CN115536052B - Fluoride nano rod, preparation method thereof and application thereof in liquid light valve - Google Patents
Fluoride nano rod, preparation method thereof and application thereof in liquid light valve Download PDFInfo
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- CN115536052B CN115536052B CN202211198921.4A CN202211198921A CN115536052B CN 115536052 B CN115536052 B CN 115536052B CN 202211198921 A CN202211198921 A CN 202211198921A CN 115536052 B CN115536052 B CN 115536052B
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- 239000002073 nanorod Substances 0.000 title claims abstract description 57
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 18
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 13
- -1 nitric acid compound Chemical class 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 229910017855 NH 4 F Inorganic materials 0.000 claims abstract description 4
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 4
- 239000000725 suspension Substances 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 11
- 239000003292 glue Substances 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 125000002947 alkylene group Chemical group 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000000975 co-precipitation Methods 0.000 claims description 3
- 238000004729 solvothermal method Methods 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 abstract description 16
- 230000005684 electric field Effects 0.000 abstract description 14
- 230000001965 increasing effect Effects 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 11
- 239000011259 mixed solution Substances 0.000 description 9
- PMBXCGGQNSVESQ-UHFFFAOYSA-N 1-Hexanethiol Chemical compound CCCCCCS PMBXCGGQNSVESQ-UHFFFAOYSA-N 0.000 description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- LDWZIXQSZWFRGT-UHFFFAOYSA-N gadolinium(3+);trinitrate;hydrate Chemical compound O.[Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O LDWZIXQSZWFRGT-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- PXRKCOCTEMYUEG-UHFFFAOYSA-N 5-aminoisoindole-1,3-dione Chemical compound NC1=CC=C2C(=O)NC(=O)C2=C1 PXRKCOCTEMYUEG-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000002591 computed tomography Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 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
- 239000002077 nanosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004984 smart glass Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- WUVRZBFIXJWTGS-UHFFFAOYSA-N yttrium(3+);trinitrate;hydrate Chemical compound O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O WUVRZBFIXJWTGS-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/36—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 halogen being the only anion, e.g. NaYF4
-
- 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
- G02F1/165—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 translational movement of particles in a fluid under the influence of an applied field
- G02F1/166—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 translational movement of particles in a fluid under the influence of an applied field characterised by the electro-optical or magneto-optical effect
-
- 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
- G02F1/165—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 translational movement of particles in a fluid under the influence of an applied field
- G02F1/166—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 translational movement of particles in a fluid under the influence of an applied field characterised by the electro-optical or magneto-optical effect
- G02F1/167—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 translational movement of particles in a fluid under the influence of an applied field characterised by the electro-optical or magneto-optical effect by electrophoresis
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Nonlinear Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Analytical Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention provides a fluoride nano rod, a preparation method thereof and application thereof in a liquid light valve, wherein the fluoride is AREF 4 Wherein A is selected from any one of Li, na, K, rb; RE is selected from any plurality of Y, la, gd, lu; the preparation method comprises the following steps: (1) Dissolving a hydrated nitric acid compound of RE in water, then adding hydroxide of A, and regulating the pH value of the solution to 7-11; (2) Adding ethylenediamine tetraacetic acid into the solution, stirring for 20-60 min, and then adding NH 4 F, uniformly stirring; (3) And (3) reacting the solution obtained in the step (2) to obtain the fluoride nano-rod. The fluoride nanorod has regular appearance, uniform size and excellent physical and chemical stability, and can enable the SPD light valve to be changed into an on-state from shading. The incident light transmittance can be adjusted in a larger range under the action of an electric field, the average transmittance increasing effect is better, and the sensitivity of the SPD light valve is obviously increased.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a fluoride nano rod, a preparation method thereof and application thereof in a liquid light valve.
Background
Rare earth fluorides have low phonon energy, good chemical stability, and have wide applications as excellent optical materials, including light emission, bio-tags, displays, lasers, and the like. In particular, hexagonal phase rare earth fluorides, naGdF4 crystals have attracted scholars' research interest. On the one hand, the NaGdF4 matrix shows good paramagnetic relaxation properties, which are attributed to Gd 3+ The 7 unpaired electrons in the ion give rise to its great potential (CT) and Magnetic Resonance Imaging (MRI) applications as an x-ray computed tomography multifunctional material. On the other hand, the magnetic particle has stronger internal dipole moment, and the direction of particles can be changed under the action of an electric field, so that the magnetic particle has great potential in the fields of intelligent windows and the like.
