CN116854470A - Doped modified bismuth vanadate material used as direct X-ray array imaging device and preparation method thereof - Google Patents
Doped modified bismuth vanadate material used as direct X-ray array imaging device and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 49
- 238000003384 imaging method Methods 0.000 title claims abstract description 42
- -1 modified bismuth vanadate Chemical class 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 61
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 61
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000000919 ceramic Substances 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 150000001768 cations Chemical class 0.000 claims abstract description 3
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- 238000010438 heat treatment Methods 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
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- 238000003756 stirring Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000004020 conductor Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
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- 229910052742 iron Inorganic materials 0.000 description 1
- RQQRAHKHDFPBMC-UHFFFAOYSA-L lead(ii) iodide Chemical compound I[Pb]I RQQRAHKHDFPBMC-UHFFFAOYSA-L 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
The invention discloses a doped modified bismuth vanadate material used as a direct X-ray array imaging device and a preparation method thereof, wherein the chemical formula of the modified bismuth vanadate material is (A) X Bi 1‑X (B) Y V 1‑Y O Z Wherein X is more than or equal to 0 and less than or equal to 1, Y is more than or equal to 0 and less than or equal to 1, Z is more than or equal to 0 and less than or equal to 4, and A, B are metal cations. By doping the bismuth vanadate material, co doping is found, so that the carrier mobility, the service life and the carrier concentration of the bismuth vanadate material are improved, the corresponding sensitivity of the material is improved, the signal current noise is reduced, and the capability of realizing substrate array imaging is realized. By integrating bismuth vanadate ceramic onto the arrayed imaging substrate, X-ray arrayed imaging is successfully realized.
Description
Technical Field
The invention belongs to the field of preparation of direct type X-ray imaging devices, and particularly relates to a doped modified bismuth vanadate material used as a direct type X-ray imaging device and a preparation method thereof.
Background
Some basic information of X-ray imaging. Currently, X-ray detectors can be divided into direct detectors and indirect detectors. The indirect X-ray detector converts the X-ray with high photon energy into ultraviolet/visible light photons with low energy, and then the ultraviolet/visible light photons are further detected and imaged by the array photoelectric detector. In a direct detector, the detection material may directly convert the high energy radiation into an electrical signal. Common direct detection materials include a-Se, hgI 2 PbI2, cdZnTe, etc. Bismuth vanadate (BiVO) 4 ) Is a cheap, nontoxic and corrosion-resistant material, and is commonly used as photocatalysis and yellow pigment. However, they have been rarely reported in the field of X-ray imaging. The array imaging is to integrate the detection material on the array substrate and directly read out the signal current of all the pixel points at one time through the reading circuit. The bismuth vanadate material needs to have high sensitivity, small current noise, high spatial resolution and other performances when being used for direct type X-ray array imaging, and the properties of the existing bismuth vanadate material cannot meet the requirements.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a doped modified bismuth vanadate material used as a direct type X-ray array imaging device and a preparation method thereof.
The aim of the invention is realized by the following technical scheme: doped modified bismuth vanadate material for direct X-ray array imaging device, and chemical formula of modified bismuth vanadate material is (A) X Bi 1-X (B) Y V 1-Y O Z Wherein X is more than or equal to 0 and less than or equal to 1, Y is more than or equal to 0 and less than or equal to 1, Z is more than or equal to 0 and less than or equal to 4, X and Y are not zero at the same time, and A, B are metal cations.
As one of the possible embodiments, the A is any one of Co, fe and La.
As one of the possible embodiments, the a is Co.
As one of the possible embodiments, the B is Mo.
