CN109651408B - Novel CuI complex and preparation method and application thereof - Google Patents
Novel CuI complex and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000010668 complexation reaction Methods 0.000 title description 2
- ITQTTZVARXURQS-UHFFFAOYSA-N 3-methylpyridine Chemical compound CC1=CC=CN=C1 ITQTTZVARXURQS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000011540 sensing material Substances 0.000 claims abstract description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 229940071870 hydroiodic acid Drugs 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 2
- 238000004729 solvothermal method Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 23
- 230000035945 sensitivity Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 238000001308 synthesis method Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- CZZBXGOYISFHRY-UHFFFAOYSA-N copper;hydroiodide Chemical compound [Cu].I CZZBXGOYISFHRY-UHFFFAOYSA-N 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 8
- 238000009529 body temperature measurement Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 150000002910 rare earth metals Chemical class 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000012229 microporous material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 125000002346 iodo group Chemical group I* 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 150000002892 organic cations Chemical group 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000012360 testing method 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
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic System
- C07F1/005—Compounds containing elements of Groups 1 or 11 of the Periodic System 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/02—Constructional details
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/188—Metal complexes of other metals not provided for in one of the previous groups
Abstract
The invention provides a novel CuI complex and a preparation method and application thereof, belonging to the technical field of materials, wherein the complex [ N-Me-MePy]Cu2I3Molecular formula is C7NH10Cu2I3Belonging to the orthorhombic system, space group is Pnma, unit cell parameter is
c-12.5868 (8), Z-4, unit cell volume
A medium-low temperature solvent thermal synthesis method which adopts 3-methylpyridine, CuI and KI as raw materials; the organic-inorganic hybrid copper-iodine complex provided by the invention is low in price, simple to prepare, high in yield, high in sensitivity and excellent in fluorescence temperature sensing effect, and the luminous intensity and the temperature are in a linear relation in a large temperature range, and the complex can be used as a fluorescence temperature sensing material. This is the first CuI complex in the field to have a fluorescence intensity temperature sensing effect.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a novel CuI complex and a preparation method and application thereof.
Background
With the development of modern industry and science and technology, fields such as scientific research, industrial production, national defense science and technology, life science and the like have more and more strict requirements on temperature test and control. The traditional thermometers are all prepared by adopting a contact type heat exchange principle, such as a thermal expansion thermometer working based on a material thermal expansion and cold contraction principle, a thermal resistance thermometer designed based on the change of resistance along with the external temperature, a thermocouple thermometer and the like. However, in many harsh and complex environments such as a strong magnetic field, a high temperature, a high pressure, a high moving speed, high corrosion, an internal cell environment, microelectronic components and the like, the traditional contact thermometers cannot meet the temperature measurement requirement due to structural limitations, and therefore, the development of a novel non-contact thermometer has very important research significance.
In recent decades, semiconductor photoelectric materials have attracted scientific and industrial interest due to their tunable structural composition and fluorescent properties. The fluorescence property of the semiconductor material has a direct relationship with the external temperature, such as physical parameters of fluorescence intensity, emission wavelength, fluorescence lifetime, and the like. Therefore, the temperature measurement method based on the fluorescence technology can be realized by utilizing the conversion relation between the fluorescence performance of the semiconductor material and the temperature. The fluorescence temperature detection method that has been implemented so far includes: fluorescence emission peak position shift, emission peak spectral width, single emission fluorescence intensity, fluorescence intensity ratio, polarization anisotropy, and fluorescence lifetime. The peak position shift and the spectral width of the fluorescence emission peak are based on the temperature rise, the crystal field intensity decrease, the spectral peak shift and the spectral band broadening, but the accuracy of the two temperature sensing technologies is poor. The polarization anisotropy temperature measurement technology is based on an anisotropic semiconductor fluorescent material, and the fluorescence lifetime temperature measurement technology requires that the luminescence of the material has certain relaxation time, and the luminescence is strong enough and the decay rate is slow, so the application range is limited. In contrast, the emission intensity temperature measurement technology based on the semiconductor fluorescent material has lower requirements on the fluorescent material, and the emission intensity is obviously increased along with the reduction of the temperature. Therefore, the temperature detection method based on the conversion relation between the fluorescence intensity and the temperature becomes a fluorescence temperature measurement sensing technology with quick response, high sensitivity and high accuracy.
