CN116622079A - Single-component white light coordination polymer - Google Patents
Single-component white light coordination polymer Download PDFInfo
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- 239000013256 coordination polymer Substances 0.000 title claims abstract description 57
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 57
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims abstract description 22
- 230000005284 excitation Effects 0.000 claims abstract description 11
- 239000001530 fumaric acid Substances 0.000 claims abstract description 11
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 11
- CEJJXIXKGPQQNG-UHFFFAOYSA-N 4-(1-oxidopyridin-4-ylidene)pyridin-1-ium 1-oxide Chemical compound C1=CN([O-])C=CC1=C1C=C[N+](=O)C=C1 CEJJXIXKGPQQNG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 13
- 239000013078 crystal Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000004729 solvothermal method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- -1 znSO 4 ·7H 2 O Chemical compound 0.000 claims description 3
- 239000002178 crystalline material Substances 0.000 abstract description 5
- 238000009877 rendering Methods 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 230000009977 dual effect Effects 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000012621 metal-organic framework Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- AICOOMRHRUFYCM-ZRRPKQBOSA-N oxazine, 1 Chemical compound C([C@@H]1[C@H](C(C[C@]2(C)[C@@H]([C@H](C)N(C)C)[C@H](O)C[C@]21C)=O)CC1=CC2)C[C@H]1[C@@]1(C)[C@H]2N=C(C(C)C)OC1 AICOOMRHRUFYCM-ZRRPKQBOSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 239000013094 zinc-based metal-organic framework Substances 0.000 description 1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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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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- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1516—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising organic material
- G02F1/15165—Polymers
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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Abstract
The application discloses a single-component white light coordination polymer, the chemical formula of which is [ Zn (bpdo) (fum) (H) 2 O) 2 ] n Wherein bpdo represents 4,4 '-bipyridine-N, N' -dioxide, fum represents fumaric acid; the structural unit of the single-component white light coordination polymer is triclinic system, the space group is P1, and the unit cell parameter isα= 87.312 (7) °, β= 82.988 (8) °, γ= 73.760 (8) °. The application synthesizes the single-component white light coordination polymer by one-step solvothermal reactionA crystalline material of a compound; white light can be emitted in the excitation wavelength range of 320-370nm, and the white light gradually changes from pink to yellow-green in 5min under the irradiation of a 200W xenon lamp; has the dual functions of emitting high color rendering index white light and photochromism.
Description
Technical Field
The application relates to the technical field of metal complexes, in particular to a single-component white light coordination polymer.
Background
White light emitting diodes have attracted considerable attention due to their energy saving and device miniaturization advantages in solid state lighting and display. Three typical methods of implementing white light emitting diodes are used: 1) combining red, green, blue (RGB) LED chips, 2) coating yellow phosphor on the blue LED chip, 3) coating a mixture of RGB phosphor on the ultraviolet LED chip. The stacking method of the blue, green and red three primary color luminescent layers has the defects of complex preparation process, high cost, poor stability of luminescent color to voltage and low luminescent quantum yield due to self-absorption of a multilayer structure; the dye doping method is disadvantageous in that it is realized. The dye doping method has the defects that higher energy transfer efficiency between the host luminescent material and the guest dye material is difficult to realize, so that the light emission of the guest dye is influenced, in addition, the influence of dye concentration and applied voltage on the light emission color and efficiency is great, and the problems of poor light emission chromaticity, low efficiency and the like can be caused if the concentration is not well controlled. The disadvantage of the composite method is that it is combined with other methods to achieve white light emission, and a white light emitting device cannot be obtained by simply using an exciplex or adding a hole blocking layer.