The synthesis strategies for preparing rare earth fluoride nano rods in the prior art are various, and comprise solid phase reaction, hydrothermal/solvothermal synthesis, chemical coprecipitation method and the like. The morphology of the synthesized crystals by the high-temperature solid phase method is not controllable and is easy to agglomerate; most of the samples are prepared by adopting citric acid, amino acid and other auxiliary hydrothermal methods to regulate the morphology and crystal size, and the prepared samples are rough in surface and uneven in size. Previous studies have shown that the morphology, size and structure of crystalline materials have a great influence on the properties of the materials. Therefore, the exploration of a simple and convenient synthesis method for preparing high-quality fluoride nano rod crystals with uniform size and unique morphology is of great importance.
Suspended Particle Device (SPD) light valves, also known as dipole particle suspended device light valves. SPD light valves have two distinct states, on and off. When an external electric field is applied, the particles polarize and rotate under the torque applied by the electric field and align with the applied electric field. More photons can pass through the medium and the light transmission increases due to the increased alignment of the particles. When the electric field is turned off, the direction of the particles becomes random in the medium, blocking more photons. Unlike most liquid crystal devices, SPDs can be well integrated on low power consumption flexible substrates, so they are advantageous for next generation flexible, low cost smart windows.
Disclosure of Invention
Based on the above, the invention aims to provide a fluoride nano rod, a preparation method thereof and application thereof in a liquid light valve, wherein the preparation method of the fluoride nano rod is simple, the appearance is regular, the size is uniform, and the incident light transmittance can be adjusted in a larger range under the action of an electric field.
In order to achieve the above purpose, the present invention adopts the following technical scheme.
Preparation method of fluoride nano rod, wherein the fluoride is AREF 4 Wherein A is selected from any one of Li, na, K, rb; RE is selected from any plurality of Y, la, gd, lu;
the preparation method comprises the following steps: (1) Dissolving a hydrated nitric acid compound of RE in water, then adding hydroxide of A, and regulating the pH value of the solution to 7-11; (2) Adding ethylenediamine tetraacetic acid into the solution, stirring for 20-60 min, and then adding NH 4 F, uniformly stirring; (3) And (3) reacting the solution obtained in the step (2) to obtain the fluoride nano-rod.
In some embodiments, the a is selected from Na.
In some embodiments, the RE is selected from Y or Gd.
In some embodiments, the hydroxide of A, the hydrated nitric acid compound of RE, NH 4 The mol ratio of F to ethylenediamine tetraacetic acid is (1-2) 1 (6-12) 0.2-0.5.
In some embodiments, the fluoride nanorods are obtained in step (3) using hydrothermal, co-precipitation, solvothermal reactions.
In some embodiments, the fluoride nanorods are obtained in step (3) by a hydrothermal reaction, specifically: and (3) reacting the solution obtained in the step (2) at 160-240 ℃ for 20-30 h, washing, and centrifuging to obtain the fluoride nano rod.
In some embodiments, the pH of the solution is adjusted to 8 to 9 in step (1).
In some embodiments, the pH is adjusted in step (1) using NaOH solution.
The invention also provides the fluoride nano-rod prepared by the method.
The invention also provides an application of the fluoride nano rod prepared by the method in preparing a light valve of a suspended particle device.
The invention also provides a suspended particle device light valve, which comprises two transparent electrodes, an insulating support frame arranged between the two transparent electrodes and a suspension arranged between the two transparent electrodes;
the suspension comprises the fluoride nano-rods prepared by the method and a suspension medium; the mass fraction of the fluoride nano-rods in the suspension is 0.5-5%.
In some preferred embodiments, the mass fraction of the fluoride nanorods in the suspension is 1-3%.
In some embodiments, the suspension medium has a viscosity of 2000cp or less; preferably, the viscosity of the suspension medium is 1000-2000 cp.
In some embodiments, the suspension medium comprises at least one of a siloxane, an acrylic acid, an alkylene oxide monomer, an alkylene oxide polymer; and/or the transparent electrode is at least one selected from ITO conductive glass, ITO conductive film, nano Ag wire conductive film, nano Cu wire conductive film, PEDOT conductive film, graphene conductive film and carbon nano tube conductive film; and/or the insulating support frame is at least one of insulating sheets made of PVC, PET, PI materials; and/or the thickness of the insulating support frame is 100-1000 um.
In some preferred embodiments, the suspension medium comprises an acrylic polymer.
The invention also provides a preparation method of the light valve of the suspended particle device, which comprises the following steps:
(1) Configuring the suspension medium; (2) Adding the fluoride nano-rods into the suspension medium to obtain a suspension; (3) Taking two transparent electrodes, placing the insulating support frame between the two transparent electrodes, and fixing the two transparent electrodes by using insulating glue; (4) And (3) placing the suspension liquid between two transparent electrodes, and sealing to obtain the light valve of the suspended particle device.
