CN106632431A - Preparation method of 1, 2-dimethyl imidazole cadmium chloride perovskite material and application - Google Patents
Preparation method of 1, 2-dimethyl imidazole cadmium chloride perovskite material and application Download PDFInfo
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- 239000000463 material Substances 0.000 title abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 11
- -1 1, 2-dimethyl imidazole cadmium chloride Chemical compound 0.000 title description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 21
- 239000002178 crystalline material Substances 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 15
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 15
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 10
- 229910052793 cadmium Inorganic materials 0.000 claims description 9
- 235000019253 formic acid Nutrition 0.000 claims description 9
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- OKIIEJOIXGHUKX-UHFFFAOYSA-L cadmium iodide Chemical compound [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims description 2
- 150000003851 azoles Chemical class 0.000 claims description 2
- 229910000011 cadmium carbonate Inorganic materials 0.000 claims description 2
- 229940075417 cadmium iodide Drugs 0.000 claims description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 2
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Chemical compound [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 claims description 2
- GKDXQAKPHKQZSC-UHFFFAOYSA-L cadmium(2+);carbonate Chemical compound [Cd+2].[O-]C([O-])=O GKDXQAKPHKQZSC-UHFFFAOYSA-L 0.000 claims description 2
- HUKFCVYEXPZJJZ-UHFFFAOYSA-N cadmium;hydrate Chemical compound O.[Cd] HUKFCVYEXPZJJZ-UHFFFAOYSA-N 0.000 claims description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 238000009396 hybridization Methods 0.000 abstract description 5
- 230000000171 quenching effect Effects 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 description 6
- 238000004467 single crystal X-ray diffraction Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- GIWQSPITLQVMSG-UHFFFAOYSA-N 1,2-dimethylimidazole Chemical compound CC1=NC=CN1C GIWQSPITLQVMSG-UHFFFAOYSA-N 0.000 description 2
- 150000008614 2-methylimidazoles Chemical class 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 238000012430 stability testing Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910017488 Cu K Inorganic materials 0.000 description 1
- 229910017541 Cu-K Inorganic materials 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000388479 Physochlaina Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- MEMUUVPUNOWAFP-UHFFFAOYSA-L cadmium(2+) dichloride hydrochloride Chemical compound [Cl-].[Cd+2].Cl.[Cl-] MEMUUVPUNOWAFP-UHFFFAOYSA-L 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000001841 imino group Chemical group [H]N=* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 238000005935 nucleophilic addition reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 230000008685 targeting Effects 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
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- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/003—Compounds containing elements of Groups 2 or 12 of the Periodic Table without C-Metal linkages
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
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- C09K2211/10—Non-macromolecular compounds
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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Abstract
The invention discloses a novel ABX3 type hybridization perovskite crystalline material, a preparation method thereof and an application of the material, and belongs to an orthorhombic crystal system. The chemical formula of the crystalline material is (C5N2H9) CdCl3, a space group of the crystalline material is Pnma, cell parameters of the crystalline material are a= 11.2-11.3A, b= 7.1-7.2 A, c=12.4-12.5 A, wherein alpha=beta=gamma= 90 degrees, and Z=4. The crystalline material has high fluorescence effect in solvents. Acetonitrile has quenching effect on solution dissolving crystals, and the crystalline material has wide application prospect in chemical sensors, luminescent systems, biomedical sciences, negative ion detection and the like.
Description
Technical field
The application is related to a kind of new A BX3Type perovskite crystal material and its synthetic method.
Background technology
ABX3It, with excellent photoelectric properties, is one that the marked feature of type organic inorganic hybridization perovskite crystal material is exactly
Plant important light, electricity, magnetic multifunctional material, in nonlinear optical element, optical pickocff, solar cell device, superconduction device
The aspects such as part are extensively applied.The preparation and performance study of hydridization perovskite crystal material has attracted that domestic and international research worker's is wide
General interest.At present, extensive ABX is studied3Type perovskite is mainly CH3NH3PbX3(X=Cl, Br, I), thus crystalloid material
The solar cell device electricity conversion of preparation is more than 20%.
However, after the organic amine on A positions is replaced by nitrogen-containing heterocycle compound, the more research ferroelectricity of crystal of synthesis,
It is less for fluorescence property systematic study.
