling for 1 hour.
The scheme is preferably as follows: in step b1, 85.8ml of butanone and 14.3ml of methyl isobutyl ketone are added for every 2.86g of PVB.
The technical principle adopted by the invention for solving the technical problems is as follows: the method is characterized in that neutrons and hydrogen atoms in a hydrogen-containing material are subjected to nuclear reaction to generate recoil protons, the recoil protons and a fluorescent storage material in an imaging plate are subjected to reaction to form a latent image of neutron beam spatial distribution, and the latent image can be read by a special imaging plate laser scanning device, so that high-energy neutron detection is realized. The imaging plate for high-energy neutron photography consists of a protective layer, a fluorescent layer and a ferromagnetic layer. The imaging plate for neutron photography at present is only suitable for thermal neutrons, and the imaging plate special for high-energy neutron photography is not developed at home and abroad. The imaging plate for high-energy neutron photography can solve the problems of low detection efficiency and poor imaging quality of high-energy neutron photography to a certain extent, and has great development potential in the field of high-energy neutron detection.
In conclusion, by adopting the technical scheme, the invention can provide the structure and the preparation method of the imaging plate special for high-energy neutron photography, and fills the technical blank in the field at home and abroad.
Drawings
Fig. 1 is a schematic diagram of a structure of an imaging plate for high-energy neutron radiography.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification (including any accompanying claims, abstract and drawings), may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
Examples
Weighing NH by means of a balance4Br(73.74g)、BaCO3(70.46g)、BaF2(65.76g)Eu2O3(0.645g), 100 zirconia balls are pre-filled in a ball milling tank, and then the weighed compound is filled in the ball milling tank and manually stirred to be preliminarily and uniformly mixed; ball-milling the fluorescent powder raw material mixture by using a ball mill, wherein the rotating speed of the ball mill is 500 r/min, the ball-milling time is 10 minutes, repeating the process for 3 times, and screening the milled raw material mixture by using a sieve for later use; placing the alumina boat filled with the fluorescent powder raw material mixture into a tubular furnace for sintering, keeping the temperature of the tubular furnace at 380 ℃ for 2 hours, then heating to 850 ℃, keeping the temperature for 2 hours, and then cooling to room temperature; after the temperature of the tube furnace is reduced to room temperature, the air valve is closed; accurately weighing PVB2.86g, putting the PVB into a 150ml beaker, adding 85.8ml of butanone and 14.3ml of methyl isobutyl ketone into the beaker respectively, stirring the mixture for 2 to 3 minutes at normal temperature, heating the mixture to 60 ℃, stirring the mixture while heating the mixture, and keeping the mixture for later use after PVB is completely dissolved; grinding the solid product with a mortar, sieving (40 mesh) to obtain a snow-white solid powder product, bottling the product, and storing in a drier to complete the preparation of the fluorescent powder；
A500-ml Teflon ball mill pot was prepared, and 100 zirconia balls having a diameter of 10mm were charged into each pot. According to the formula, 1.14ml of dibutyl phthalate and 20g of fluorescent powder are added into a ball milling tank; pouring all the PVB solution dissolved in the beaker into a ball milling tank, turning off the ball milling tank after ball milling for 5 hours, not opening the ball milling tank, standing for not less than 12 hours, and then turning on the ball milling tank again to ball mill for 1 hour for later use; pouring all the mixed liquid in the ball milling tank into a 150ml beaker, opening the cover of the beaker, putting the beaker into a coating device, locking the cover of the coating device, and closing a valve; pouring all the coating liquid in the beaker into a frame on a platform, leveling the coating liquid for 3-5 minutes, turning off hot water, turning on ice water, reducing the temperature of the platform, keeping the temperature below 15 ℃ for 5 minutes, opening a valve on a coating device to a half position, continuously turning on the ice water for not less than 4 hours, then opening the maximum position of the valve, volatilizing all the solvent after 40 hours, and drying the fluorescent coating to finish the coating process of the fluorescent layer;
quantitatively weighing ferromagnetic powder raw material mixture polyvinyl butyral and Fe3O4Mixing the materials according to the weight ratio of 1:1, and grinding the mixture in a ball mill for later use; and (3) putting the alumina boat filled with the ferromagnetic powder raw material mixture into a tubular furnace for sintering, and grinding the solid product obtained by sintering through a 200-mesh screen to obtain a powdery product, namely the ferromagnetic powder.
