CN109749740A - A kind of embedded photoluminescent material, preparation method and application - Google Patents
A kind of embedded photoluminescent material, preparation method and application Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of embedded photoluminescent material, comprising: S1) cesium salt, silver salt, indium salts are mixed in an acidic solution with bismuth salt, obtain mixed solution；Cesium ion in the cesium salt, silver salt, indium salts and bismuth salt, silver ion, indium ion and bismuth ion molar ratio be 2:1:(1-x): x, 0≤x≤0.7；Contain in halogens and/or acid solution in the cesium salt, silver salt, indium salts and bismuth salt and contains halogens；S2) mixed solution is heated and is reacted, embedded photoluminescent material Cs is obtained2AgIn1‑xBixX6；X is halogens.Compared with prior art, high-temperature chemical reaction method provided by the invention prepares that polynary full-inorganic metal non-lead halogen micron crystalline substance size is small, it is few to lack, and there is efficient X-ray response characteristic, raw material needed for this method is simple simultaneously, reaction condition is mild, easy to operate, product production rate is high, has huge application potential in photodetection field.
Description
Technical field
The invention belongs to optoelectronic materials technology more particularly to a kind of embedded photoluminescent materials, preparation method and application.
Background technique
Metal halide perovskite material (ABX3) energy conversion efficiency with higher and excellent optical property, aobvious
Show that device, solar battery and luminescent device etc. have wide application prospect.Wherein, organic and inorganic halide perovskite material
(MAPbX3, MA=CH3NH3 +) have many advantages, such as that phototransformation efficiency is high, hole-electron recombination energy is small, carrier mobility is big, but
It is the disadvantage poor there is also stability.And full-inorganic metal halide perovskite material (CsPbX3, X=Cl, Br, I) then because
More excellent photoelectric property is presented and preferable stability has become current research hotspot.
Most recently newly perovskite structural material Cs4PbBr6(A4BX6) cause to pay close attention to, it shows and ABX3Profile material is not
Same photoelectric property (such as luminous efficiency is high, exciton binding energy is big), this A made4BX6Profile material is in light emitting diode, electroluminescent
The application such as device and photoelectric detector has great potential.However the generally existing heavy metal lead of metal halide material, prepare work
Skill is complicated, and material is caused to have bio-toxicity problem.It will increase if using the lead in nontoxic heavy metal components alternative materials
The defect density in material reduces device performance and stability is brought to decline problem.Therefore, it solves to stablize while one feasible
Property and the scheme of heavy metal lead toxicity be that the new structural haloid material of design becomes focus on research direction.
The Chinese patent of Publication No. CN107299393A discloses a kind of polynary perovskite structural material Cs2NaxAg1- xInyBi1-y X6(A2BIBIIX6, X=Cl, Br, I), it is prepared by hydro-thermal method, which is polynary full-inorganic gold
Belong to non-lead halogen and to ultraviolet light response characteristic, has potential application foreground in UV photodetector part field, but it rings
Answer speed still to be improved.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that provide a kind of embedded photoluminescent material, preparation method and
Using the embedded photoluminescent material size of this method preparation is small, and defect is few and X-ray response is fast.
The present invention provides a kind of preparation methods of embedded photoluminescent material, comprising:
S1) cesium salt, silver salt, indium salts are mixed in an acidic solution with bismuth salt, obtains mixed solution；The cesium salt, silver salt,
Cesium ion in indium salts and bismuth salt, silver ion, indium ion and bismuth ion molar ratio be 2:1:(1-x): x, 0≤x≤0.7；It is described
Contain in halogens and/or acid solution in cesium salt, silver salt, indium salts and bismuth salt and contains halogens；
S2) mixed solution is heated and is reacted, embedded photoluminescent material Cs is obtained2AgIn1-xBixX6；X is halogens.
Preferably, the cesium salt is selected from cesium chloride and/or cesium nitrate；The silver salt is selected from silver chlorate and/or silver nitrate；Institute
It states indium salts and is selected from inidum chloride and/or indium nitrate；The bismuth salt is selected from bismuth chloride and/or bismuth nitrate；The acid solution is selected from salt
Acid solution and/or nitric acid solution.
Preferably, concentration sour in the acid solution is 8~10mol/L；The ratio of the silver salt and acid solution is
1mmol:(5~15) ml.
Preferably, the step S1) in be blended under non-illuminated conditions and carry out；The mixed time is 6~10h.
Preferably, the temperature of the heating reaction is 150 DEG C~200 DEG C；It is described heating reaction time be 20~
40min。
Preferably, after heating reaction, reaction solution is cooled to 80 DEG C~100 DEG C with 0.5~2 DEG C/h, then naturally cools to
Room temperature obtains embedded photoluminescent material.