The single-component white light emitting material not only overcomes the defects, but also has the advantages of simple preparation, high color reproducibility and the like, and is attracting attention in recent years. Metal-organic frameworks (MOFs) are an emerging crystalline material with a rich and diverse structure, which makes them have great advantages in the fields of catalysis, gas capture and purification, magnetism, etc. Luminescent MOFs (LMOF) have shown various applications such as optoelectronic devices and sensors. The study of Zn-MOFs as luminescence sensors has also attracted attention, for example, xie Yang et al (synthetic chemistry, 2020, 28 (7), 632-636) studied the synthesis of novel zinc (II) coordination polymers and their near-white light temperature sensing properties, and synthesized a novel Zn (II) complex [ Zn 2 (L) 2 (bpe) 2 ]n, the complex has a strong emission peak at 550nm at an excitation wavelength of 380 nm. However, if the zinc coordination polymer is used for industrial production, a novel single-component white light material needs to be developed, which has very important and urgent significance for improving the performance of the white light emitting diode.
Disclosure of Invention
In view of the above prior art, it is an object of the present application to provide a one-component white light coordination polymer. The application synthesizes the single-component white light coordination polymer crystalline material by one-step solvothermal reaction; the compound can emit white light in the excitation wavelength range of 320-370nm and has high color rendering index.
In order to achieve the above purpose, the application adopts the following technical scheme:
in a first aspect of the present application, there is provided a one-component white light coordination polymer having the chemical formula [ Zn (bpdo) (fum) (H) 2 O) 2 ] n Wherein bpdo represents 4,4 '-bipyridine-N, N' -dioxide and fum represents fumaric acid.
Preferably, the structural unit of the single-component white light coordination polymer is a triclinic system, the space group is P1, and the unit cell parameter isα＝87.312(7)°，β＝82.988(8)°，γ＝73.760(8)°。
Preferably, the unit cell volume of the one-component white light coordination polymer
Preferably, the number of molecules in the unit cell of the single-component white light coordination polymer is z=1.
Preferably, the single component white light coordination polymer emits white light in the excitation wavelength range of 320-370 nm.
More preferably, the single-component white light coordination polymer has a color coordinate (0.24,0.25) at a laser wavelength of 330nm, a color temperature of 91.3, a color coordinate (0.24,0.25) at a laser wavelength of 340nm, a color temperature of 92.1, a color coordinate (0.25,0.26) at a laser wavelength of 350nm, a color temperature of 91.8, a color coordinate (0.26,0.27) at a laser wavelength of 360nm, a color temperature of 90.7, a color coordinate (0.27,0.30) at a laser wavelength of 370nm, and a color temperature of 88.4.
Preferably, the single-component white light coordination polymer changes color under the irradiation of a 200W xenon lamp: gradually changing from pink to yellow-green within 5 min.
In a second aspect of the present application, there is provided a method for preparing the above single-component white light coordination polymer, the method comprising:
combining 4,4 '-bipyridine-N, N' -dioxide, fumaric acid and ZnSO 4 ·7H 2 O is added into a mixed solution composed of DMF, absolute ethyl alcohol and distilled water to carry out solvothermal reaction, and pink blocky crystals are obtained by filtering, namely the single-component white light coordination polymer.
Preferably, the 4,4 '-bipyridine-N, N' -dioxide, fumaric acid, znSO 4 ·7H 2 O, DMF, absolute ethanol and distilled water were added in a ratio of 0.1mmol:0.1mmol:0.094mmol:3mL:3mL:3mL.
Preferably, the solvothermal reaction is carried out at a temperature of 80-100 ℃ for 12-36 hours.
In a third aspect of the present application, there is provided the use of a single component white light coordination polymer in the preparation of a white light emitting device and in the preparation of a photochromic device.
The application has the beneficial effects that:
the application synthesizes the single-component white light coordination polymer crystalline material by one-step solvothermal reaction; the compound can emit white light in the excitation wavelength range of 320-370nm and has high color rendering index. Meanwhile, the single-component white light coordination polymer crystalline material prepared by the application can generate photochromism under the irradiation of a 200W xenon lamp, thereby realizing the dual functions of emitting high-color-rendering-index white light and photochromism.