At present, the fluorescent materials with more applications are mainly based on rare earth oxides or complexes, but the rare earth materials are expensive, and the large-scale use of the rare earth materials in industrial production is severely limited, so that the development of the non-rare earth fluorescent materials with low price becomes the key point of the research on the large-scale development of the fluorescent temperature sensor. The monovalent Cu complex has important application value in the aspects of LED luminescence, illumination, display and optical communication due to low price, rich structure types and strong luminous intensity. Meanwhile, the luminous intensity of the fluorescent powder is obviously changed along with the temperature, and the fluorescent powder has higher sensitivity.
Disclosure of Invention
Aiming at the technical problems of high price, unstable excitation power and luminous intensity, weak anti-interference capability and the like of the current rare earth luminescent material, the invention provides a novel CuI complex and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
the novel CuI complex [ N-Me-MePy ] of the invention]Cu2I3Has a molecular formula of C7NH10Cu2I3Belonging to the orthorhombic system, space group is Pnma, unit cell parameter is
c-12.5868 (8), Z-4, unit cell volume
The preparation method of the novel CuI complex adopts a medium-low temperature solvothermal reaction synthesis method: weighing CuI, KI and 3-methylpyridine as reaction raw materials according to the molar ratio of (2-3) to (1-2), dissolving the reaction raw materials into a mixed solvent of 3-4 mL of acetonitrile, 0.5-1 mL of hydroiodic acid and 1-2 mL of methanol, sealing the mixture in a reaction kettle, reacting for 5-7 days in a drying box at 140 ℃ and 160 ℃, naturally cooling to room temperature, filtering the mixed solution, washing the filtered yellow block with ethanol for 2-3 times, and drying for 1-2 hours in a vacuum drying box at 80 ℃ to obtain the complex [ N-Me-MePy]Cu2I3Yellow crystals of (4).
The application of the novel CuI complex is characterized in that the complex can be used as a fluorescence temperature sensing material.
The invention provides a complex [ N-Me-MePy]Cu2I3Has high thermal stability, can be heated to 300 ℃ in air without decomposition, can absorb ultraviolet light in the range of 200-450nm, has an optical band gap of 2.5eV, and belongs to semiconductor materials.
Under the excitation of ultraviolet light with the wavelength of 325nm, the complex [ N-Me-MePy]Cu2I3Can emit strongIntense red light with a maximum emission wavelength of 702 nm. At the same time, the complex [ N-Me-MePy]Cu2I3The luminous intensity of the sensor can be gradually increased along with the reduction of the external temperature, and the luminous intensity and the external temperature have a linear relation in the temperature range of 80-220K, so that the sensor can be used as a sensor material for temperature detection. Furthermore, the complex [ N-Me-MePy]Cu2I3The luminous intensity of the fluorescent material has large variation range with temperature, so that the fluorescent material has high sensitivity, the maximum sensitivity is 5.5 at 220K, and the fluorescent material is far larger than a common rare earth complex luminous semiconductor. The data show that the complex [ N-Me-MePy ] provided by the invention]Cu2I3The fluorescent temperature sensing material has excellent fluorescent temperature sensing effect, can be used as a novel fluorescent temperature sensing material, and is applied to temperature detection in non-contact working environments such as high-intensity magnetic fields, flowing and high-voltage environments.
The invention has the beneficial effects that: the novel CuI complex provided by the invention is low in price, simple to prepare, high in sensitivity and excellent in fluorescence temperature sensing effect, and has a linear relation between the luminous intensity and the temperature in a large temperature range, and is the first CuI complex with the fluorescence intensity temperature sensing effect in the field.