The present invention also provides a kind of embedded photoluminescent materials, as shown in formula (I):
Cs2AgIn1-xBixX6(I)
Wherein, 0≤x≤0.7, X are halogens.
Preferably, the X is Cl.
Preferably, 0.15≤x≤0.5.
The present invention also provides above-mentioned embedded photoluminescent material X-ray embedded photoluminescent material application.
The present invention provides a kind of preparation methods of embedded photoluminescent material, comprising: S1) by cesium salt, silver salt, indium salts and bismuth salt
It mixes in an acidic solution, obtains mixed solution；Cesium ion, silver ion, indium ion in the cesium salt, silver salt, indium salts and bismuth salt
Molar ratio with bismuth ion is 2:1:(1-x): x, 0≤x≤0.7；Contain halogen member in the cesium salt, silver salt, indium salts and bismuth salt
Contain halogens in element and/or acid solution；S2) mixed solution is heated and is reacted, embedded photoluminescent material Cs is obtained2AgIn1- xBixX6；X is halogens.Compared with prior art, high-temperature chemical reaction method provided by the invention prepares polynary full-inorganic metal
Non-lead halogen micron crystalline substance size is small, it is few to lack, and has efficient X-ray response characteristic, while raw material needed for this method is simple, instead
Mild condition is answered, easy to operate, product production rate is high, has huge application potential in photodetection field.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph for the luminescence generated by light being prepared in the embodiment of the present invention 1~5；
Fig. 2 is the XRD spectra for the embedded photoluminescent material being prepared in the embodiment of the present invention 1~5；
Fig. 3 is the x-ray fluorescence spectrogram (excitation wave for the embedded photoluminescent material being prepared in the embodiment of the present invention 1~5
It is long: copper K α line 0.15406nm)；
Fig. 4 be the embodiment of the present invention 1~5 in be prepared embedded photoluminescent material luminescence generated by light spectrogram (excitation wavelength:
325nm laser).
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
The present invention provides a kind of embedded photoluminescent materials, as shown in formula (I):
Cs2AgIn1-xBixX6 (I)
Wherein, 0≤x≤0.7, preferably 0.15≤x≤0.7, more preferable 0.15≤x≤05, further preferably 0.15≤x≤0.3；
X is halogens, preferably Cl.
Embedded photoluminescent material provided by the invention is a kind of polynary full-inorganic metal non-lead salt material and for perovskite structure,
Size is small, and defect is few, and X-ray response is fast.
The present invention also provides a kind of preparation methods of above-mentioned embedded photoluminescent material, comprising: S1) by cesium salt, silver salt, indium salts
It is mixed in an acidic solution with bismuth salt, obtains mixed solution；Cesium ion in the cesium salt, silver salt, indium salts and bismuth salt, silver ion,
The molar ratio of indium ion and bismuth ion is 2:1:(1-x): x, 0≤x≤0.7；Contain in the cesium salt, silver salt, indium salts and bismuth salt
Contain halogens in halogens and/or acid solution；S2) mixed solution is heated and is reacted, embedded photoluminescent material is obtained
Cs2AgIn1-xBixX6；X is halogens.
Wherein, the present invention is not particularly limited the source of all raw materials, is commercially available.
Cesium salt, silver salt, indium salts are mixed in an acidic solution with bismuth salt, obtain mixed solution；The cesium salt is preferably chlorine
Change caesium and/or cesium nitrate；The silver salt is preferably silver chlorate and/or silver nitrate；The indium salts are preferably inidum chloride and/or nitric acid
Indium；The bismuth salt is preferably bismuth chloride and/or bismuth nitrate；The acid solution is preferably hydrochloric acid solution and/or nitric acid solution；Institute
Stating concentration sour in acid solution is preferably 8~10mol/L, more preferably 9~10mol/L, is further preferably 10mol/L；It is described
The ratio of silver salt and acid solution is preferably 1mmol:(5~15) ml, more preferably 1mmol:(6~12) ml, further preferably for
1mmol:(8~10) ml, most preferably 1mmol:8ml；The mixed method preferably stirs；The mixing is preferably in no light
Under the conditions of carry out；The mixed time is preferably 6~10h, more preferably 7~9h, is further preferably 8h, to guarantee that metal salt is complete
Fully dissolved is in acid solution.
Mixed solution is heated and is reacted；The temperature of the heating reaction is preferably 150 DEG C~200 DEG C, more preferably 160 DEG C
~190 DEG C, be further preferably 170 DEG C~180 DEG C；The time of the heating reaction is preferably 20~40min, more preferably 25~
35min is further preferably 20min；In heating reaction process when being heated to 140 DEG C, solution becomes to clarify, and continues to be heated to anti-
Answer temperature, isothermal reaction.