Adding ferromagnetic powder and PVB solution into a ball milling tank, and performing ball milling for a specified time for later use; pouring the mixed liquid reserved in the ball milling tank into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed; through the operation of gloves on a glove box of the coating device, the mixed liquid in the beaker is poured into a frame arranged on a PET film base on the back of the fluorescent layer, the frame is leveled for 10 minutes, hot water is closed, ice water is turned on, the temperature of the platform is reduced and kept below 15 ℃ for 5 minutes, a valve on the coating device is opened to a half position, the ice water is continuously introduced for no less than 5 hours, then the maximum position of the valve is opened, and after 20 hours, the solvent is completely volatilized, so that the coating and drying of the ferromagnetic layer are completed.
Stripping the prepared fluorescent layer from the PET film base; stripping the prepared ferromagnetic layer from the PET film base; a piece of double-sided adhesive tape is flatly stuck on two sides of a clean 100-micron PET film with the thickness of 240mm multiplied by 290mm at room temperature by using a printing film laminating machine; respectively sticking the peeled fluorescent layer and ferromagnetic layer on two surfaces of the PET at room temperature by using a printing film laminating machine; compacting the prepared sample at 60 ℃ by using a printing glazing machine; covering the outer surfaces of the fluorescent layer and the ferromagnetic layer with a BOPP film with the thickness of 12 microns by using a printing film covering machine at 80 ℃; punching and forming by using a punching machine; a lead plate with a thickness of 1mm was coated on the outer surface of the phosphor layer.
Comparative example 1
Weighing NH by means of a balance4Br(73.74g)、BaCO3(70.46g)、BaF2(65.76g)Eu2O3(0.645g), 100 zirconia balls are pre-filled in a ball milling tank, and then the weighed compound is filled in the ball milling tank and manually stirred to be preliminarily and uniformly mixed; ball-milling the fluorescent powder raw material mixture by using a ball mill at the rotating speed of 500 r/min for 10 min, repeating the ball-milling for 3 times, and screening the milled raw material mixture by using a sieve for later use; loading the alumina boat filled with the raw material mixture into a tubular furnace for sintering, keeping the temperature of the tubular furnace at 180 ℃ for 2 hours, then heating to 450 ℃, keeping the temperature for 2 hours, then cooling to room temperature; after the temperature of the tube furnace is reduced to room temperature, the air valve is closed; accurately weighing PVB2.86g, putting the PVB into a 150ml beaker, adding 85.8ml of butanone and 14.3ml of methyl isobutyl ketone into the beaker respectively, stirring the mixture for 2 to 3 minutes at normal temperature, heating the mixture to 40 ℃, stirring the mixture while heating the mixture, and keeping the mixture for later use after PVB is completely dissolved; the solid product was ground with a mortar and sieved (40 mesh) to obtain a snow-white solid powder product. Bottling the product, and storing in a dryer to finish the preparation of the fluorescent powder; 500ml of a polytetrafluoroethylene ball mill pot was prepared, and 100 zirconia balls having a diameter of 10mm were charged into each pot. According to the formula, 1.14ml of dibutyl phthalate and 20g of fluorescent powder are added into a ball milling tank; pouring all the PVB solution dissolved in the beaker into a ball milling tank, turning off the ball mill after 3 hours of ball milling, standing for not less than 12 hours without turning on the ball milling tank,then the ball mill is started again, and ball milling is carried out for 1 hour for standby; pouring all the mixed liquid in the ball milling tank into a 150ml beaker, opening the lid of the beaker, putting the beaker into a coating device, locking the lid of the coating device, and closing a valve; pouring all the coating liquid in the beaker into a frame on a platform, leveling the coating liquid for 3-5 minutes, turning off hot water, turning on ice water, reducing the temperature of the platform, keeping the temperature below 15 ℃ for 5 minutes, opening a valve on a coating device to a half position, continuously turning on the ice water for not less than 4 hours, then opening the maximum position of the valve, volatilizing all the solvent after 40 hours, and drying the fluorescent coating to finish the coating process;
quantitatively weighing ferromagnetic powder raw material mixture polyvinyl butyral and Fe3O4Mixing the materials according to the weight ratio of 1:1, and grinding the mixture in a ball mill for later use; and (3) putting the alumina boat filled with the ferromagnetic powder raw material mixture into a tubular furnace for sintering, and grinding the solid product obtained by sintering through a 200-mesh screen to obtain a powdery product, namely the ferromagnetic powder.