Drawings
Fig. 1: a crystal structure diagram of the single-component white light coordination polymer;
fig. 2: XRD pattern of single-component white light coordination polymer;
fig. 3: thermal gravimetric curve of single-component white light coordination polymer under nitrogen atmosphere;
fig. 4: white light photograph of single-component white light coordination polymer under irradiation of 365nm ultraviolet lamp and corresponding color code coordinate (c) of (a) and (b) compound 1.
Fig. 5: photograph (a) and solid ultraviolet spectrum (b) of the single-component white light coordination polymer under different illumination time.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background section, the zinc coordination polymers of the prior art only emit near white light and have poor color rendering. Based on this, it was an object of the present application to provide a one-component white light coordination polymer. In the crystal structure of the single-component white light coordination polymer of the present application as shown in fig. 1, in the crystal structure of the zinc metal coordination polymer of the present application, each Zn (II) ion is coordinately bound with two fumaric acid ligands, two 4,4 '-bipyridine-N, N' -dioxide ligands, and two water molecules to form a two-dimensional layered structure. Wherein fumaric acid is used as an electron donor, 4 '-bipyridine-N, N' -dioxide is used as an electron acceptor, and photoinduced electron transfer can occur under the excitation of a xenon lamp light source, so that a photochromic function is generated. Meanwhile, due to the coordination synergistic effect of fumaric acid, 4 '-bipyridine-N, N' -dioxide and Zn (II) ions, the white light emitting function can be generated under the excitation of ultraviolet light in the range of 320-370 nm.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present application, the technical scheme of the present application will be described in detail with reference to specific embodiments.
The test materials used in the examples of the present application are all conventional in the art and are commercially available.
Examples
4,4 '-bipyridine-N, N' -dioxide (bpdo, 0.1mmol,20 mg), fumaric acid (fum, 0.1mmol,11 mg) and ZnSO 4 ·7H 2 O (0.094 mmol,27 mg) was added to a mixed solution of 3mL DMF,3mL absolute ethanol and 3mL distilled water, and the mixture was placed in a 17mL stainless steel reaction vessel and reacted at 90℃for 1 day, followed by filtration to obtain pink bulk crystals.
Characterization:
selecting proper size monocrystal during the measurement of zinc metal coordination polymer crystal structure, placing on Gemi E/xx-9100CCD X-ray diffractometer with graphite monochromator (Agilent Gemi E/xx-9100CCD four-circle monocrystal diffractometer in U.S.), and measuring the crystal structure by Cu K α (λ= 1.54184 nm) rays, data were collected in an ω/2θ scan at 293 (2) K. All diffraction intensity data are corrected by LP factors and empirical absorption, a crystal structure is solved by a direct method, the structure analysis work is completed by using an Olex 2 program, and the full matrix least square method F is carried out on the coordinates and anisotropic parameters of all non-hydrogen atoms 2 And (5) finishing.
The crystallographic data of the single-component white light coordination polymer prepared in the examples are shown in table 1.
TABLE 1
Note that: a R 1 ＝∑||F o |–|F c ||/∑|F o |； b ωR 2 ＝{∑ω[(F o ) 2 –(F c ) 2 ] 2 /∑ω[(F o ) 2 ] 2 } 1/2 。
the purity (experimental peak) of the single-component white light coordination polymer prepared in the example can be demonstrated by comparison with the simulated X-ray powder peak, as shown in fig. 2. The prepared zinc metal coordination polymer sample is a pure phase. The single-component white light coordination polymer prepared in the example can be stabilized to at least 185 ℃ (as shown in figure 3), which shows that the prepared zinc metal coordination polymer sample has high thermal stability.
Note that: the experimental peak is obtained by testing the single-component white light coordination polymer prepared in the embodiment by an X-ray powder diffractometer; the simulated peak was obtained by converting the single crystal cif file by Mercury software, which can be compared to indicate whether the bulk of the synthesized crystalline powder is pure phase.
