CN110330335A - Bismuthino halide ceramic material, preparation method and X-ray detector - Google Patents
Bismuthino halide ceramic material, preparation method and X-ray detector Download PDFInfo
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- CN110330335A CN110330335A CN201910658874.9A CN201910658874A CN110330335A CN 110330335 A CN110330335 A CN 110330335A CN 201910658874 A CN201910658874 A CN 201910658874A CN 110330335 A CN110330335 A CN 110330335A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/5152—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on halogenides other than fluorides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
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Abstract
The invention discloses bismuthino halide ceramic material, preparation method and X-ray detectors, the X-ray detector, it is made of the electrode of bismuthino halide ceramics and its both ends, the bismuthino halide ceramics are the potsherd of bismuthino halide ceramic material pressed disc method preparation, both ends evaporation metal electrode.The present invention provides bismuthino halide ceramic material, be not only easy to prepare, environmental-friendly, stability is high, and resistivity is big, and prepared X-ray detector high-voltage resistance capability is strong, and radiation-resistant property is good, responds X-ray sensitive, and detection limit is low.
Description
Technical field
The present invention relates to halide technical field of ceramic material more particularly to bismuthino halide ceramic materials, preparation method
And X-ray detector.
Background technique
X-ray radiates in environmental monitoring, safety inspection, Nuclear Science and Technology, medical imaging, industrial nondestructive testing, space
Many fields such as detection and high-energy physics are widely used.Nuclear radiation detector for X-ray detection is X-ray application process
In one of key technology, therefore continue to develop X-ray detection material and X-ray detection technology is current ray research field
Important development direction.
The third generation X-ray detector in phase early 1960s is risen, i.e., semiconductor detector has rings faster
Speed, stronger power spectrum resolution capability, broader energy linearity range and more compact system construction are answered, in accurate power spectrum
Measurement aspect is substantially better than gas ionization detector and scintillator detector.Especially Room-temperature Nuclear Radiation Detectors, it is simultaneous
Have cryogenic semiconductor detector high energy resolution and scintillator detector high detection efficient the advantages that, be very suitable for core section
, space science, medical imaging, safety inspection and environmental protection etc. are to detector quick response, high detection efficient, low detection
The multi-demands of lower limit, simply portable etc. properties.
Pb based perovskite material is applied to X-ray detection field for the first time within 2015.Hereafter, multinomial about halide perovskite
Material is applied to X, and the work of gamma-ray detection is reported successively.Document report result concentrates on three-dimensional Pb base halide perovskite
Crystalline material.Generally contain lead in these materials, it is harmful to environment and biology, and there are Ion transfer phenomenon, applied electric fields
Caused Ion transfer is unfavorable for the control of device creepage, causes the noise level of detector higher, limits detector spirit
The promotion of sensitivity is unfavorable for the long-time stability of device.In addition to this, the growth course of crystal is also not simple enough, is unfavorable for quotient
Industry is promoted the use of.
And bismuthino perovskite material is nontoxic, environmental sound, existing bismuthino perovskite material only has Cs2AgBiBr6For
X-ray detection X field, Cs2AgBiBr6Monocrystalline is strong with falling temperature method growth uncontrollability, another existing Cs2AgBiBr6Ceramics are to use it
The powder that monocrystalline is ground is suppressed, and since the source of its raw material monocrystalline is not easy, is unfavorable for mass production.
Summary of the invention
In view of the above-mentioned problems, the invention proposes bismuthino halide ceramic material, with anti-solvent method/polishing and pressed disc method
It is prepared for the bismuthino perovskite ceramics material of novel environmental close friend a kind of and is applied to X-ray detection, preparation is simple, shape size
It is adjustable, it is conducive to business and uses, and detection performance is good, detection limit is low, high sensitivity.
The present invention through the following technical solutions to achieve the above objectives:
Bismuthino halide ceramic material, molecular formula R3Bi2X9, (Bi therein2X9)3Unit is by organic ion R+Surround shape
At dotted discontinuously arranged in three-dimensional space；
Wherein, X ion is one or more of halogen, Pseudohalides；Organic ion R is CnH2n+1NH3 +(1≤n
≤5)、CnH2n+1C (=NH) NH2 +(0≤n≤5)、C6H5CnH2n+1NH3 +(1≤n≤4)、C6H5CnH2n+1C (=NH) NH2 +(0≤n
One or more of≤4).