In some embodiments, the fluoride nanorods are NaGdF 4 Nanorods or NaYF 4 A nanorod.
The invention provides a fluoride nano-rod and a preparation method thereof, and the inventor surprisingly discovers that EDTA is adopted as a chelating agent, and forms a precursor with hydroxide of A and hydrated nitric acid compound of RE, and then forms a precursor with NH 4 F, reacting to prepare fluoride nano rod crystals with regular appearance, uniform size and good dispersibility. This is probably because EDTA can better aid the coordination of atoms or ions in the starting materials and thus link better together to form fluoride nanorods of a specific morphology and size.
The fluoride nanorod has regular appearance, uniform size, excellent physical and chemical stability and stronger dipole moment in the interior, and the characteristics enable the fluoride nanorod to be directionally arranged under the action of an electric field and perpendicular to electrodes, so that the SPD light valve can be converted from a shading state to an on state, the transmittance of incident light can be adjusted to a larger extent under the action of the electric field, the average transmittance increasing effect is better, the sensitivity of the SPD light valve is obviously increased, and the development of an intelligent window is enabled to enter a new stage.
Drawings
FIG. 1 shows NaGdF obtained by the preparation of example 1 4 Morphology of nanorods.
Fig. 2 is a graph showing the result of detecting the light transmittance of the SPD light valve prepared in example 1 in the on and off states.
Fig. 3 is a schematic diagram of the SPD light valve prepared in example 1 in on and off states.
FIG. 4 is a NaYF obtained by the preparation of example 2 4 Morphology of nanorods.
Fig. 5 is a graph showing the result of detecting the light transmittance of the SPD light valve prepared in example 2 in the on and off states.
FIG. 6 shows NaGdF obtained by the comparative example 4 Morphology of nanorods.
Fig. 7 is a graph of the transmittance detection result of the SPD light valve prepared in the comparative example in the on and off states.
Detailed Description
The experimental methods of the present invention, in which specific conditions are not specified in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The various chemicals commonly used in the examples are commercially available.
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 invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The terms "comprising" and "having" and any variations thereof, are intended to cover a non-exclusive inclusion. For example, a process, method, apparatus, article, or device that comprises a list of steps is not limited to the elements or modules listed but may alternatively include additional steps not listed or inherent to such process, method, article, or device.
In the present invention, the term "plurality" means two or more. "and/or", describes an association relationship of an association object, and indicates that there may be three relationships, for example, a and/or B, and may indicate: a exists alone, A and B exist together, and B exists alone. The character "/" generally indicates that the context-dependent object is an "or" relationship.
The following description is made with reference to specific embodiments.
Example 1
The present embodiment provides a NaGdF 4 Nanorods and SPD light valve containing same, naGdF 4 The preparation method of the nanorod and SPD light valve comprises the following steps:
1. gadolinium nitrate hydrate (Gd (NO) 3 ) 3 ·5H 2 O) dissolving in 20mL of deionized water, fully and uniformly stirring, and dripping 4mL of NaOH solution with the concentration of 1 mol/L;
2. 1mmol of ethylenediamine tetraacetic acid (EDTA) was added to the mixed solution, stirring was continued for 30 minutes, and then 8ml of NH with a concentration of 2mol/L was added 4 F, continuously stirring the solution for 30min;
3. transferring the obtained liquid into a hydrothermal kettle, and then placing the hydrothermal kettle in a constant-temperature drying oven at 180 ℃ for reaction for 24 hours;
4. after the hydrothermal reaction is finished, washing and centrifuging the reaction product for 2-4 times respectively by using water and ethanol, and then drying to obtain the NaGdF 4 A nanorod;
5. 24.4g of lauryl methacrylate, 0.6g of hydroxypropyl methacrylate and 30g of toluene were uniformly mixed in a two-necked flask, and 2g of hexanethiol was added to the obtained mixed solution;
6. 10g of toluene solution containing 0.2g of azobisisobutyronitrile was uniformly mixed with the above organic mixed solution and stirred in N 2 Under the protection, carrying out polymerization reaction for 18 hours at 60 ℃ to obtain a suspension medium with the viscosity of about 1600 cp;
7. the NaGdF is subjected to 4 The nano rods are mixed in a suspending medium in an ultrasonic and stirring mode according to the mass fraction of 2% to obtain a suspending liquid;
8. inserting a PVC transparent frame with the thickness of 200 mu m between two pieces of ITO conductive glass, and fixing the two pieces of ITO conductive glass by using insulating glue;
9. and (3) taking a proper amount of suspension, filling the space between two layers of ITO conductive glass by using a syringe, and packaging by using insulating glue to obtain the SPD light valve.