Test example 1: white light emission test
The coordination polymers prepared in the examples are respectively placed in FLS1000 fluorescence spectrometers, 5 fluorescence emission spectrums are obtained through testing at excitation wavelengths of 330nm, 340nm, 350nm, 360nm and 370nm, and color scale coordinates and color temperatures obtained through processing and converting emission spectrum data through CIE camera-version 3 software are shown in tables 2 and 4.
TABLE 2
| Excitation wavelength (nm) | Color coordinates | Color temperature |
| 330 | (0.24,0.25) | 91.3 |
| 340 | (0.24,0.25) | 92.1 |
| 350 | (0.25,0.26) | 91.8 |
| 360 | (0.26,0.27) | 90.7 |
| 370 | (0.27,0.30) | 88.4 |
As can be seen from Table 2 and FIG. 4, the complex prepared by the present application can emit white light at an excitation wavelength of 330-370 nm, and the color coordinates thereof are in the white light range and have a high color rendering index.
The coordination polymer prepared in the example was irradiated by 365nm ultraviolet lamp to emit white light, see FIG. 4 (b).
Test example 2: photochromic test
The coordination polymer prepared in the example was put into the shape of an octave, and the octave was irradiated with a 200W xenon lamp to simulate sunlight, and as can be seen from fig. 5 (a), the note was changed from pink to yellow after 1min of irradiation, and from pink to yellowish green after 5min of irradiation. Accordingly, as shown in FIG. 5 (b), the ultraviolet absorption spectrum is gradually increased in the range of 400-1200 nm. The single-component white light coordination polymer prepared by the application has photochromic performance.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A single-component white light coordination polymer is characterized in that the chemical formula of the single-component white light coordination polymer is [ Zn (bpdo) (fum) (H) 2 O) 2 ] n Wherein bpdo represents 4,4 '-bipyridine-N, N' -dioxide and fum represents fumaric acid.
2. The one-component white light coordination polymer of claim 1, wherein the one-component white light coordination polymer has a triclinic structure, a space group of P1, and a unit cell parameter of α＝87.312(7)°，β＝82.988(8)°，γ＝73.760(8)°。
3. The one-component white light coordination polymer of claim 1, wherein the unit cell volume of the one-component white light coordination polymer
4. The one-component white light coordination polymer of claim 1, wherein the number of molecules in the unit cell of the one-component white light coordination polymer z=1.
5. The single component white light coordination polymer of claim 1 wherein said single component white light coordination polymer emits white light in the excitation wavelength range of 320-370 nm.
6. The one-part white light coordination polymer of claim 1, wherein the one-part white light coordination polymer changes color upon irradiation with a 200W xenon lamp: gradually changing from pink to yellow-green within 5 min.
7. The method for preparing the single-component white light coordination polymer as claimed in claim 1, which is characterized in that the method comprises the following steps:
combining 4,4 '-bipyridine-N, N' -dioxide, fumaric acid and ZnSO 4 ·7H 2 O is added into a mixed solution composed of DMF, absolute ethyl alcohol and distilled water to carry out solvothermal reaction, and pink blocky crystals are obtained by filtering, namely the single-component white light coordination polymer.
8. The preparation method according to claim 7, wherein the 4,4 '-bipyridine-N, N' -dioxide, fumaric acid, znSO 4 ·7H 2 O, DMF, absolute ethanol and distilled water were added in a ratio of 0.1mmol:0.1mmol:0.094mmol:3mL:3mL:3mL.
9. The method according to claim 7, wherein the solvothermal reaction is carried out at a temperature of 80 to 100 ℃ for a period of 12 to 36 hours.
10. Use of the one-component white light coordination polymer according to any one of claims 1 to 6 for the preparation of white light emitting devices and for the preparation of photochromic devices.
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