CN115558130B - Double-refraction-adjustable optical hydrogel and preparation method and application thereof - Google Patents
Double-refraction-adjustable optical hydrogel and preparation method and application thereof Download PDFInfo
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- CN115558130B CN115558130B CN202211199024.5A CN202211199024A CN115558130B CN 115558130 B CN115558130 B CN 115558130B CN 202211199024 A CN202211199024 A CN 202211199024A CN 115558130 B CN115558130 B CN 115558130B
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- 230000003287 optical effect Effects 0.000 title claims abstract description 82
- 239000000017 hydrogel Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 197
- 239000004973 liquid crystal related substance Substances 0.000 claims abstract description 99
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 81
- 238000009830 intercalation Methods 0.000 claims description 26
- 230000002687 intercalation Effects 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 16
- 229910017052 cobalt Inorganic materials 0.000 claims description 15
- 239000010941 cobalt Substances 0.000 claims description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 11
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 8
- 230000009471 action Effects 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 8
- 239000003504 photosensitizing agent Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 150000007530 organic bases Chemical class 0.000 claims description 6
- 230000010287 polarization Effects 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims description 2
- 230000010365 information processing Effects 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 claims 2
- 230000004044 response Effects 0.000 abstract description 19
- 238000007906 compression Methods 0.000 abstract description 5
- 230000006835 compression Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 30
- 239000000047 product Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 19
- 238000012360 testing method Methods 0.000 description 16
- 238000002834 transmittance Methods 0.000 description 15
- 239000012071 phase Substances 0.000 description 11
- 238000012512 characterization method Methods 0.000 description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229910000428 cobalt oxide Inorganic materials 0.000 description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 125000004386 diacrylate group Chemical group 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
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- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910001414 potassium ion Inorganic materials 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 241000238366 Cephalopoda Species 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910008449 SnF 2 Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003938 response to stress Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- 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
- G02F1/0009—Materials therefor
- G02F1/0063—Optical properties, e.g. absorption, reflection or birefringence
-
- 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
- G02F1/13—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 liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/13363—Birefringent elements, e.g. for optical compensation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2335/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Derivatives of such polymers
- C08J2335/02—Characterised by the use of homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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Abstract
The invention discloses an optical hydrogel with adjustable birefringence, a preparation method and application thereof. The optical hydrogel can control parameters such as optical path, arrangement order degree of the magnetic element doped two-dimensional titanium dioxide liquid crystal and the like through compression or stretching, further can realize continuous and stable modulation of deep ultraviolet light, has simpler modulation operation, easy control, accurate control and quick response time, and has no crosstalk to surrounding devices.
Description
Technical Field
The invention relates to the technical field of optical materials, in particular to an optical hydrogel with adjustable birefringence, a preparation method and application thereof.
Background
By quantitatively regulating and controlling parameters such as amplitude, phase, frequency, polarization state and the like of the light waves, an optical modulation technology can superimpose an external signal carrying information on the carrier light waves, then the optical signal is utilized for information transmission, and the related technology is widely applied to various fields such as precise measurement, precise control, optical storage, information transmission and the like. One of the most important components in light modulation systems is the birefringent optical element, but currently the birefringent optical element operates in a wavelength range that is mainly focused in the visible and near infrared (355 nm-1800 nm) bands, whereas in the deep ultraviolet (lambda <350 nm) band there are fewer relevant reports and much focusing on inorganic optical single crystals.
With the development of scientific technology, it is increasingly important to modulate deep ultraviolet light, and development of a transmission type birefringent element is needed to realize continuous modulation of the shape, polarization and phase of deep ultraviolet pulse without changing the propagation direction of light. In recent years, related researches are developed at home and abroad, and novel deep ultraviolet birefringent single crystals such as Ca (BO 2)2, alpha-SnF 2 and the like) are prepared, but after the shapes and the sizes of the materials are fixed, the birefringent indexes of the single crystal materials are fixed, so that continuous regulation and control of the deep ultraviolet light are difficult, and practical application is limited.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides an optical hydrogel with adjustable birefringence, a preparation method and application thereof.
In a first aspect of the present invention, an optical hydrogel with adjustable birefringence is provided, which includes a hydrogel matrix and a magnetic element doped two-dimensional titania liquid crystal, wherein the hydrogel matrix has a network cross-linked structure, and the magnetic element doped two-dimensional titania liquid crystal is filled in the network cross-linked structure and is arranged in an oriented manner.