As shown in FIG. 1, the NaGdF 4 The nano rod has regular shape and uniform size, the length is 600-800 nm, and the diameter is less than 100 nm.
The SPD light valve was detected to have an average transmittance of 13.3% for light in the wavelength range of 200-900 nm in the "OFF" state, and an average transmittance of about 26.5% for light in the "ON" state after a 220V voltage was applied thereto (fig. 2). As shown in FIG. 3, the NaGdF when an external electric field is applied 4 The nanorod particles polarize and rotate under the torque applied by the electric field and align with the applied electric field. Due to the increased alignment of the particles, more photons can pass through the medium and thus the light transmission increases. When the electric field is turned off, the direction of the particles becomes random in the medium, blocking more photons.
Example 2
The present embodiment provides a method ofNaYF 4 Nanorods and SPD light valve containing same, naYF 4 The preparation method of the nanorod and SPD light valve comprises the following steps:
1. 2mmol of yttrium nitrate hydrate (Y (NO) 3 ) 3 ·5H 2 O) dissolving in 20mL of deionized water, fully and uniformly stirring, and dripping 4mL of NaOH solution with the concentration of 1 mol/L;
2. 1mmol of ethylenediamine tetraacetic acid (EDTA) was added to the mixed solution, stirring was continued for 30 minutes, and then 8ml of NH with a concentration of 2mol/L was added 4 F, continuously stirring the solution for 30min;
3. transferring the obtained liquid into a hydrothermal kettle, and then placing the hydrothermal kettle in a constant-temperature drying oven at 180 ℃ for reaction for 24 hours;
4. after the hydrothermal reaction is finished, washing and centrifuging the reaction product for 2-4 times respectively by using water and ethanol, and then drying to obtain the NaYF 4 The length of the nanorods is 1000-1200nm, and the diameter is below 200nm, as shown in figure 4;
5. 24.4g of lauryl methacrylate, 0.6g of hydroxypropyl methacrylate and 30g of toluene were uniformly mixed in a two-necked flask, and 2g of hexanethiol was added to the obtained mixed solution;
6. 10g of toluene solution containing 0.2g of azobisisobutyronitrile was uniformly mixed with the above organic mixed solution and stirred in N 2 Under the protection, carrying out polymerization reaction for 18 hours at 60 ℃ to obtain a suspension medium with the viscosity of about 1600 cp;
7. the NaYF is processed 4 The nano rods are mixed in a suspending medium in an ultrasonic and stirring mode according to the mass fraction of 2% to obtain a suspending liquid;
8. inserting a PVC transparent frame with the thickness of 200 mu m between two pieces of ITO conductive glass, and fixing the two pieces of ITO conductive glass by using insulating glue;
9. and (3) taking a proper amount of suspension, filling the space between two layers of ITO conductive glass by using a syringe, and packaging by using insulating glue to obtain the SPD light valve.
The light valve was detected to have an average transmittance of 14.9% for light in the wavelength range of 200 to 00nm in the "OFF" state, and an average transmittance of about 25.9% for light in the "ON" state after a 220V voltage was applied thereto (fig. 5).
Comparative example
This comparative example provides a NaGdF 4 Nanoparticle and SPD light valve containing same, naGdF 4 The preparation method of the nanorods comprises the following steps in the same manner as in example 1 except that EDTA is replaced by citric acid:
1. gadolinium nitrate hydrate (Gd (NO) 3 ) 3 ·5H 2 O) dissolving in 20mL of deionized water, fully and uniformly stirring, and dripping 4mL of NaOH solution with the concentration of 1 mol/L;
2. 1mmol of Citric Acid (CA) was added to the mixed solution, stirring was continued for 30min, and 8ml of NH with a concentration of 2mol/L was added 4 F, continuously stirring the solution for 30min;
3. transferring the obtained liquid into a hydrothermal kettle, and then placing the hydrothermal kettle in a constant-temperature drying oven at 180 ℃ for reaction for 24 hours;
4. after the hydrothermal reaction is finished, washing and centrifuging the reaction product for 2-4 times respectively by using water and ethanol, and then drying to obtain NaGdF with uneven size 4 Nanorods or nanospheres with a length of 100-500nm and a diameter below 100nm, as shown in FIG. 6;
5. 24.4g of lauryl methacrylate, 0.6g of hydroxypropyl methacrylate and 30g of toluene were uniformly mixed in a two-necked flask, and 2g of hexanethiol was added to the obtained mixed solution;
6. 10g of toluene solution containing 0.2g of azobisisobutyronitrile was uniformly mixed with the above organic mixed solution and stirred in N 2 Under the protection, carrying out polymerization reaction for 18 hours at 60 ℃ to obtain a suspension medium with the viscosity of about 1600 cp;
7. the NaGdF is subjected to 4 The nano particles are mixed in a suspension medium in an ultrasonic and stirring mode according to the mass fraction of 2%, so as to obtain a suspension;
8. inserting a PVC transparent frame with the thickness of 200 mu m between two pieces of ITO conductive glass, and fixing the two pieces of ITO conductive glass by using insulating glue;
9. and (3) taking a proper amount of suspension, filling the space between two layers of ITO conductive glass by using a syringe, and packaging by using insulating glue to obtain the SPD light valve.