Adding ferromagnetic powder and PVB solution into a ball milling tank, and performing ball milling for a specified time for later use; pouring the mixed liquid reserved in the ball milling tank into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed; through the operation of gloves on a glove box of the coating device, the mixed liquid in the beaker is poured into a frame arranged on a PET film base on the back of the fluorescent layer, the frame is leveled for 10 minutes, hot water is closed, ice water is turned on, the temperature of the platform is reduced and kept below 15 ℃ for 5 minutes, a valve on the coating device is opened to a half position, the ice water is continuously introduced for no less than 5 hours, then the maximum position of the valve is opened, and after 20 hours, the solvent is completely volatilized, so that the coating and drying of the ferromagnetic layer are completed.
Stripping the prepared fluorescent layer from the PET film base; stripping the prepared ferromagnetic layer from the PET film base; a piece of double-sided adhesive tape is flatly stuck on two sides of a clean 100-micron PET film with the thickness of 240mm multiplied by 290mm at room temperature by using a printing film laminating machine; respectively sticking the peeled fluorescent layer and ferromagnetic layer on two surfaces of the PET at room temperature by using a printing film laminating machine; compacting the prepared sample at 60 ℃ by using a printing glazing machine; covering the outer surfaces of the fluorescent layer and the ferromagnetic layer with a BOPP film with the thickness of 12 microns by using a printing film covering machine at 80 ℃; punching and forming by using a punching machine; a lead plate with a thickness of 1mm was coated on the outer surface of the phosphor layer.
Comparative example 2
Weighing NH by means of a balance4Br(73.74g)、BaCO3(70.46g)、BaF2(65.76g)Eu2O3(0.645g), 100 zirconia balls are pre-filled in a ball milling tank, and then the weighed compound is filled in the ball milling tank and manually stirred to be preliminarily and uniformly mixed; ball-milling the fluorescent powder raw material mixture by using a ball mill, wherein the rotating speed of the ball mill is 500 r/min, the ball-milling time is 10 minutes, repeating the process for 3 times, and screening the milled raw material mixture by using a sieve for later use; placing the alumina boat filled with the raw material mixture into a tubular furnace for sintering, keeping the temperature of the tubular furnace at 380 ℃ for 2 hours, then heating to 850 ℃, keeping the temperature for 2 hours, and then cooling to room temperature; after the temperature of the tube furnace is reduced to room temperature, the air valve is closed; accurately weighing PVB2.86g, putting the PVB into a 150ml beaker, adding 85.8ml of butanone and 14.3ml of methyl isobutyl ketone into the beaker respectively, stirring the mixture for 2 to 3 minutes at normal temperature, heating the mixture to 60 ℃, stirring the mixture while heating the mixture, and keeping the mixture for later use after PVB is completely dissolved; the solid product was ground with a mortar and sieved (40 mesh) to obtain a snow-white solid powder product. Bottling the product, and storing in a dryer to finish the preparation of the fluorescent powder; 500ml of a polytetrafluoroethylene ball mill pot was prepared, and 100 zirconia balls having a diameter of 10mm were charged into each pot. According to the formula, 1.14ml of dibutyl phthalate and 20g of fluorescent powder are added into a ball milling tank; pouring all the PVB solution dissolved in the beaker into a ball milling tank, turning off the ball mill after ball milling for 5 hours, standing for no less than 8 hours without turning on the ball milling tank, and then turning on the ball mill again to ball mill for 1 hour for later use; pouring all the mixed liquid in the ball milling tank into a 150ml beaker, opening the cover of the beaker, putting the beaker into a coating device, locking the cover of the coating device, and closing a valve; pouring all the coating liquid in the beaker into a frame on a platform, leveling the coating liquid for 3-5 minutes, turning off hot water, turning on ice water, reducing the temperature of the platform, andafter keeping the temperature below 15 ℃ for 5 minutes, opening a valve on the coating device to a half position, continuously introducing ice water for not less than 4 hours, then opening the valve to the maximum position, and after 40 hours, completely volatilizing the solvent to finish drying the fluorescent coating, thus finishing the coating process;
quantitatively weighing ferromagnetic powder raw material mixture polyvinyl butyral and Fe3O4Mixing the materials according to the weight ratio of 1:1, and grinding the mixture in a ball mill for later use; and (3) putting the alumina boat filled with the ferromagnetic powder raw material mixture into a tubular furnace for sintering, and grinding the solid product obtained by sintering through a 200-mesh screen to obtain a powdery product, namely the ferromagnetic powder.