The optical hydrogel with adjustable birefringence according to the embodiment of the invention has at least the following beneficial effects: the birefringence-adjustable optical hydrogel comprises a hydrogel matrix with a network cross-linked structure and magnetic element doped two-dimensional titanium dioxide liquid crystals which are directionally arranged and filled in the network cross-linked structure of the hydrogel matrix, and by the aid of the birefringence-adjustable optical hydrogel, parameters such as optical path, arrangement order degree of the magnetic element doped two-dimensional titanium dioxide liquid crystals and the like can be controlled through compression or stretching, further continuous and stable modulation of deep ultraviolet light can be achieved, and compared with magnetic modulation and the like, the mechanical modulation mode has the advantages of being simpler to operate, easy to control, accurate to control, quick in response time, free of crosstalk to surrounding devices and the like.
The optical hydrogel with adjustable birefringence has the working wave band range in deep ultraviolet band (lambda <350 nm), specifically in the wavelength range of 300-350 nm, belongs to stress response optical hydrogel, can realize continuous and stable modulation of deep ultraviolet birefringence through compressive or tensile stress, has a larger phase adjustable range, can adjust and control the phase retardation to be 10-30 degrees, and can solve the problem of photophysical or photochemical degradation of organic liquid crystal under ultraviolet light.
In some embodiments of the present invention, the magnetic element doped in the two-dimensional titanium dioxide liquid crystal is at least one of cobalt, manganese and nickel; cobalt is preferred.
In order to ensure the deep ultraviolet transmissivity and magnetic response sensitivity of the material, the magnetic element doped two-dimensional titanium dioxide liquid crystal generally adopts low-concentration magnetic element doped two-dimensional titanium dioxide liquid crystal. In some embodiments of the present invention, the doping amount of the magnetic element in the magnetic element doped two-dimensional titanium dioxide liquid crystal is controlled to be 3-9% of the molar ratio of the magnetic element to the titanium element, for example, 3%, 5%, 6%, 8%, 9%. By controlling the doping amount of the magnetic element in the above relatively low suitable range, the material can be ensured to have high deep ultraviolet light transmittance and sensitive magnetic response, so that the situation that the birefringence value is smaller due to the too low concentration of the magnetic element, and the material performance is influenced due to the too low transmittance due to the too high concentration of the magnetic element can be avoided.
In some embodiments of the invention, the ratio of the diameter to thickness (i.e., the ratio of the lateral dimension to the thickness) of the magnetic element doped two-dimensional titanium dioxide liquid crystal is above 10 3. Under the large radius-thickness ratio, the magnetic element doped two-dimensional titanium dioxide liquid crystal has sensitive magnetic response characteristic, can complete orientation control under a small magnetic field, and causes larger birefringence.
In some embodiments of the invention, the magnetic element doped two-dimensional titania liquid crystal comprises 10 -4～10-3 wt% of the optical hydrogel. The content of the magnetic element doped two-dimensional titanium dioxide liquid crystal in the optical hydrogel is controlled in the range, so that the optical hydrogel of the product has a high birefringence value and high deep ultraviolet transmittance, and the transmissive and birefringence-adjustable deep ultraviolet optical hydrogel is obtained.
In a second aspect of the present invention, a method for preparing any one of the optical hydrogels with adjustable birefringence according to the first aspect of the present invention is provided, including the following steps:
S1, mixing a magnetic element doped two-dimensional titanium dioxide liquid crystal, a polymer monomer, a photosensitizer and a solvent to prepare a mixed solution;
S2, transferring the mixed solution into a mold, and performing ultraviolet curing under the action of a magnetic field.
In the preparation method, the magnetic element doped two-dimensional titanium dioxide liquid crystal with sensitive magnetic response and high deep ultraviolet transmittance is mixed with polymer monomers, a photosensitizer and a solvent to prepare mixed liquid, the mixed liquid is transferred into a die, the two-dimensional titanium dioxide liquid crystal is solidified into optical hydrogel under the action of a magnetic field by adopting a magnetic auxiliary photo-solidification technology, the magnetic element doped two-dimensional titanium dioxide liquid crystal is directionally arranged along the magnetic field under the action of the magnetic field to form an ordered structure and cause double refraction, and in the solidification process, the ordered structure of the magnetic element doped two-dimensional titanium dioxide liquid crystal arranged along the magnetic field is completely preserved, so that the deep ultraviolet optical hydrogel with adjustable double refraction is prepared, and parameters such as optical path, arrangement order degree of the magnetic element doped two-dimensional titanium dioxide liquid crystal and the like can be controlled by compression or stretching to realize continuous and stable regulation of deep ultraviolet light.