Drawings
FIG. 1 shows the complex [ N-Me-MePy]Cu2I3Wherein the gray skeleton is [ N-Me-MePy]Template agent, the black part is Cu2I3A one-dimensional chain.
FIG. 2 shows the complex [ N-Me-MePy]Cu2I3The organic cations form quadrilateral pores, Cu2I3The one-dimensional chain is positioned in the pore canal.
FIG. 3 shows the complex [ N-Me-MePy]Cu2I3X-ray powder diffraction pattern of (a). The X-ray powder diffraction pattern collected by the experiment is consistent with the theoretical value, which indicates that the material is single-phase [ N-Me-MePy]Cu2I3The purity is close to 100%.
FIG. 4 shows the complex [ N-Me-MePy]Cu2I3Thermal stability curve of (2).
FIG. 5 shows the complex [ N-Me-MePy]Cu2I3Ultraviolet visible absorption ofAnd (6) collecting the spectrum.
FIG. 6 shows the complex [ N-Me-MePy]Cu2I3Emission spectra at different temperatures.
FIG. 7 shows the complex [ N-Me-MePy]Cu2I3The luminous intensity of (2) is plotted against temperature.
FIG. 8 shows the complex [ N-Me-MePy]Cu2I3Sensitivity of the luminescence intensity with temperature.
Detailed Description
Example 1
The novel CuI complex [ N-Me-MePy ] of the invention]Cu2I3The preparation method comprises the following steps: the medium-low temperature solvent thermal reaction synthesis method comprises the following steps: weighing CuI, KI and 3-methylpyridine as raw materials according to the molar ratio of 2:3:1, dissolving the raw materials into a mixed solvent of 3mL acetonitrile, 0.5mL hydroiodic acid and 1mL methanol, sealing the mixture in a stainless steel reaction kettle, reacting for 5 days in a constant-temperature forced air drying oven at 140 ℃, naturally cooling to room temperature, filtering the mixed solution, washing the filtered yellow block with ethanol for 2 times, and drying in a vacuum oven at 80 ℃ for 1 hour to obtain the complex [ N-Me-MePy]Cu2I3Yellow crystals of (4).
Example 2
The novel CuI complex [ N-Me-MePy ] of the invention]Cu2I3The preparation method comprises the following steps: the medium-low temperature solvent thermal reaction synthesis method comprises the following steps: weighing CuI, KI and 3-methylpyridine as raw materials according to the molar ratio of 3:3:2, dissolving the raw materials into a mixed solvent of 4mL of acetonitrile, 1mL of hydroiodic acid and 2mL of methanol, sealing the mixture in a reaction kettle, reacting for 7 days at 160 ℃ in a drying oven, naturally cooling to room temperature, filtering the mixed solution, washing the filtered yellow block with ethanol for 3 times, and drying for 2 hours at 80 ℃ in a vacuum oven to obtain the complex [ N-Me-MePy]Cu2I3Yellow crystals of (4).
FIG. 1 shows the complex [ N-Me-MePy]Cu2I3Crystal structure of (2). All Cu atoms are in a four-coordinate tetrahedral structure, and the tetrahedrons are connected through a shared I atom to form one-dimensional Cu2I3Chain, N-Me-MePy with Cu2I3Chain alternationArranged and connected with each other by hydrogen bonding force.
FIG. 2 shows the complex [ N-Me-MePy]Cu2I3The gray frame represents a three-dimensional frame structure constructed by N-Me-MePy through hydrogen bonding, and the black part represents one-dimensional Cu2I3And (3) a chain.
Example 3
FIG. 3 shows the complex [ N-Me-MePy]Cu2I3The diffraction pattern of the polycrystalline powder is the same as the data of the single crystal structure simulation, which shows that the polycrystalline powder is a pure complex [ N-Me-MePy]Cu2I3The purity was 99%.
The microporous lead iodide photoelectric material shown in FIG. 4 is in N2The thermogravimetric curve of the microporous material heated to 800 ℃ from room temperature in the atmosphere loses weight from 300 ℃, which shows that the microporous material can be heated to 300 ℃, has better thermal stability and can meet the requirement of being used as a semiconductor luminescent material.