Another aspect of the present invention provides the preparation method of bismuthino halide ceramic material, comprising:
Anti-solvent method prepares ceramic material powder: by BiX3R is configured with RX3Bi2X9Precursor solution, solution concentration are
0.2M-2M, one or more of solvent GBL, DMF, DMSO etc. take supernatant after the completion of dissolution, will be molten after centrifugation
Liquid stirring instills in anti-solvent, and anti-solvent is one of chlorobenzene, ethyl acetate, ethyl alcohol, isopropanol or a variety of, after filtration drying
Obtain powder.The anti-solvent, which can extend to other, cannot dissolve the R3Bi2X9The solvent of bismuthino perovskite material.
Polishing prepares ceramic material powder: by BiX3R is configured with RX3Bi2X9Precursor solution grows crystal, takes the crystalline substance
Body is pulverized with agate mortar, and powder can be obtained.
Further scheme is solution concentration 0.5M-1M.
Further aspect of the present invention provides a kind of X-ray detector, by bismuthino halide ceramics and its electrode group at both ends
At the bismuthino halide ceramics are the potsherd of bismuthino halide ceramic material pressed disc method preparation, both ends evaporation metal
Electrode.
Further scheme is that the electrode material is gold, silver, copper, aluminium, platinum, palladium, graphite, conductive charcoal.
The beneficial effects of the present invention are:
The invention proposes bismuthino halide ceramic materials, have the features such as environmental-friendly, stability is high, and resistivity is big,
Prepared X-ray detector, radiation-resistant property is good, sensitive to X-ray response, and detection limit is low.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to embodiment or description of the prior art
In required practical attached drawing be briefly described, it should be apparent that, the accompanying drawings in the following description is only the one of the present embodiment
A little embodiments for those of ordinary skill in the art without creative efforts, can also be according to these
Attached drawing obtains other attached drawings.
Fig. 1 is the structural schematic diagram for the X-ray detector that the embodiment of the present invention is prepared；
Fig. 2 is the (CH that the embodiment of the present invention is prepared3NH3)3Bi2I9Ceramic sample；
Fig. 3 is the material phase analysis result data for the ceramics that the embodiment of the present invention is prepared；
Fig. 4 is the resistivity measurement result data for the potsherd that the embodiment of the present invention is prepared；
Fig. 5 is the (CH that the embodiment of the present invention is prepared3NH3)3Bi2I9The detection limit data of ceramics；
Fig. 6 is based on (CH3NH3)3Bi2I9The X-ray response data of the X-ray detection device of potsherd.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, the described embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art without making creative work it is obtained it is all its
Its embodiment belongs to the range that the present invention is protected.
Embodiment one
Present embodiments provide the method for obtaining high sensitivity X-ray detector using bismuthino perovskite ceramics material.
The X-ray detector, structure are as shown in Fig. 1.By bismuthino halide ceramics 2 and the electrode 1 at its both ends,
3 compositions.
Wherein bismuthino halide ceramics 2 are obtained by pressed disc method, shape such as Fig. 2 after compacting.Then in bismuthino halide ceramics
Both ends evaporation metal electrode, has just been prepared X-ray detector.The electrode material is gold, silver, copper, aluminium, platinum, palladium, stone
Ink, conductive charcoal etc..
Fig. 3 is the material phase analysis result data of counter sample, and display material is (CH3NH3)3Bi2I9, hexagonal structure, category
P63/mmc space group.Fig. 4 is the resistivity measurement result data of potsherd, the results showed that (CH3NH3)3Bi2I9The body of potsherd
Resistivity is 4.0 × 109Ω·cm.Fig. 5 gives (CH3NH3)3Bi2I9Ceramic material is under 20V operating voltage, to X-ray
Signal-to-noise ratio, detection limit is down to 0.3 μ GairY/s, than the 5.5 μ G of requirement of medical imaging device detection limitairY/s is much lower.
Fig. 6 is based on (CH3NH3)3Bi2I9The X-ray response data of the X-ray detection device of ceramics, in this embodiment it is possible to find out
When x-ray source open when, detector due to resistance reduce and export big current signal, when x-ray source close when, detector by
Restore initial value in resistance and export small current signal, detector responds X-ray sensitive.