In some embodiments of the invention, step S1 comprises: firstly, mixing magnetic element doped two-dimensional titanium dioxide liquid crystal and a solvent to prepare a liquid crystal solution with the concentration of 10 -4～10-3 wt%, and then adding a polymer monomer accounting for 3-5 wt% of the liquid crystal solution and a photosensitizer accounting for 0.3-1 wt% of the liquid crystal solution to prepare a mixed solution. By diluting the above magnetic element doped two-dimensional titanium dioxide liquid crystal to the above specific concentration, both the sensitive magnetic response and the high deep ultraviolet light transmittance can be ensured. Wherein the polymer monomer can specifically adopt at least one of poly (ethylene glycol) diacrylate and N-isopropyl acrylamide; the photosensitizer may be at least one of potassium persulfate and 2-hydroxy-4' - (2-hydroxyethoxy) -2-methylpropionate.
In some embodiments of the present invention, step S1 is preceded by: s0, preparing the magnetic element doped two-dimensional titanium dioxide liquid crystal by an ion intercalation method.
In some embodiments of the present invention, step S0 specifically includes:
(1) Mixing preparation raw materials comprising titanium dioxide, a magnetic element source and carbonate, and calcining to obtain a calcined product;
(2) Mixing the calcined product with protonic acid, and performing a first intercalation reaction to obtain a first intercalation product;
(3) Mixing the first intercalation product with organic base, and performing a second intercalation reaction to obtain a second intercalation product;
(4) And mechanically stripping the second intercalation product in a liquid phase to obtain the magnetic element doped two-dimensional titanium dioxide liquid crystal.
The magnetic element doped two-dimensional titanium dioxide liquid crystal with a large diameter-thickness ratio can be effectively stripped and prepared by adopting the ion intercalation method, and the obtained magnetic element doped two-dimensional titanium dioxide liquid crystal has excellent magneto-optical response characteristics, high magneto-optical response sensitivity and high birefringence value.
In some embodiments of the present invention, step (1) specifically includes: mixing the preparation raw materials comprising titanium dioxide, a magnetic element source and carbonate, calcining for 5-6 hours at 800-1200 ℃, then taking out and grinding, and then heating to 800-1200 ℃ and calcining for 20-24 hours. Wherein, the first calcination is used for fully reacting the raw materials; a second calcination to grow grains; taking out the grind between the two calcines can improve the uniformity of the material. The carbonate can be at least one of sodium carbonate, potassium carbonate and lithium carbonate, and by adopting the carbonate, metal ions in the carbonate can provide positive charges and are inserted between titanium dioxide layers so as to facilitate the subsequent stripping of the carbonate into a single-layer material; in addition, since the radius of the K + ion is larger than that of Na + and Li + ion, ti 4+ ion in the titanium oxide layer is not replaced, and thus, potassium carbonate is preferably used as the carbonate. The magnetic element source can be at least one of cobalt oxide, manganese oxide and nickel oxide; specifically, the preparation raw materials can comprise titanium dioxide, cobalt oxide, potassium carbonate and lithium carbonate with the molar ratio of elements of K, ti, li, co, O=0.8: [ (5.2-x)/3 ]: [ (0.8-2 x)/3 ]: x:4 and x=0.05-0.15.
In some embodiments of the present invention, in step (2), the protonic acid may be at least one of hydrochloric acid and sulfuric acid. Specifically, the calcined product is mixed with 150-250 mL of protonic acid with the concentration of 1-2M, and the mixture is stirred for 4-5 days by magnetic force, then the mixture is stood for collecting sediment, and then the sediment is washed and dried by deionized water.