Adding ferromagnetic powder and PVB solution into a ball milling tank, and performing ball milling for a specified time for later use; pouring the mixed liquid reserved in the ball milling tank into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed; through the operation of gloves on a glove box of the coating device, the mixed liquid in the beaker is poured into a frame installed on a PET (polyethylene terephthalate) sheet base on the back of the fluorescent layer, the frame is leveled for 10 minutes, hot water is turned off, ice water is turned on, the temperature of the platform is reduced and kept below 15 ℃ for 5 minutes, a valve on the coating device is opened to a half position, the ice water is continuously introduced for no less than 5 hours, then the maximum position of the valve is opened, and after 20 hours, the solvent is completely volatilized, so that the coating and drying of the ferromagnetic layer are completed.
Stripping the prepared fluorescent layer from the PET film base; stripping the prepared ferromagnetic layer from the PET film base; a piece of double-sided adhesive tape is flatly stuck on two sides of a clean 100-micron PET film with the thickness of 240mm multiplied by 290mm at room temperature by using a printing film laminating machine; respectively sticking the peeled fluorescent layer and ferromagnetic layer on two surfaces of the PET at room temperature by using a printing film laminating machine; compacting the prepared sample at 60 ℃ by using a printing glazing machine; covering the outer surfaces of the fluorescent layer and the ferromagnetic layer with a BOPP film with the thickness of 12 microns by using a printing film covering machine at 80 ℃; punching and forming by using a punching machine; a lead plate with a thickness of 1mm was coated on the outer surface of the phosphor layer.
Comparative example 3
Weighing NH by means of a balance4Br(73.74g)、BaCO3(70.46g)、BaF2(65.76g)Eu2O3(0.645g), 100 zirconia balls are pre-filled in a ball milling tank, and then the weighed compound is filled in the ball milling tank and manually stirred to be preliminarily and uniformly mixed; ball-milling the fluorescent powder raw material mixture by using a ball mill, wherein the rotating speed of the ball mill is 500 r/min, the ball-milling time is 10 minutes, repeating the process for 3 times, and screening the milled raw material mixture by using a sieve for later use; placing the alumina boat filled with the raw material mixture into a tubular furnace for sintering, keeping the temperature of the tubular furnace at 380 ℃ for 0.5 hour, then heating to 850 ℃, keeping the temperature for 0.5 hour, then keeping the temperature for 2 hours, and then cooling to room temperature; after the temperature of the tube furnace is reduced to room temperature, the air valve is closed; accurately weighing PVB2.86g, putting the PVB into a 150ml beaker, adding 85.8ml of butanone and 14.3ml of methyl isobutyl ketone into the beaker respectively, stirring the mixture for 2 to 3 minutes at normal temperature, heating the mixture to 60 ℃, stirring the mixture while heating the mixture, and keeping the mixture for later use after PVB is completely dissolved; the solid product was ground with a mortar and sieved (40 mesh) to obtain a snow-white solid powder product. Bottling the product, and storing in a dryer to finish the preparation of the fluorescent powder; 500ml of a polytetrafluoroethylene ball mill pot was prepared, and 100 zirconia balls having a diameter of 10mm were charged into each pot. According to the formula, 1.14ml of dibutyl phthalate and 20g of fluorescent powder are added into a ball milling tank; pouring all the PVB solution dissolved in the beaker into a ball milling tank, turning off the ball mill after ball milling for 5 hours, standing for no less than 12 hours without turning on the ball milling tank, and then turning on the ball mill again to ball mill for 1 hour for later use; pouring all the mixed liquid in the ball milling tank into a 150ml beaker, opening the cover of the beaker, putting the beaker into a coating device, locking the cover of the coating device, and closing a valve; pouring all the coating liquid in the beaker into a frame on a platform, leveling the coating liquid for 3-5 minutes, turning off hot water, turning on ice water, reducing the temperature of the platform, keeping the temperature below 15 ℃ for 5 minutes, opening a valve on a coating device to a half position, continuously turning on the ice water for not less than 4 hours, then opening the maximum position of the valve, volatilizing all the solvent after 40 hours, and drying the fluorescent coating to finish the coating process;
quantitatively weighing ferromagnetic powder raw material mixture polyvinyl butyral and Fe3O4Mixing the materials according to the weight ratio of 1:1, and grinding the mixture in a ball mill for later use; and (3) putting the alumina boat filled with the ferromagnetic powder raw material mixture into a tubular furnace for sintering, and grinding the solid product obtained by sintering through a 200-mesh screen to obtain a powdery product, namely the ferromagnetic powder.