The average transmittance of the SPD light valve for light in the wavelength range of 200 to 900nm in the "OFF" state is 15.2%, and after 220V voltage is applied thereto, that is, in the "ON" state, the average transmittance of the light increases to about 18.0% (fig. 7).
In conclusion, the fluoride nanorod prepared by using EDTA has regular morphology, uniform size and excellent physical and chemical stability, the SPD light valve can be converted from shading to on-state, the incident light transmittance can be adjusted in a larger range under the action of an electric field, and the average transmittance increasing effect is better.
The technical features of the above embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (9)
1. Use of a fluoride nanorod for the preparation of a light valve of a suspended particle device, wherein the fluoride is AREF 4 Wherein A is selected from any one of Li, na, K, rb; RE is selected from Y or Gd;
the preparation method of the fluoride nano rod comprises the following steps: (1) Dissolving a hydrated nitric acid compound of RE in water, then adding hydroxide of A, and adjusting the pH value of the solution to 7-11; (2) Adding ethylenediamine tetraacetic acid into the solution, stirring for 20-60 min, and then adding NH 4 F, uniformly stirring; (3) And (3) reacting the solution obtained in the step (2) to obtain the fluoride nano-rod.
2. The method of claim 1, wherein the fluoride nanorods are used in preparing a light valve of a suspended particle deviceThe application of (2) is characterized in that the hydroxide of A, the hydrated nitric acid compound of RE and NH 4 The mol ratio of F to ethylenediamine tetraacetic acid is (1-2) 1 (6-12) 0.2-0.5.
3. The use of the fluoride nanorods according to claim 1 for preparing a light valve of a suspended particle device, wherein the fluoride nanorods are obtained in the step (3) by a hydrothermal method, a coprecipitation method or a solvothermal method.
4. The use of the fluoride nanorods according to claim 1 for preparing a light valve of a suspended particle device, wherein the fluoride nanorods are obtained by a hydrothermal reaction in the step (3), specifically: and (3) reacting the solution obtained in the step (2) at 160-240 ℃ for 20-30 hours, washing, and centrifuging to obtain the fluoride nanorod.
5. The light valve of the suspended particle device is characterized by comprising two transparent electrodes, an insulating supporting frame arranged between the two transparent electrodes and a suspension arranged between the two transparent electrodes;
the suspension comprising the fluorochemical nanorods of any of claims 1 to 4 and a suspension medium; and the mass fraction of the fluoride nano rods in the suspension is 0.5-5%.
6. The suspended particle device light valve of claim 5, wherein the viscosity of the suspending medium is below 2000cp.
7. The suspended particle device light valve of claim 6, wherein the viscosity of the suspending medium is 1000-2000 cp.
8. The suspended particle device light valve of claim 5, wherein the suspending medium comprises at least one of a siloxane, an acrylic, an alkylene oxide monomer, and an alkylene oxide polymer; and/or the transparent electrode is at least one selected from ITO conductive glass, ITO conductive film, nano Ag wire conductive film, nano Cu wire conductive film, PEDOT conductive film, graphene conductive film and carbon nano tube conductive film; and/or the insulating support frame is at least one of insulating sheets made of PVC, PET, PI materials; and/or the thickness of the insulating support frame is 100-1000.
9. The method for preparing a light valve for a suspended particle device according to any one of claims 5 to 8, comprising the steps of: (1) configuring the suspension medium; (2) Adding the fluoride nano-rods into the suspension medium to obtain a suspension; (3) Taking two transparent electrodes, placing the insulating support frame between the two transparent electrodes, and fixing the two transparent electrodes by using insulating glue; (4) And (3) placing the suspension liquid between two transparent electrodes, and sealing to obtain the light valve of the suspended particle device.
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