In the step (3), the organic base generally adopts organic base with large-particle-size positive ions, so that the positive ions in the organic base are inserted between titanium dioxide layers, and the stripping preparation of a single-layer two-dimensional material is facilitated. In some embodiments of the present invention, in step (3), the organic base may be at least one of tetrabutylammonium hydroxide and quaternary ammonium base. Specifically, the first intercalation product is mixed with the organic amine salt solution and kept stand for 5 to 6 hours to carry out the second intercalation reaction.
In some embodiments of the present invention, in step (4), the mechanical stripping means may be at least one of mechanical shaking and water bath ultrasound. For example, the second intercalation product may be mixed with deionized water and mechanically shaken for 48 to 50 hours.
In a third aspect of the present invention, the use of any of the birefringent tunable optical hydrogels according to the first aspect of the present invention in optical communications, laser polarization techniques, polarization information processing or precision measurement is provided.
In a fourth aspect of the invention, an optical device is provided comprising any of the birefringent tunable optical hydrogels set forth in the first aspect of the invention. The optical device comprises any one of an optical isolator, an optical circulator, a phase retarder and an optical comb filter.
Drawings
The invention is further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is a graph showing the statistical result of the transverse dimensions of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1;
FIG. 2 is a graph showing the thickness statistics of the cobalt-doped two-dimensional titania liquid crystal prepared in example 1;
FIG. 3 is a graph showing the results of the deep ultraviolet transmittance test of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1;
FIG. 4 is a graph showing the magnetic anisotropy test result of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1;
FIG. 5 is a graph showing the magnetic response test results of the cobalt-doped two-dimensional titania liquid crystal prepared in example 1;
FIG. 6 is a graph showing the results of the deep ultraviolet stability test of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1;
FIG. 7 is a graph showing the magnetic response test results of the cobalt-doped two-dimensional titania liquid crystal prepared in example 1 and the cobalt-doped titania liquid crystal prepared in comparative example 1;
FIG. 8 is a graph showing the results of the deep ultraviolet transmittance test of the cobalt-doped two-dimensional titanium dioxide liquid crystals prepared in example 1 and comparative example 3;
FIG. 9 is a schematic diagram showing the preparation process of the optical hydrogel with adjustable birefringence in example 2;
FIG. 10 is a physical view of the optical hydrogel with adjustable birefringence obtained in example 2;
FIG. 11 is a graph showing the pressure-deformation curve of the birefringence-tunable optical hydrogel obtained in example 2;
FIG. 12 is a graph showing tension-strain curves of the birefringence-tunable optical hydrogels prepared in example 2;
FIG. 13 is a graph showing the results of a test for the modulation of deep ultraviolet light by compressing the birefringent tunable optical hydrogel prepared in example 2;
FIG. 14 is a graph showing the results of a test for the modulation of deep ultraviolet light by stretching the birefringent tunable optical hydrogel prepared in example 2;
FIG. 15 is a graph showing the results of repeated compression stability test of the optical hydrogel with tunable birefringence prepared in example 2;
FIG. 16 is a graph showing the results of repeated tensile stability test of the optical hydrogels with tunable birefringence prepared in example 2;
FIG. 17 is a graph showing the results of magnetic response tests of the optical hydrogels with tunable birefringence prepared in example 2 and comparative example 4.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
Example 1
The preparation method of the magnetic element doped two-dimensional titanium dioxide liquid crystal comprises the following steps:
S1, uniformly mixing titanium dioxide, cobalt oxide, potassium carbonate and lithium carbonate in a corundum crucible according to the element molar ratio of K to Ti to Li to O=0.8 to 1.7 to 0.2 to 0.1 to 4, fully grinding, and then heating to 1000 ℃ in a muffle furnace at a speed of 10 ℃/min, and keeping heat treatment for 5 hours; taking out a sample obtained by heat treatment, placing the sample in a corundum crucible at room temperature, uniformly mixing and fully grinding, heating to 1000 ℃ in a muffle furnace at a speed of 10 ℃/min, and keeping the heat treatment for 20 hours to obtain a calcined product K 0.8Ti1.7Li0.2Co0.1O4 which has a layered structure and good crystallinity;
S2, mixing the calcined product obtained in the step S1 with 200mL of hydrochloric acid (2 mol/L), and continuously magnetically stirring for 4 days to perform a first intercalation reaction so as to protonate the calcined product, so that Li + ions and K + ions can be fully ion-exchanged with H + ions; after standing, collecting the precipitate, washing 3 times by using deionized water and drying in an oven to obtain a first intercalation product HTi 1.7Co0.1O4;
S3, soaking the first intercalation product HTi 1.7Co0.1O4 in 200mL of tetrabutylammonium hydroxide solution with the concentration of 10% (w/v), standing for 5H to perform a second intercalation reaction so as to replace H + ions with TBA + ions with larger particle size, thus obtaining a second intercalation product BA zH1-zTi1.7Co0.1O4;
S4, mixing the second intercalation product with deionized water, mechanically shaking for 48 hours, and stripping to obtain the magnetic element doped two-dimensional titanium dioxide liquid crystal, namely the cobalt doped two-dimensional titanium dioxide liquid crystal.