Adding ferromagnetic powder and PVB solution into a ball milling tank, and performing ball milling for a specified time for later use; pouring the mixed liquid reserved in the ball milling tank into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed; through the operation of gloves on a glove box of the coating device, the mixed liquid in the beaker is poured into a frame arranged on a PET film base on the back of the fluorescent layer, the frame is leveled for 10 minutes, hot water is closed, ice water is turned on, the temperature of the platform is reduced and kept below 15 ℃ for 5 minutes, a valve on the coating device is opened to a half position, the ice water is continuously introduced for no less than 5 hours, then the maximum position of the valve is opened, and after 20 hours, the solvent is completely volatilized, so that the coating and drying of the ferromagnetic layer are completed.
Stripping the prepared fluorescent layer from the PET film base; stripping the prepared ferromagnetic layer from the PET film base; a piece of double-sided adhesive tape is flatly stuck on two sides of a clean 100-micron PET film with the thickness of 240mm multiplied by 290mm at room temperature by using a printing film laminating machine; respectively sticking the peeled fluorescent layer and ferromagnetic layer on two surfaces of the PET at room temperature by using a printing film laminating machine; compacting the prepared sample at 60 ℃ by using a printing glazing machine; covering the outer surfaces of the fluorescent layer and the ferromagnetic layer with a BOPP film with the thickness of 12 microns by using a printing film covering machine at 80 ℃; punching and forming by using a punching machine; a lead plate with a thickness of 1mm was coated on the outer surface of the phosphor layer.
Comparative example 4
Weighing NH by a balance4Br(73.74g)、BaCO3(70.46g)、BaF2(65.76g)Eu2O3(0.645g), 100 zirconia balls are pre-filled in a ball milling tank, and then the weighed compound is filled in the ball milling tank and manually stirred to be preliminarily and uniformly mixed; ball-milling the fluorescent powder raw material mixture by a ball mill at the rotating speed of 500 r/min for 10 min, repeating the milling for 3 times, and sieving the milled fluorescent powder raw material mixture by a sieveThe raw material mixture of (1) is ready for use; placing the alumina boat filled with the raw material mixture into a tubular furnace for sintering, keeping the temperature of the tubular furnace at 380 ℃ for 2 hours, then heating to 850 ℃, keeping the temperature for 2 hours, and then cooling to room temperature; after the temperature of the tube furnace is reduced to room temperature, the air valve is closed; accurately weighing PVB2.86g, putting the PVB into a 150ml beaker, adding 85.8ml of butanone and 14.3ml of methyl isobutyl ketone into the beaker respectively, stirring the mixture for 2 to 3 minutes at normal temperature, heating the mixture to 60 ℃, stirring the mixture while heating the mixture, and keeping the mixture for later use after PVB is completely dissolved; the solid product was ground with a mortar and sieved (40 mesh) to obtain a snow-white solid powder product. Bottling the product, and storing in a dryer to finish the preparation of the fluorescent powder; 500ml of a polytetrafluoroethylene ball mill pot was prepared, and 100 zirconia balls having a diameter of 10mm were charged into each pot. According to the formula, 1.14ml of dibutyl phthalate and 20g of fluorescent powder are added into a ball milling tank; pouring all the PVB solution dissolved in the beaker into a ball milling tank, turning off the ball mill after ball milling for 5 hours, standing for no less than 12 hours without turning on the ball milling tank, and then turning on the ball mill again to ball mill for 1 hour for later use; pouring all the mixed liquid in the ball milling tank into a 150ml beaker, opening the cover of the beaker, putting the beaker into a coating device, locking the cover of the coating device, and closing a valve; pouring all the coating liquid in the beaker into a frame on a platform, leveling the coating liquid for 3-5 minutes, turning off hot water, turning on ice water, reducing the temperature of the platform, keeping the temperature below 15 ℃ for 5 minutes, opening a valve on a coating device to a half position, continuously turning on the ice water for not less than 4 hours, then opening the maximum position of the valve, volatilizing all the solvent after 40 hours, and drying the fluorescent coating to finish the coating process;
quantitatively weighing ferromagnetic powder raw material mixture polyvinyl butyral and Fe3O4Mixing the materials according to the weight ratio of 1:1, and grinding the mixture in a ball mill for later use; and (3) putting the alumina boat filled with the ferromagnetic powder raw material mixture into a tubular furnace for sintering, and grinding the solid product obtained by sintering through a 200-mesh screen to obtain a powdery product, namely the ferromagnetic powder.