Example 4
FIG. 6 shows the complex [ N-Me-MePy]Cu2I3Emission spectra at different temperatures. The maximum position of the emission peak is 702nm, and the emission peak belongs to red light. The emission intensity is strongest at 80K and weakest at 300K, the emission intensity is gradually increased along with the reduction of the temperature, the luminous intensity is in a linear relation with the temperature in the range of 80-220K, and the calculation formula is Imax-0.0051T +1.6962 wherein ImaxRepresents the luminous intensity and T represents the temperature. The sensitivity of temperature detection is calculated by the following formula:
sr represents the sensitivity of the compound to be detected,
represents the range of the luminous intensity of the emitted light,
representing the temperature range, I represents the luminescenceStrength.
Claims (3)
1. A CuI complex, which is characterized in that the complex [ N-Me-MePy]Cu2I3Has a molecular formula of C7NH10Cu2I3Belonging to the orthorhombic system, space group is Pnma, unit cell parameter is
c-12.5868 (8), Z-4, unit cell volume
2. A process for the preparation of the CuI complex of claim 1, wherein the synthesis is carried out using medium low temperature solvothermal reaction: weighing CuI, KI and 3-methylpyridine as reaction raw materials according to the molar ratio of (2-3) to (1-2), dissolving the reaction raw materials into a mixed solvent of 3-4 mL of acetonitrile, 0.5-1 mL of hydroiodic acid and 1-2 mL of methanol, sealing the mixture in a reaction kettle, reacting for 5-7 days in a drying box at 140 ℃ and 160 ℃, naturally cooling to room temperature, filtering the mixed solution, washing the filtered yellow block with ethanol for 2-3 times, and drying for 1-2 hours in a vacuum drying box at 80 ℃ to obtain the complex [ N-Me-MePy]Cu2I3Yellow crystals of (4).
3. Use of the CuI complex of claim 1 or 2, wherein the complex can emit red light at 702nm, has a linear relationship between the luminous intensity and the temperature in the range of 80-220K, and can be used as a fluorescent temperature sensing material.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804023A (en) * | 2015-05-12 | 2015-07-29 | 哈尔滨工业大学 | Thermotropic fluorescent color-variable coordination polymer containing [Cu414]n clusters as well as synthesis method and application thereof |
| CN106588981A (en) * | 2017-01-19 | 2017-04-26 | 福州大学 | Temperature-sensitive fluorescent photochromic material with high quantum yield |
| CN106867503A (en) * | 2017-03-18 | 2017-06-20 | 福州大学 | Reversible force/heat/solvent multiple stimulation responsive materials that cuprous iodide/tri- (4 chlorphenyl) phosphine is constructed and preparation method thereof |
| CN108456217A (en) * | 2018-03-23 | 2018-08-28 | 南京晓庄学院 | A kind of fluorescence temperature measuring appliance hybrid material and preparation method and application |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804023A (en) * | 2015-05-12 | 2015-07-29 | 哈尔滨工业大学 | Thermotropic fluorescent color-variable coordination polymer containing [Cu414]n clusters as well as synthesis method and application thereof |
| CN106588981A (en) * | 2017-01-19 | 2017-04-26 | 福州大学 | Temperature-sensitive fluorescent photochromic material with high quantum yield |
| CN106867503A (en) * | 2017-03-18 | 2017-06-20 | 福州大学 | Reversible force/heat/solvent multiple stimulation responsive materials that cuprous iodide/tri- (4 chlorphenyl) phosphine is constructed and preparation method thereof |
| CN108456217A (en) * | 2018-03-23 | 2018-08-28 | 南京晓庄学院 | A kind of fluorescence temperature measuring appliance hybrid material and preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| "A Family of Highly Efficient CuI-Based Lighting Phosphors Prepared by a Systematic, Bottom-up Synthetic Approach";Wei Liu et al.,;《J. Am. Chem. Soc.》;20150707;第137卷(第29期);第9400-9408页 * |
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