After reaction, preferably cooling, more preferable reaction solution is cooled to 80 DEG C~100 DEG C with 0.5~2 DEG C/h, then certainly
So it is cooled to room temperature；Further preferably reaction solution is cooled to 85 DEG C~95 DEG C with 0.5~1.5 DEG C/h, then cooled to room temperature；Most
It is preferred that reaction solution is cooled to 90 DEG C with 1 DEG C/h, then cooled to room temperature.
After being cooled to room temperature, alcoholic solvent centrifuge washing is preferably used to obtain embedded photoluminescent material after dry；The alcoholic solvent
Preferably ethyl alcohol；The drying is preferably that room temperature in vacuo is dry；The time of the drying is preferably 6~10h, more preferably 7~
9h is further preferably 8h.
High-temperature chemical reaction method provided by the invention prepares that polynary full-inorganic metal non-lead halogen micron crystalline substance size is small, lacks
It is few, and there is efficient X-ray response characteristic, while raw material needed for this method is simple, reaction condition is mild, easy to operate, product
Productivity is high, has huge application potential in photodetection field.
The present invention also provides a kind of embedded photoluminescent material X-ray embedded photoluminescent material application
In order to further illustrate the present invention, with reference to embodiments in a kind of high-purity ethyl orthosilicate provided by the invention
The detection method and detection system of micro-moisture are described in detail.
Reagent used in following embodiment is commercially available.
Embodiment 1
1.1 by 2mmol CsCl, 1mmol AgCl and 1mmol InCl3·4H2The metal chloride of O is placed in a beaker, to
8ml hydrochloric acid (10M) solution is added in beaker.
Under 1.2 no lights, above-mentioned metal salt solution is sufficiently stirred 8 hours, so that above-mentioned metal salt is dissolved completely in hydrochloric acid
Solution.
When 1.3 heating said solutions are to 140 DEG C, solution becomes clear；Continue to be warming up to 170 DEG C of isothermal reactions 0.5 small
When.
1.4 end of reaction, above-mentioned solution are cooled to 90 DEG C with 1 DEG C/h；Then room temperature is naturally cooled to.
1.5 use the above-mentioned sample of ethyl alcohol centrifuge washing for several times, and room temperature in vacuo is 8 hours dry, obtain Cs2AgInCl6Powder-like
Product.
To the polynary perovskite structure Cs prepared in embodiment 12AgInCl6Sample carries out characterization and optical property test such as
Under: the Cs of preparation2AgInCl6The SEM of crystallite is as shown in Figure 1, it can be seen that crystallite dimension is 1~2 μm；Preparation
Cs2AgInCl6Crystallite XRD is as shown in Fig. 2, belong to a cube structure of double perovskite；The Cs of preparation2AgInCl6Crystallite X-ray fluorescence light
Spectrum is as shown in figure 3, it can be seen from figure 3 that this sample X-ray fluorescence is weaker, emission wavelength 607nm；The Cs of preparation2AgInCl6Crystallite light
Photoluminescence spectrum is as shown in figure 4, as seen from Figure 4, this sample luminescence generated by light is weaker, emission wavelength 609nm.
Embodiment 2
Similar to Example 1, difference is, by InCl in the step 1.1 of embodiment 13·4H2The amount of the substance of O is changed to
The amount of the substance of 0.85mmol and BiCl is 0.15mmol, and other conditions are consistent.Obtain Cs2AgIn0.85Bi0.15Cl6Crystallite
Powder.
To the polynary perovskite structure Cs prepared in embodiment 22AgIn0.85Bi0.15Cl6Sample carry out characterization and it is optical
Matter test is as follows: the Cs of preparation2AgIn0.85Bi0.15Cl6The SEM of crystallite is consistent with Fig. 1, and crystallite dimension is 1~2 μm；Preparation
Cs2AgIn0.85Bi0.15Cl6Crystallite XRD is as shown in Fig. 2, belong to a cube structure of double perovskite；The Cs of preparation2AgIn0.85Bi0.15Cl6
As shown in figure 3, it can be seen from figure 3 that doping 15%Bi, sample X-ray fluorescence are remarkably reinforced, emission wavelength is crystallite X-ray fluorescence spectrum
642nm；The Cs of preparation2AgIn0.85Bi0.15Cl6Crystallite photoluminescence spectra adulterates 15%Bi as shown in figure 4, as seen from Figure 4,
Sample luminescence generated by light is remarkably reinforced, emission wavelength 638nm.