Adding ferromagnetic powder and PVB solution into a ball milling tank, and performing ball milling for a specified time for later use; pouring the mixed liquid reserved in the ball milling tank into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed; through the operation of gloves on a glove box of the coating device, the mixed liquid in the beaker is poured into a frame arranged on a PET film base on the back of the fluorescent layer, the frame is leveled for 10 minutes, hot water is closed, ice water is turned on, the temperature of the platform is reduced and kept below 15 ℃ for 5 minutes, a valve on the coating device is opened to a half position, the ice water is continuously introduced for no less than 5 hours, then the maximum position of the valve is opened, and after 20 hours, the solvent is completely volatilized, so that the coating and drying of the ferromagnetic layer are completed.
Stripping the prepared fluorescent layer from the PET film base; stripping the prepared ferromagnetic layer from the PET film base; a piece of double-sided adhesive tape is flatly adhered to two sides of a clean 100-micron PET film with the thickness of 240mm multiplied by 290mm at room temperature by using a printing laminating machine; respectively sticking the peeled fluorescent layer and ferromagnetic layer on two surfaces of the PET at room temperature by using a printing film laminating machine; compacting the prepared sample at 60 ℃ by using a printing glazing machine; covering the outer surfaces of the fluorescent layer and the ferromagnetic layer with a BOPP film with the thickness of 12 microns by using a printing film covering machine at 80 ℃; and (5) punching and forming by using a punching machine.
Comparative example 5
Weighing NH by means of a balance4Br(73.74g)、BaCO3(70.46g)、BaF2(65.76g)Eu2O3(0.645g), 100 zirconia balls are pre-filled in a ball milling tank, and then the weighed compound is filled in the ball milling tank and manually stirred to be preliminarily and uniformly mixed; ball-milling the fluorescent powder raw material mixture by using a ball mill, wherein the rotating speed of the ball mill is 500 r/min, the ball-milling time is 10 minutes, repeating the process for 3 times, and screening the milled raw material mixture by using a sieve for later use; placing the alumina boat filled with the raw material mixture into a tubular furnace for sintering, keeping the temperature of the tubular furnace at 380 ℃ for 2 hours, then heating to 850 ℃, keeping the temperature for 2 hours, and then cooling to room temperature; after the temperature of the tube furnace is reduced to room temperature, the air valve is closed; accurately weighing PVB2.86g, putting the PVB2.86g into a 150ml beaker, adding 85.8ml of butanone and 14.3ml of methyl isobutyl ketone into the beaker respectively, and stirring the mixture for 2 to 3 minutes at normal temperatureThen heating to 60 ℃, stirring while heating, and after PVB is completely dissolved, keeping for later use; the solid product was ground with a mortar and sieved (40 mesh) to obtain a snow-white solid powder product. Bottling the product, and storing in a dryer to finish the preparation of the fluorescent powder; 500ml of a polytetrafluoroethylene ball mill pot was prepared, and 100 zirconia balls having a diameter of 10mm were charged into each pot. According to the formula, 1.14ml of dibutyl phthalate and 20g of fluorescent powder are added into a ball milling tank; pouring all the PVB solution dissolved in the beaker into a ball milling tank, turning off the ball mill after ball milling for 5 hours, standing for no less than 12 hours without turning on the ball milling tank, and then turning on the ball mill again to ball mill for 1 hour for later use; pouring all the mixed liquid in the ball milling tank into a 150ml beaker, opening the cover of the beaker, putting the beaker into a coating device, locking the cover of the coating device, and closing a valve; pouring all the coating liquid in the beaker into a frame on a platform, leveling the coating liquid for 3-5 minutes, turning off hot water, turning on ice water, reducing the temperature of the platform, keeping the temperature below 15 ℃ for 5 minutes, opening a valve on a coating device to a half position, continuously turning on the ice water for not less than 4 hours, then opening the maximum position of the valve, volatilizing all the solvent after 40 hours, and drying the fluorescent coating to finish the coating process;
quantitatively weighing ferromagnetic powder raw material mixture polyvinyl butyral and Fe3O4Mixing the materials according to the weight ratio of 1:1, and grinding the mixture in a ball mill for later use; and (3) putting the alumina boat filled with the ferromagnetic powder raw material mixture into a tubular furnace for sintering, and grinding the solid product obtained by sintering through a 200-mesh screen to obtain a powdery product, namely the ferromagnetic powder.