The application further enriches the photoelectric properties research of nitrogen heterocyclic ring class organic inorganic hybridization perovskite, by under room temperature
Synthesizing new ABX3Type organic inorganic hybridization perovskite (C5N2H9)CdCl3, gently, preparation method is simple, can prepare for preparation condition
Go out the crystal of large scale, there is stronger fluorescence in a solvent, preparation method and related work are not reported so far.(C5N2H9)
CdCl3Strong fluorescence is shown in the solution and to acetonitrile recognition reaction, be the new organic inorganic hybridization that there is using value
Perovskite crystal material.
The content of the invention
According to the one side of the application, there is provided a kind of novel crystal material, the crystalline material has in the solution larger
Fluorescent effect, excitation wavelength is 315nm, and launch wavelength is 420nm.Meanwhile, acetonitrile is quenched to the solution of the crystalline material
Effect.Additionally, the crystalline material has good heat stability, its heat decomposition temperature about at 226 DEG C, chemical sensor,
Luminescent system, biomedicine, Anionic recognition etc. have wide practical use.
The crystalline material, it is characterised in that chemical formula is (C5N2H9)CdCl3, belonging to rhombic system, space group is
Pnma, cell parameter is α=β=γ=90 °, Z
=4.
Preferably, the cell parameter of the crystalline material is Z=4, unit cell volume is
Compound (the C5N2H9)CdCl3Crystal structure it is as shown in Figure 1.Each Cd atom is connected into 5 Cl atoms
CdCl5Polyhedron, each polyhedron forms unlimited one-dimensional chain structure, parallel between 1,2- methylimidazole by the way that side is shared
Row, are filled between chain and chain.It is to produce epipolic main cause, the CN of acetonitrile that this compound has π-π * structures-And miaow
On azoles ring there is nucleophilic addition in imino group, and it is to produce the main cause being quenched to make π-π * destructurized.
According to the another aspect of the application, there is provided the preparation method of the crystalline material, it is characterised in that adopt liquid phase
Prepared by volatility process, the precursor liquid that 1,2- methylimidazoles, cadmium source, methanol, formic acid, mixed in hydrochloric acid are formed, and volatilizees at room temperature
Crystallization is obtained.
Preferably, in forerunner's liquid mixture, 1,2- methylimidazole, cadmium element, methanol, formic acid, hydrochloric acid mole
Than for C5N2H8:Cd:CH3OH:HCOOH:HCl=0.5～15.0:0.5～7.0:50～1000:20～100:20～100.Enter
One step preferably, in forerunner's liquid mixture, C5N2H8:Cd:CH3OH:HCOOH:HCl=7.0～9.0:3.0～5.0:50
～150:20～50:20～50.
Preferably, the volatilization crystallization temperature is 7～35 DEG C, and volatilization crystallization time is no less than 48 hours.
Preferably, the volatilization time is 48～168 hours.
Preferably, described cadmium source is optionally from cadmium carbonate, cadmium nitrate, Caddy (Cleary), Aska-Rid., cadmium iodide, Cadmium hydrate.
At least one.
Preferably, described cadmium source is from compound Caddy (Cleary).
According to the another aspect of the application, there is provided a kind of acetonitrile detector, containing any of the above-described crystalline material or by upper
State the crystalline material prepared by either method.
According to the another aspect of the application, there is provided the application process of the acetonitrile detector, used in above-mentioned solvent, use
In detection acetonitrile for fluorescent quenching effect at its in the solution 420nm.
The beneficial effect that the present invention can be produced at least includes：
(1) this application provides a kind of novel crystal material, crystalline material has in a solvent stronger fluorescent effect,
Excite at 315nm, launch at 420nm.Additionally, the crystalline material has good heat stability, its heat decomposition temperature is about
At 226 DEG C.Have wide practical use in chemical sensor, luminescent system, biomedicine, Anionic recognition etc..
(2) this application provides the preparation method of above-mentioned crystalline material, using mild condition liquid phase volatility process, 7～35
DEG C room temperature under, by solvent flashing crystallization, can high yield obtain high-purity sample.Method is simple, mild condition is conducive to
Realize large-scale industrial production.
(3) this application provides using the detector of above-mentioned material, can be used to detect acetonitrile for it in the solution
Fluorescent quenching effect at 420nm.