As one of the possible embodiments, a method for preparing a doped modified bismuth vanadate material for use as a direct type X-ray arrayed imaging device, comprising the steps of:
s1, preparation of bismuth vanadate powder
5mmol of Bi (NO) 3 ) 3 •5H 2 O was dissolved in 20ml of 2M nitric acid as solution I; the solution I is dissolved with the A and the B;
5mmol of NH 4 VO 3 Dissolving in 20ml of water, heating at 60deg.C and stirring for 30min to obtain solution II;
slowly dripping the solution II into the solution I, regulating the pH of the solution to 8 by using a sodium hydroxide solution, and heating and stirring at 60 ℃ for 30min in the regulating process to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, heating by using microwaves, and preserving heat for 2 hours at 180 ℃ to obtain a reaction product;
repeatedly cleaning the reaction product with ethanol and deionized water, and drying to obtain bismuth vanadate powder;
s2, preparation of bismuth vanadate ceramic
Using a PVA aqueous solution with the weight percent of 2 as an adhesive, putting 1g of bismuth vanadate powder and 1ml of adhesive into a mortar for uniform grinding, drying the slurry by an infrared lamp to remove water, and grinding by the mortar to obtain powder containing the adhesive;
placing the powder into a stainless steel die with the diameter of 7mm, applying 15MPa pressure to the stainless steel die by using hydraulic equipment, maintaining the pressure for 5min, and demolding to obtain a bismuth vanadate block pressed by bismuth vanadate powder;
and (3) putting the bismuth vanadate block into a tube furnace, introducing nitrogen into the tube furnace, heating at a high temperature of 700 ℃ for 8 hours, and cooling to obtain the bismuth vanadate ceramic.
As one of the possible embodiments, the bismuth vanadate ceramic is used for preparing a direct type X-ray imaging device, and specifically comprises the following steps:
cleaning a TFT imaging substrate and the bismuth vanadate ceramic, spin-coating a layer of conductive graphite glue on the surface of the bismuth vanadate ceramic as an adhesive, and then pressing the bismuth vanadate ceramic and the TFT imaging substrate together by using hot-pressing equipment;
evaporating a layer of conductive material on the surface of the pressed bismuth vanadate ceramic to serve as a back electrode, wherein the evaporating material is gold, silver, copper, ITO and the like;
finally, a line is led out from the conductive substrate to obtain the direct X-ray imaging device.
The beneficial effects of the invention are as follows: bismuth vanadate material is doped (Co) to improve the carrier mobility, the mobility life product and the carrier concentration of the material, and the sensitivity of the bismuth vanadate material can be improved to 1500 mu C G air -1cm-2 Signal current noise is reduced, and the detection lower limit reaches 28.17 and 28.17G air -1 s -1 The modified bismuth vanadate material is successfully integrated on the array substrate, and the array imaging of the modified bismuth vanadate material on X rays is realized.
Drawings
FIG. 1 is a schematic diagram of a direct X-ray imaging device;
FIG. 2 is a top view of a direct X-ray imaging device;
FIG. 3 is a graph of carrier mobility change of bismuth vanadate material doped with different elements;
FIG. 4 is a graph showing the signal current and bias voltage changes of bismuth vanadate material doped with different elements;
FIG. 5 is a graph comparing the sensitivity of Co-doped bismuth vanadate material at different voltages;
FIG. 6 is a graph showing the lower detection limit comparison of Co-doped bismuth vanadate material;
FIG. 7 is a graph showing the signal current contrast of Co-doped bismuth vanadate material under different measured X-rays;
FIG. 8 is an XRD pattern of bismuth vanadate material before and after Co doping;
FIG. 9 is a view of an imaged article;
fig. 10 is a diagram of imaging results.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the accompanying drawings, but the scope of the present invention is not limited to the following description.
