CN116854470B - 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 47
- 238000003384 imaging method Methods 0.000 title claims abstract description 39
- -1 modified bismuth vanadate Chemical class 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 64
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 64
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
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- 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 type X-ray array imaging device and a preparation method thereof, wherein the chemical formula of the modified bismuth vanadate material is (A) XBi1‑X(B)YV1‑YOZ, 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, and the like. Bismuth vanadate (BiVO 4) is an inexpensive, non-toxic, corrosion-resistant material commonly used as a photocatalytic 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, provides a doped modified bismuth vanadate material used as a direct type X-ray array imaging device and a preparation method thereof, and the bismuth vanadate material is doped, the Co-doped material has the advantages of improving the carrier mobility, improving the mobility service life product and reducing the carrier concentration, so that the sensitivity of the bismuth vanadate material is improved, the signal current noise is reduced, the bismuth vanadate ceramic is successfully doped and modified and integrated on an arrayed substrate, and the arrayed imaging of X rays is realized.
The aim of the invention is realized by the following technical scheme: the doped modified bismuth vanadate material is used as a direct type X-ray array imaging device, the chemical formula of the modified bismuth vanadate material is (A) XBi1-X(B)YV1-YOZ, 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 simultaneously zero, 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
Dissolving 5mmol of Bi (NO 3)3•5H2 O in 20ml of nitric acid with a concentration of 2M as a solution I in which the A and the B are dissolved;
dissolving 5mmol of NH 4VO3 in 20ml of water, heating and stirring at 60 ℃ for 30min to obtain a 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: the bismuth vanadate material is doped (Co), so that the carrier mobility of the material is improved, the mobility life product is improved, the carrier concentration is reduced, the sensitivity of the bismuth vanadate material can be improved to 1500 mu C G air -1cm-2, the signal current noise is reduced, the detection lower limit reaches 28.17G air -1s-1, the modified bismuth vanadate material is successfully integrated on an arrayed substrate, and the array imaging of 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
The doped modified bismuth vanadate material is used as a direct type X-ray array imaging device, and the chemical formula of the modified bismuth vanadate material is (A) XBi1-X(B)YV1-YOZ, 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 ions, and B is Mo ions;
The preparation method comprises the following steps:
S1, preparation of bismuth vanadate powder
Dissolving 5mmol of Bi (NO 3)3•5H2 O in 20ml of nitric acid with the concentration of 2M as a solution I, wherein either one or two of the A and the B are dissolved in the solution I;
dissolving 5mmol of NH 4VO3 in 20ml of water, heating and stirring at 60 ℃ for 30min to obtain a 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. The carrier transit time (t tr) can be obtained from the graph from equation (1), where d is the ceramic sheet thickness and V is the applied bias. the mobility after Co doping is calculated to be improved from 3.24X10 -2cm2·V-1·s-1 to 6.81× -2cm2·V-1·s-1, the mobility after La doping is not changed obviously, and the mobility after Mo, fe and Co+Mo doping is reduced. 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 results, the product of mu tau after Co and La doping was increased from 5.84X10 -5cm2·V-1 to 9.03X10 -5cm2·V-1 and 8.47X10 -5cm2·V-1, respectively, and the product of mu tau after Mo, fe and Co+Mo doping was decreased. 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. The subsequent test is carried out by taking the doped Co as a Target group (Target), the signal current of the device is obviously improved under the same X-ray measurement (as shown in figure 7), The sensitivity was increased from 980 μ C G air -1cm-2 to 1500 μ C G air -1cm-2 (as shown in fig. 5).
(1)
(2)
Hall tests were performed on bismuth vanadate material, and the test results showed that the carrier concentration was reduced from 1.44×10 8cm-3 to 1.01×10 8cm-3, indicating that the number of mobile carriers in the Co-doped bismuth vanadate material was reduced, which could explain the significant reduction in the noise current of 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. Since the Co-doped bismuth vanadate material has a larger signal current and a smaller noise current under the same dose of X-ray irradiation, the lower detection limit of Target is reduced from 197.4 nGy airs-1 to 28.17 nGy airs-1 (as can be seen from 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 (1)
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 XBi1-XBYV1-YOZ, 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;
the A is Co; the B is Mo;
the preparation method of the doped modified bismuth vanadate material used as the direct type X-ray array imaging device comprises the following steps:
S1, preparation of bismuth vanadate powder
Dissolving Bi (NO 3) 3•5H2 O in nitric acid with the concentration of 2M as a solution I, wherein either one or two of the A and the B are dissolved in the solution I;
Dissolving NH 4VO3 in water, heating and stirring at 60 ℃ for 30min to obtain a 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 concentration of 2wt% as an adhesive, putting the bismuth vanadate powder and the adhesive into a mortar for grinding uniformly, 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; 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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