Embodiment 3
Similar to Example 1, difference is, by InCl in the step 1.1 of embodiment 13·4H2The amount of the substance of O is changed to
The amount of the substance of 0.7mmol and BiCl is 0.3mmol, and other conditions are consistent.Obtain Cs2AgIn0.7Bi0.3Cl6Micro-crystal powder
End.
To the polynary perovskite structure Cs prepared in embodiment 32AgIn0.7Bi0.3Cl6Sample carries out characterization and optical property
It tests as follows: the Cs of preparation2AgIn0.7Bi0.3Cl6The SEM of crystallite is consistent with Fig. 1, and crystallite dimension is 1~2 μm；Preparation
Cs2AgIn0.7Bi0.3Cl6Crystallite XRD is as shown in Fig. 2, belong to a cube structure of double perovskite；The Cs of preparation2AgIn0.7Bi0.3Cl6It is micro-
Brilliant X-ray fluorescence spectrum is as shown in figure 3, it can be seen from figure 3 that adulterate 30%Bi, and sample X-ray fluorescence dramatically increases and X-ray fluorescence is most strong,
Emission wavelength is 640nm；The Cs of preparation2AgIn0.7Bi0.3Cl6Crystallite photoluminescence spectra is as shown in figure 4, as seen from Figure 4, adulterate
30%Bi, sample luminescence generated by light dramatically increases and luminescence generated by light is most strong, emission wavelength 640nm.
Embodiment 4
Similar to Example 1, difference is, by InCl in the step 1.1 of embodiment 13·4H2The amount of the substance of O is changed to
The amount of the substance of 0.5mmol and BiCl is 0.5mmol, and other conditions are consistent, and obtains Cs2AgIn0.5Bi0.5Cl6Micro-crystal powder
End.
To the polynary perovskite structure Cs prepared in embodiment 42AgIn0.5Bi0.5Cl6Sample carries out characterization and optical property
It tests as follows: the Cs of preparation2AgIn0.5Bi0.5Cl6The SEM of crystallite is consistent with Fig. 1, and crystallite dimension is 1~2 μm；Preparation
Cs2AgIn0.5Bi0.5Cl6Crystallite XRD is as shown in Fig. 2, belong to a cube structure of double perovskite；The Cs of preparation2AgIn0.5Bi0.5Cl6It is micro-
Brilliant X-ray fluorescence spectrum is as shown in figure 3, it can be seen from figure 3 that adulterate 50%Bi, and sample X-ray fluorescence starts to weaken and X-ray fluorescence is stronger,
Emission wavelength is 660nm；The Cs of preparation2AgIn0.5Bi0.5Cl6Crystallite photoluminescence spectra is as shown in figure 4, as seen from Figure 4, adulterate
50%Bi, sample luminescence generated by light starts to weaken and luminescence generated by light is stronger, emission wavelength 658nm.
Embodiment 5
Similar to Example 1, difference is, by InCl in the step 1.1 of embodiment 13·4H2The amount of the substance of O is changed to
The amount of the substance of 0.3mmol and BiCl is 0.7mmol, and other conditions are consistent, and obtains Cs2AgIn0.3Bi0.7Cl6Micro-crystal powder
End.
To the polynary perovskite structure Cs prepared in embodiment 52AgIn0.3Bi0.7Cl66Sample carries out characterization and optical property
It tests as follows: the Cs of preparation2AgIn0.3Bi0.7Cl6The SEM of crystallite is consistent with Fig. 1, and crystallite dimension is 1~2 μm；Preparation
Cs2AgIn0.3Bi0.7Cl6Crystallite XRD is as shown in Fig. 2, belong to a cube structure of double perovskite；The Cs of preparation2AgIn0.3Bi0.7Cl6It is micro-
As shown in figure 3, it can be seen from figure 3 that doping 70%Bi, sample X-ray fluorescence weaken rapidly, emission wavelength is brilliant X-ray fluorescence spectrum
660nm；The Cs of preparation2AgIn0.3Bi0.7Cl6Crystallite photoluminescence spectra is as shown in figure 4, as seen from Figure 4, adulterate 70%Bi, sample
Product luminescence generated by light is weaker rapidly, emission wavelength 658nm.