Embodiment two
The preparation method for present embodiments providing bismuthino halide ceramic material, using anti-solvent method or polishing preparation pottery
Porcelain powder prepares potsherd using pressed disc method, specifically:
The process that anti-solvent method prepares powder is as follows:
By BiI3(bismuth iodide) and CH3NH3I (methylamino salt compounded of iodine) configures (CH3NH3)3Bi2I9Precursor solution, solution concentration
For 0.2M-2M (optimum condition 0.5-1M), solvent can be GBL, and one or more of DMF, DMSO etc. take supernatant
Liquid instills the solution after centrifugation in anti-solvent in the case where being stirred continuously, and anti-solvent can be chlorobenzene, ethyl acetate, second
One of alcohol, isopropanol are a variety of, obtain powder after dry, the size of powder is at 0.1~10 micron.Wherein, BiI3(iodate
Bismuth) it could alternatively be BiX (halogenation bismuth), CH3NH3It is similar for synthesizing that I (methylamino salt compounded of iodine) could alternatively be RX (organic halogen)
Bismuthino halide ceramic material powder.
The process that polishing prepares powder is as follows:
The crystal for taking the bismuthino halide ceramic material, is pulverized with agate mortar, powder can be obtained.
Bismuthino halide potsherd the preparation method is as follows:
A certain amount of powder is taken, different molds is chosen, mold can be various sizes of rectangular or circular mold etc.,
It is formed with hydraulic press, hydraulic press pressure is compacted in 0.5~5Mpa, time in 10~60s, then with isostatic pressing, waits static pressure pressure
Power, in 10~180s, obtains the potsherd of different shape any thickness in 10~500Mpa, time.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.Various embodiments of the present invention can be combined randomly, only
Want it without prejudice to thought of the invention, it should also be regarded as the disclosure of the present invention.
Claims (6)
1. bismuthino halide ceramic material, which is characterized in that molecular formula R3Bi2X9, (Bi therein2X9)3-Unit by it is organic from
Sub- R+Encirclement forms dotted discontinuously arranged in three-dimensional space；
Wherein, X ion is one or more of halogen, Pseudohalides；Organic ion R is CnH2n+1NH3 +(1≤n≤5)、
CnH2n+1C (=NH) NH2 +(0≤n≤5)、C6H5CnH2n+1NH3 +(1≤n≤4)、C6H5CnH2n+1C (=NH) NH2 +(0≤n≤4)
One or more of.
2. the preparation method of bismuthino halide ceramic material as described in claim 1 characterized by comprising
Anti-solvent method prepares ceramic material powder: by BiX3R is configured with RX3Bi2X9Precursor solution, solution concentration 0.2M-2M,
Solvent is one or more of GBL, DMF, DMSO etc., takes supernatant after the completion of dissolution, and the solution after centrifugation is stirred drop
Enter in anti-solvent, anti-solvent is one of chlorobenzene, ethyl acetate, ethyl alcohol, isopropanol or a variety of, and powder is obtained after filtration drying
Body.
3. the preparation method of bismuthino halide ceramic material as described in claim 1 characterized by comprising
Polishing prepares ceramic material powder: by BiX3R is configured with RX3Bi2X9Precursor solution grows crystal, and the crystal is taken to use
Agate mortar is pulverized, and powder can be obtained.
4. the preparation method of bismuthino halide ceramic material as claimed in claim 2, which is characterized in that solution concentration 0.5M-
1M。
5. a kind of X-ray detector, which is characterized in that be made of the electrode of bismuthino halide ceramics and its both ends, the bismuthino
Halide ceramics are the potsherd of bismuthino halide ceramic material pressed disc method preparation, both ends evaporation metal electrode.
6. X-ray detector as claimed in claim 5, which is characterized in that the electrode material be gold, silver, copper, aluminium, platinum,
Palladium, graphite, conductive charcoal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910658874.9A CN110330335A (en) | 2019-07-19 | 2019-07-19 | Bismuthino halide ceramic material, preparation method and X-ray detector |
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| CN108559503A (en) * | 2018-03-30 | 2018-09-21 | 华中科技大学 | A kind of Cs2AgBiBr6Double-perovskite and preparation method thereof |
| CN109873080A (en) * | 2019-01-24 | 2019-06-11 | 暨南大学 | A kind of perovskite Single Crystal X-ray detector and preparation method thereof |
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|---|---|---|---|---|
| EP2134457A1 (en) * | 2007-03-19 | 2009-12-23 | Prosonix Limited | Process for making crystals |
| CN106433619A (en) * | 2016-09-27 | 2017-02-22 | 华中科技大学 | Preparation method of Bi-based perovskite quantum dot material |
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Application publication date: 20191015 |