Adding ferromagnetic powder and PVB solution into a ball milling tank, and performing ball milling for a specified time for later use; pouring the mixed liquid reserved in the ball milling tank into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed; through the operation of gloves on a glove box of the coating device, the mixed liquid in the beaker is poured into a frame arranged on a PET film base on the back of the fluorescent layer, the frame is leveled for 10 minutes, hot water is closed, ice water is turned on, the temperature of the platform is reduced and kept below 15 ℃ for 5 minutes, a valve on the coating device is opened to a half position, the ice water is continuously introduced for no less than 5 hours, then the maximum position of the valve is opened, and after 20 hours, the solvent is completely volatilized, so that the coating and drying of the ferromagnetic layer are completed.
Stripping the prepared fluorescent layer from the PET film base; stripping the prepared ferromagnetic layer from the PET film base; a piece of double-sided adhesive tape is flatly stuck on two sides of a clean 20-micron PET film with the thickness of 240mm multiplied by 290mm at room temperature by using a printing film laminating machine; respectively sticking the peeled fluorescent layer and ferromagnetic layer on two surfaces of the PET at room temperature by using a printing film laminating machine; compacting the prepared sample at 60 ℃ by using a printing glazing machine; covering the outer surfaces of the fluorescent layer and the ferromagnetic layer with a BOPP film with the thickness of 12 microns by using a printing film covering machine at 80 ℃; punching and forming by using a punching machine; a lead plate with a thickness of 1mm was coated on the outer surface of the phosphor layer.
In table 1, the forming effect and the luminous efficiency of the examples and the comparative examples are compared, and the imaging plate for high-energy neutron photography of the present example is obviously superior to the comparative example.
TABLE 1 comparison of the parameters of examples and comparative examples, their molding effect and luminous efficiency
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (6)
1. A preparation method of an imaging plate for high-energy neutron photography is characterized by comprising the following steps: the method comprises the following steps:
a. preparing fluorescent powder and ferromagnetic powder:
a1, quantitatively weighing a fluorescent powder raw material mixture of polyvinyl butyral and BaFBr to Eu2+ fluorescent powder according to the weight ratio of 1 to 1, mixing and putting into a ball mill for grinding;
a2, quantitatively weighing ferromagnetic powder raw material mixture polyvinyl butyral and Fe3O4 according to the weight ratio of 1:1, mixing and putting into a ball mill for grinding;
a3, putting the ground fluorescent powder raw material into an alumina boat, putting the alumina boat into a quartz tube of a tube furnace, and sintering to obtain a snow white hard solid product;
a4, grinding the solid product obtained in the step a3 through a 40-mesh screen to obtain a powdery product, namely the fluorescent powder;
a5, putting the ground ferromagnetic powder raw material into an alumina boat, putting the alumina boat into a quartz tube of a tube furnace, and sintering to obtain a snow-white hard solid product;
a6, grinding the solid product obtained in the step a5 through a 200-mesh screen to obtain a powdery product, namely ferromagnetic powder;
b. coating:
b1, weighing a proper amount of PVB, putting the PVB into a beaker, adding butanone and methyl isobutyl ketone into the beaker respectively, stirring for 2-3 minutes at normal temperature, heating to 60 ℃, stirring while heating, and standing by after the PVB is completely dissolved;
b2, adding the fluorescent powder, dibutyl phthalate and PVB solution into a ball milling tank, and carrying out ball milling for a specified time for later use;
b3, fixing the PET substrate on a stainless steel platform of a coating device, evacuating the PET substrate by using a vacuum pump, installing the frame on the PET substrate, adjusting the level of the platform, opening a pipeline through which hot water passes in the stainless steel platform, controlling the temperature of the hot water to be 36 ℃, heating the platform, adding 10-15 ml of butanone into two cups in the coating device respectively, heating to 50 ℃, filling butanone gas in the coating device, and making butanone atmosphere;
b4, pouring the mixed liquid reserved in the ball milling tank in the step b2 into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed;