Examples
Doped modified bismuth vanadate material for direct X-ray array imaging device, and chemical formula of modified bismuth vanadate material is (A) X Bi 1-X (B) Y V 1-Y O Z Wherein X is more than or equal to 0 and less than or equal to 1, Y is more than or equal to 0 and less than or equal to 1, Z is more than or equal to 0 and less than or equal to 4, wherein A is Co or Fe or La ion, and B is Mo ion;
the preparation method comprises the following steps:
s1, preparation of bismuth vanadate powder
5mmol of Bi (NO) 3 ) 3 •5H 2 O was dissolved in 20ml of 2M nitric acid as solution I; any one or two of the A and the B are dissolved in the solution I;
5mmol of NH 4 VO 3 Dissolving in 20ml of water, heating at 60deg.C and stirring for 30min to obtain solution II;
slowly dripping the solution II into the solution I, regulating the pH of the solution to 8 by using a sodium hydroxide solution, and heating and stirring at 60 ℃ for 30min in the regulating process to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, heating by using microwaves, and preserving heat for 2 hours at 180 ℃ to obtain a reaction product;
repeatedly cleaning the reaction product with ethanol and deionized water, and drying to obtain bismuth vanadate powder;
s2, preparation of bismuth vanadate ceramic
Using a PVA aqueous solution with the weight percent of 2 as an adhesive, putting 1g of bismuth vanadate powder and 1ml of adhesive into a mortar for uniform grinding, drying the slurry by an infrared lamp to remove water, and grinding by the mortar to obtain powder containing the adhesive;
placing the powder into a stainless steel die with the diameter of 7mm, applying 15MPa pressure to the stainless steel die by using hydraulic equipment, maintaining the pressure for 5min, and demolding to obtain a bismuth vanadate block pressed by bismuth vanadate powder;
putting the bismuth vanadate block into a tube furnace, introducing nitrogen into the tube furnace, heating at 700 ℃ for 8 hours, and cooling to obtain bismuth vanadate ceramic;
s3, preparation of direct X-ray imaging device
Cleaning a TFT imaging substrate and the bismuth vanadate ceramic, spin-coating a layer of conductive graphite glue on the surface of the bismuth vanadate ceramic as an adhesive, and then pressing the bismuth vanadate ceramic and the TFT imaging substrate together by using hot-pressing equipment;
evaporating a layer of conductive material on the surface of the pressed bismuth vanadate ceramic to serve as a back electrode, wherein the evaporating material is gold, silver, copper, ITO and the like;
finally, a line is led out from the conductive substrate to obtain the direct X-ray imaging device.
The performance of the modified bismuth vanadate material is detected, and the detection results are shown in fig. 3-8, and as can be seen from fig. 8, the (040) peak of the Target group after doping is obviously enhanced, which means that the exposed (040) surface of the bismuth vanadate material after doping with Co is more. The (010) surface corresponding to the (040) peak in the monoclinic bismuth vanadate material has higher carrier mobility than other surfaces, so that the carrier mobility after Co doping is obviously improved. The carrier mobility of bismuth vanadate material doped with different elements was measured according to the TOF (Time-of-flight) method, as shown in FIG. 3. From the graph, the transfer time (t tr ) From equation (1), where d is the ceramic sheet thickness and V is the applied bias. The mobility after Co doping was calculated to be from 3.24X10 -2 cm 2 ·V -1 ·s -1 Raised to 6.81 multiplied by 10 -2 cm 2 ·V -1 ·s -1 The mobility is not obviously changed after La is doped, and the mobility is reduced after Mo, fe and Co+Mo are doped. In addition, the relationship between the signal current and the bias voltage under illumination was also measured, as shown in fig. 4. The mobility lifetime product (mu tau product) of the material can be calculated by fitting a curve using a simplified Hecht equation. From the calculation result, the product of mu tau after doping Co and La is found to be 5.84 multiplied by 10 -5 cm 2 ·V -1 Respectively up to 9.03X10 -5 cm 2 ·V -1 And 8.47×10 -5 cm 2 ·V -1 The mu tau product is reduced after Mo, fe and Co+Mo are doped. According to the experimental results, the carrier mobility and the mobility service life product of the bismuth vanadate material are obviously improved after Co doping, so that the capability of the device for transmitting and collecting carriers is improved. Targeting doped CoSubsequent tests were performed on the group (Target) with a significant increase in signal current for the device (as shown in FIG. 7) for the same X-ray dose, with a sensitivity of 980. Mu. C G air -1cm-2 Up to 1500 mu C G air -1cm-2 (as shown in fig. 5).
(1)
(2)
Hall test is carried out on bismuth vanadate material, and the test result shows that the carrier concentration is 1.44 multiplied by 10 8 cm -3 Reduced to 1.01X10 8 cm -3 The reduction in the number of mobile carriers in the Co-doped bismuth vanadate material is shown to explain the significant reduction in the noise current of the Co-doped bismuth vanadate (as shown in fig. 7). SNR (Signal to Noise Ratio) signal-to-noise ratio is the ratio of signal current intensity to noise current intensity, with the dose rate at snr=3 as the lower detection limit. The Co-doped bismuth vanadate material has larger signal current and smaller noise current under the irradiation of X-rays with the same dosage, so the lower detection limit of the Target is 197.4 nGy air s -1 Reduced to 28.17 nGy air s -1 (as can be seen in FIG. 6).