Description of the drawings
Fig. 1 is the compound (C5N2H9)CdCl3Crystal structure schematic diagram.
Fig. 2 is the X ray diffracting spectrum of sample 1#；Wherein (a) is that the crystal parsed according to single crystal X-ray diffraction is tied
Structure, is fitted the X ray diffracting spectrum for obtaining；B () is that sample 1# pulverizes the collection of illustrative plates that the test of last X-ray diffraction obtains.
Fig. 3 is the fluorescence spectrum under each solvent of sample 1#.
Fig. 4 is that sample 1# is dissolved in DMF, quenching fluorescence spectrum of the acetonitrile to sample 1# solution.
Fig. 5 is the thermogravimetric analysis figure of sample 1#.
Specific embodiment
With reference to embodiment, the application is expanded on further.It should be understood that these embodiments be merely to illustrate the application and not
For limiting scope of the present application.The experimental technique of unreceipted actual conditions in the following example, generally according to normal condition or
According to the condition proposed by manufacturer.
Inorganic compound preferably (C is prepared as one5N2H9)CdCl3Preferred embodiment, typical method is as follows：Will
Raw material DMIZ 1,2 dimethylimidazole, CdCl2·2.5H2O, methanol, formic acid, hydrochloric acid uniformly mix in clean sample bottle, volatilization temperature
Spend for 7～35 DEG C, the response time is 1～7 day, filters cleaning, you can obtain colourless block (C5N2H9)CdCl3Crystal.
The sample preparation of embodiment 1
By 1,2- methylimidazoles, cadmium source, formic acid, hydrochloric acid, methanol, according to a certain percentage mix homogeneously obtains precursor liquid, will
Precursor liquid is added in the test tube of 20mL, and under crystallization temperature after volatilization a period of time, Jing is filtered, cleans, is dried, and obtains colourless
Bulk (C5N2H9)CdCl3Crystal prototype.The species and proportioning, crystallization temperature, crystallization time and sample of forerunner's liquid mixture Central Plains material
The relation of product numbering is as shown in table 1.
The relation of the sample synthesis condition of table 1 and sample number into spectrum
The crystallographic structural analysis of the sample of embodiment 2
Using single crystal X-ray diffraction and powder X-ray diffraction method, structure elucidation is carried out to sample 1#～10#.
Wherein single crystal X-ray diffraction is in German Bruker companies Rigaku Mercury CCD type X-ray single crystal diffractometers
On carry out.Crystalline size is 0.12 × 0.10 × 0.12mm3；Data collection temperature is 293K, and diffraction light sources are graphite monochromatised
Mo-K alpha rays Scan mode is ω -2 θ；Data carry out absorption correction using Multi-Scan methods
Process.Structure elucidation is completed using SHELXTL-97 program bags；Determine the position of heavy atom with direct method, synthesized with difference Fourier
Method obtains remaining atomic coordinates；With based on F2The all atoms of complete matrix least square method refine coordinate and anisotropy physochlaina infudibularis
Number.
Powder X-ray diffraction is carried out on the x-ray powder diffraction instrument of German Bruker companies D8 types, and test condition is solid
Targeting monochromater Cu-K α, wavelengthSweep limitss 3-80 °, 0.02 ° of scanning step.
Wherein, single crystal X-ray diffraction result shows that sample 1# and sample 6# chemical formulas are (C5N2H9)CdCl3, belong to just
Crystallographic system is handed over, space group is Pnma, and cell parameter is
α=β=γ=90 °, Z=4, unit cell volume is
With sample 1# as Typical Representative, its crystal structural data is Z=4, unit cell volume isSample 1#
As shown in table 2, its crystal structure is as shown in Figure 1 for each atomic coordinates.
Each atomic coordinates, equivalent thermal parameter in the sample 1# of table 2
Wherein, powder X-ray diffraction result shows that in XRD spectra, peak position is essentially identical, various kinds for sample 1# and 6#
Product peak intensity slightly has difference.
With sample 1# as Typical Representative, as shown in Figure 2.The crystal parsed according to its single crystal X-ray diffraction in Fig. 2 (a)
Structure, is fitted the X ray diffracting spectrum that obtains and sample 1# in Fig. 2 (b) and pulverizes the figure that last X-ray diffraction test obtains
Spectrum, peak position is consistent with peak intensity.Illustrate that gained sample has very high-purity.