b5, pouring the mixed liquid in the beaker into a frame installed on a PET sheet base through the operation of gloves on a glove box of the coating device, leveling the mixed liquid for 3-5 minutes, closing hot water, turning on ice water, reducing the temperature of a platform, keeping the temperature below 15 ℃ for 5 minutes, opening a valve on the coating device to a half position, continuously introducing the ice water for not less than 4 hours, opening the maximum position of the valve, and volatilizing all the solvent after 40 hours to finish the coating and drying of the fluorescent layer;
b6, adding the ferromagnetic powder and the PVB solution into a ball milling tank, and performing ball milling for a specified time for later use;
b7, pouring the mixed liquid reserved in the ball milling tank in the step b6 into a beaker, covering a cup cover, transferring the beaker into a coating device, and ensuring the interior of the coating device to be sealed;
b8, pouring the mixed liquid in the beaker into a frame arranged on a PET sheet base on the back of the fluorescent layer prepared in the step b5 through the operation of gloves on a glove box of the coating device, leveling the mixed liquid for 10 minutes, closing hot water, opening ice water, reducing the temperature of the platform, keeping the temperature below 15 ℃ for 5 minutes, opening a valve on the coating device to a half position, continuously introducing the ice water for not less than 5 hours, then opening the maximum position of the valve, and after 20 hours, completely volatilizing the solvent to finish the coating and drying of the ferromagnetic layer;
c. molding:
c1, stripping the prepared fluorescent layer and the prepared ferromagnetic layer from the PET film base;
c2, using a printing film laminating machine to smoothly adhere a piece of double-sided adhesive tape on two sides of the clean PET film at room temperature;
c3, respectively sticking the peeled fluorescent layer and the ferromagnetic layer on two surfaces of the PET at room temperature by using a printing film covering machine;
c4, compacting the sample prepared in the step c3 at 60 ℃ by using a printing glazing machine, and covering the outer surfaces of the fluorescent layer and the ferromagnetic layer with a BOPP film with the thickness of 12 microns by using a printing film covering machine at 80 ℃;
and c5, using a punching machine to cover a lead plate with a matched size above the fluorescent layer after punching and forming.
2. A method according to claim 1, characterized by: in the step a1, the fluorescent powder comprises the following raw materials in parts by weight: NH4Br73.74 parts, BaCO370.46 parts, BaF265.76 parts and Eu2O30.645 parts; the raw materials of each component are put into a ball mill and then manually stirred to preliminarily mix the components, then the ball mill is started, the rotating speed of the ball mill is controlled to be 500 r/m, the ball milling time is 10 minutes, the operation is repeated for 3 times, and the ground raw material powder is obtained after sieving.
3. A method according to claim 1, characterized by: in the step a3, the specific sintering process is as follows: vacuumizing the quartz tube, introducing mixed gas containing 93% of argon and 7% of hydrogen when the negative pressure in the quartz tube reaches 0.08MPa, and enabling the air pressure in the quartz tube to reach 0.02 MPa;
setting a temperature control program of the tube furnace:
a. heating to 380 ℃ from room temperature for 2 hours;
b. keeping the temperature at 380 ℃ for 2 hours;
c. heating from 380 ℃ to 850 ℃ for 2 hours;
d. keeping the temperature at 850 ℃ for 2 hours;
e. cooling to room temperature from 850 ℃;
synchronously connecting the mixed gas, when the temperature control stage of the tube furnace is in the stages a to d, the gas flow rate is 10-12ml/min, and the gas flow rate is kept at 4-6ml/min in the stage e.
4. A method according to claim 1, characterized by: in the step b2, 1.14ml of dibutyl phthalate is added for every 20g of fluorescent powder.
5. A method according to claim 1, characterized by: in the step b2, the working process of the ball mill is as follows: after ball milling for 5 hours, stopping the machine and standing for not less than 12 hours, and then starting the ball mill again for ball milling for 1 hour.
6. A method according to claim 1, characterized by: in the step b1, 85.8ml of butanone and 14.3ml of methyl isobutyl ketone are required to be added in a matched manner for every 2.86g of PVB.
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