Curve in Fig. 3 is from top to bottom successively are as follows: Cs2AgIn0.7Bi0.3Cl6、Cs2AgIn0.85Bi0.15Cl6、
Cs2AgIn0.3Bi0.7Cl6、Cs2AgIn0.5Bi0.5Cl6、Cs2AgInCl6。
Curve in Fig. 4 is from top to bottom successively are as follows: Cs2AgIn0.7Bi0.3Cl6、Cs2AgIn0.85Bi0.15Cl6、
Cs2AgIn0.5Bi0.5Cl6、Cs2AgInCl6、Cs2AgIn0.3Bi0.7Cl6。
Claims (10)
1. a kind of preparation method of embedded photoluminescent material characterized by comprising
S1) cesium salt, silver salt, indium salts are mixed in an acidic solution with bismuth salt, obtains mixed solution；The cesium salt, silver salt, indium salts
Molar ratio with cesium ion in bismuth salt, silver ion, indium ion and bismuth ion is 2:1:(1-x): x, 0≤x≤0.7；The cesium salt,
Contain in halogens and/or acid solution in silver salt, indium salts and bismuth salt and contains halogens；
S2) mixed solution is heated and is reacted, embedded photoluminescent material Cs is obtained2AgIn1-xBixX6；X is halogens.
2. preparation method according to claim 1, which is characterized in that the cesium salt is selected from cesium chloride and/or cesium nitrate；Institute
It states silver salt and is selected from silver chlorate and/or silver nitrate；The indium salts are selected from inidum chloride and/or indium nitrate；The bismuth salt is selected from bismuth chloride
And/or bismuth nitrate；The acid solution is selected from hydrochloric acid solution and/or nitric acid solution.
3. preparation method according to claim 1, which is characterized in that in the acid solution sour concentration be 8~
10mol/L；The ratio of the silver salt and acid solution is 1mmol:(5~15) ml.
4. preparation method according to claim 1, which is characterized in that the step S1) in be blended under non-illuminated conditions
It carries out；The mixed time is 6~10h.
5. preparation method according to claim 1, which is characterized in that the temperature of the heating reaction is 150 DEG C~200
℃；The time of the heating reaction is 20~40min.
6. preparation method according to claim 1, which is characterized in that after heating reaction, reaction solution is cold with 0.5~2 DEG C/h
But to 80 DEG C~100 DEG C, then cooled to room temperature, obtains embedded photoluminescent material.
7. a kind of embedded photoluminescent material, as shown in formula (I):
Cs2AgIn1-xBixX6 (I)
Wherein, 0≤x≤0.7, X are halogens.
8. embedded photoluminescent material according to claim 7, which is characterized in that the X is Cl.
9. embedded photoluminescent material according to claim 7, which is characterized in that 0.15≤x≤0.5.
10. light described in embedded photoluminescent material prepared by claim 1~6 any one or claim 7~9 any one
Application of the electroluminescent material in X-ray embedded photoluminescent material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114085669A (en) * | 2021-10-26 | 2022-02-25 | 兰州大学 | Preparation method of lead-free double perovskite scintillator applied to X-ray detector |
| CN114751447B (en) * | 2022-04-13 | 2023-09-19 | 滨州裕能化工有限公司 | Cs (cell lines) 2 TiBr 6 Process for preparing powder |
| CN117025218A (en) * | 2023-08-08 | 2023-11-10 | 西南大学 | Rare earth doped mixed halogen double perovskite scintillator film and preparation method thereof |
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| CN107299393A (en) * | 2017-06-08 | 2017-10-27 | 华中科技大学 | A kind of polynary perovskite material and its preparation and application |
| CN108649128A (en) * | 2018-04-27 | 2018-10-12 | 华中科技大学 | A kind of one pack system electroluminescent white light device and preparation method thereof |
| CN108659827A (en) * | 2018-06-15 | 2018-10-16 | 华中科技大学 | Near ultraviolet excitated double-perovskite single-substrate white fluorescent material and preparation and application |
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| CN107299393A (en) * | 2017-06-08 | 2017-10-27 | 华中科技大学 | A kind of polynary perovskite material and its preparation and application |
| CN108649128A (en) * | 2018-04-27 | 2018-10-12 | 华中科技大学 | A kind of one pack system electroluminescent white light device and preparation method thereof |
| CN108659827A (en) * | 2018-06-15 | 2018-10-16 | 华中科技大学 | Near ultraviolet excitated double-perovskite single-substrate white fluorescent material and preparation and application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114085669A (en) * | 2021-10-26 | 2022-02-25 | 兰州大学 | Preparation method of lead-free double perovskite scintillator applied to X-ray detector |
| CN114751447B (en) * | 2022-04-13 | 2023-09-19 | 滨州裕能化工有限公司 | Cs (cell lines) 2 TiBr 6 Process for preparing powder |
| CN117025218A (en) * | 2023-08-08 | 2023-11-10 | 西南大学 | Rare earth doped mixed halogen double perovskite scintillator film and preparation method thereof |
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