The bismuth vanadate detector was subjected to imaging tests under X-rays. The object for imaging is shown in fig. 9, which is a Chinese character "living bright" metal sheet. The imaging results are shown in fig. 10, and it can be seen that the imaging can be clearly performed under X-rays.
The foregoing is merely a preferred embodiment of the invention, and it is to be understood that the invention is not limited to the form disclosed herein but is not to be construed as excluding other embodiments, but is capable of numerous other combinations, modifications and environments and is capable of modifications within the scope of the inventive concept, either as taught or as a matter of routine skill or knowledge in the relevant art. And that modifications and variations which do not depart from the spirit and scope of the invention are intended to be within the scope of the appended claims.
Claims (6)
1. The doping modified bismuth vanadate material used as a direct X-ray array imaging device is characterized in that: the chemical formula of the modified bismuth vanadate material is (A) X Bi 1-X (B) Y V 1-Y O Z Wherein X is more than or equal to 0 and less than or equal to 1, Y is more than or equal to 0 and less than or equal to 1, Z is more than or equal to 0 and less than or equal to 4, X and Y cannot be zero at the same time, and A, B are metal cations.
2. The doped modified bismuth vanadate material for use as a direct X-ray arrayed imaging device according to claim 1, wherein: the A is any one of Co, fe and La.
3. The doped modified bismuth vanadate material for use as a direct X-ray arrayed imaging device according to claim 2, wherein: the A is Co.
4. The doped modified bismuth vanadate material for use as a direct X-ray arrayed imaging device according to claim 1, wherein: and B is Mo.
5. The method of preparing a doped modified bismuth vanadate material for use as a direct X-ray arrayed imaging device according to claim 1,2,3 or 4, comprising the steps of:
s1, preparation of bismuth vanadate powder
Bi (NO) 3 ) 3 •5H 2 O is dissolved into nitric acid with the concentration of 2M to be used as a solution I; the solution I is dissolved with the A and the B;
NH of the reaction chamber 4 VO 3 Dissolving in water, heating at 60deg.C, stirring for 30min to obtain solution II;
slowly dripping the solution II into the solution I, regulating the pH of the solution to 8 by using a sodium hydroxide solution, and heating and stirring at 60 ℃ for 30min in the regulating process to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, heating by using microwaves, and preserving heat for 2 hours at 180 ℃ to obtain a reaction product;
repeatedly cleaning the reaction product with ethanol and deionized water, and drying to obtain bismuth vanadate powder;
s2, preparation of bismuth vanadate ceramic
Using a PVA aqueous solution with the weight percent of 2 as an adhesive, putting the bismuth vanadate powder and the adhesive into a mortar for uniform grinding, drying the slurry by an infrared lamp to remove water, and grinding by the mortar to obtain powder containing the adhesive;
placing the powder into a stainless steel die with the diameter of 7mm, applying 15MPa pressure to the stainless steel die by using hydraulic equipment, maintaining the pressure for 5min, and demolding to obtain a bismuth vanadate block pressed by bismuth vanadate powder;
and (3) putting the bismuth vanadate block into a tube furnace, introducing nitrogen into the tube furnace, heating at a high temperature of 700 ℃ for 8 hours, and cooling to obtain the bismuth vanadate ceramic.
6. The method for preparing the doped modified bismuth vanadate material for use as a direct type X-ray arrayed imaging device according to claim 5, wherein the method comprises the steps of: the bismuth vanadate ceramic is used for preparing a direct X-ray imaging device, and specifically comprises the following steps of:
cleaning a TFT imaging substrate and the bismuth vanadate ceramic, spin-coating a layer of conductive graphite glue on the surface of the bismuth vanadate ceramic as an adhesive, and then pressing the bismuth vanadate ceramic and the TFT imaging substrate together by using hot-pressing equipment;
evaporating a layer of conductive material on the surface of the pressed bismuth vanadate ceramic to serve as a back electrode;
finally, a line is led out from the conductive substrate to obtain the direct X-ray imaging device.
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