The fluorometric investigation of embodiment 3 is tested and result
The fluorometric investigation experiment of sample 1# is specific as follows：Using QM/TM fluorescent spectrophotometer assay dissolved with sample 1#'s
The fluorescence excitation of solution, emission spectrum, are dissolved in sample 1# and respectively in above-mentioned solvent, are made into the solution of 1mg/3ml, exist respectively
The light of 315nm is excited down, determines the emission spectrum under different solvents.Choosing the solution with N,N-dimethylformamide as solvent is
Typical Representative, adds 60 μ L acetonitriles, surveys the change of fluorescence intensity under the different plus angle of incidence.
Test result as shown in Figures 3 and 4, shows compound (C5N2H9)CdCl3Crystal has in the solution stronger fluorescence,
Acetonitrile has fluorescent quenching to act on sample 1# solution.
The heat stability testing of embodiment 4
The heat stability testing of sample 1# is enterprising in Mettler Toledo Inc. of Switzerland TGA/1100SF type thermogravimetric analyzers
OK.Sample 1# grind into powders, take 5mg and are added in crucible, debugging 30～900 DEG C of temperature range of scanning, and scanning speed is 15
℃/min.As a result as shown in figure 5, as seen from the figure the compound starts to decompose at 226 DEG C, illustrate sample 1# at 200 DEG C
Before have good stability.
The above, is only several embodiments of the present invention, and any type of restriction is not done to the present invention, although this
It is bright to be disclosed as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art are not taking off
In the range of technical solution of the present invention, make a little variation using the technology contents of the disclosure above or modification is equal to
Effect case study on implementation, belongs in the range of technical scheme.
Claims (8)
1. a kind of crystalline material, it is characterised in that chemical formula is (C5N2H9)CdCl3, belonging to rhombic system, space group is Pnma,
Cell parameter is α=β=γ=90 °, Z=4.
2. the method for preparing crystalline material described in claim 1, it is characterised in that prepared using liquid phase volatility process, by 1,2- bis-
The initial precursor liquid that Methylimidazole., cadmium source, methanol, formic acid, mixed in hydrochloric acid are formed, at room temperature solvent flashing crystallization is obtained.
3. method according to claim 2, it is characterised in that in initial forerunner's liquid mixture, 1,2- dimethyl miaow
Azoles, cadmium element, methanol, formic acid, the mol ratio of hydrochloric acid are C5N2H8：Cd:CH3OH:HCOOH:HCl=7.0～9.0:3.0～
5.0:50～150:20～50:20～50.
4. method according to claim 2, it is characterised in that the crystallization temperature is room temperature (7 DEG C～35 DEG C), during crystallization
Between be no less than 48 hours.
5. method according to claim 2, it is characterised in that the cadmium source optionally from cadmium carbonate, cadmium nitrate, Caddy (Cleary),
At least one in Aska-Rid., cadmium iodide, Cadmium hydrate..
6. a kind of acetonitrile detector, it is characterised in that containing the crystalline material described in claim 1 and/or according to claim
The crystalline material that 2-5 any one methods describeds are prepared is dissolved in the solution obtained in different solvents.
7. the acetonitrile detector described in claim 6, it is characterised in that the solvent is DMF, water, second
Alcohol, methanol, dimethyl sulfoxide.
8. the acetonitrile detector described in claim 6, the solution for dissolving crystal is excited in wavelength 315nm, there is stronger at 420nm
Fluorescence emission peak.
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| CN113089101A (en) * | 2021-03-30 | 2021-07-09 | 厦门大学 | Multi-polar axis plastic ferroelectric and piezoelectric material containing trimethyl chloroethyl amine and preparation and application thereof |
| CN114195718A (en) * | 2021-12-17 | 2022-03-18 | 北京理工大学 | One-dimensional edge-sharing perovskite fluorescent material and preparation method thereof |
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| CN113089101A (en) * | 2021-03-30 | 2021-07-09 | 厦门大学 | Multi-polar axis plastic ferroelectric and piezoelectric material containing trimethyl chloroethyl amine and preparation and application thereof |
| CN114195718A (en) * | 2021-12-17 | 2022-03-18 | 北京理工大学 | One-dimensional edge-sharing perovskite fluorescent material and preparation method thereof |
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