In order to examine the characteristics of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared by the method, the morphology, the transmissivity, the magnetism, the magneto-optical response and the stability of the cobalt-doped two-dimensional titanium dioxide liquid crystal are characterized, and the characteristics are as follows:
(1) Characterization of topography
Specifically, the prepared cobalt-doped two-dimensional titanium dioxide liquid crystal is diluted to 0.01g/L, is dripped on a silicon wafer, is spin-coated and dried, and then uses an Atomic Force Microscope (AFM) to characterize the transverse dimension and thickness of the two-dimensional nano sheet, and the obtained results are shown in fig. 1 and 2, wherein fig. 1 is a transverse dimension statistical graph of the cobalt-doped two-dimensional titanium dioxide liquid crystal, and fig. 2 is a thickness statistical graph of the cobalt-doped two-dimensional titanium dioxide liquid crystal. FIG. 1 shows that the average transverse dimension of the two-dimensional nano-sheet is 1.6 mu m, and FIG. 2 shows that the average thickness of the two-dimensional nano-sheet is 1.1nm, and the diameter-thickness ratio (transverse dimension/thickness) of the prepared cobalt-doped two-dimensional titanium dioxide liquid crystal can reach more than 10 3.
(2) Transmittance characterization
Specifically, a certain amount of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared above was taken, and the transmittance was tested by using an ultraviolet-visible spectrophotometer, and the obtained results are shown in fig. 3. As can be seen from the experimental results shown in fig. 3, the transmittance of the two-dimensional liquid crystal prepared in this example is higher in the deep ultraviolet band of 300nm to 350nm (the average transmittance in this range is > 70%); the high deep ultraviolet transmittance provides a basis for preparing the deep ultraviolet optical element with adjustable transmission double refraction.
(3) Magnetic characterization
Specifically, a suction filtration method is adopted to prepare a cobalt-doped two-dimensional titanium dioxide film, then a SQUID magnetic measuring instrument is utilized to carry out magnetic characterization, and the obtained result is shown in figure 4. As shown in fig. 4, the in-plane polarizability of the cobalt-doped two-dimensional titanium dioxide material is greater than the out-of-plane polarizability, and the cobalt-doped two-dimensional titanium dioxide material exhibits obvious magnetic anisotropy, and under the action of a magnetic field, the magnetic anisotropy causes the cobalt-doped two-dimensional titanium dioxide material to be aligned along the direction of the magnetic field, so that birefringence is caused.
(4) Magneto-optical response characterization
The cobalt-doped two-dimensional titanium dioxide liquid crystal prepared above was subjected to magnetic sensitivity characterization and magneto-optical Keton-Mu Du coefficient test by using a magneto-optical system, and the results are shown in FIG. 5. With reference to the experimental data in fig. 5, the magneto-optical koton-Mu Du coefficient of the cobalt-doped two-dimensional titania liquid crystal is calculated to be 3.9×10 6T-2m-1 according to the formula c=Δn/(λ×h 2). The sensitive magnetic response indicates that a small magnetic field can cause ordered arrangement of two-dimensional liquid crystal molecules and birefringence, and the method can lay a foundation for preparing deep ultraviolet optical hydrogel by adopting a magnetic auxiliary photo-curing technology.
(5) Stability characterization
The cobalt-doped two-dimensional titanium dioxide liquid crystal prepared above was irradiated with 303nm laser for 5 hours to examine whether it had strong stability under deep ultraviolet light, and the obtained results are shown in fig. 6. As can be seen from fig. 6, after 5 hours of irradiation, the light intensity decay in the "on" and "off" states of the magnetic field is within 5%, which is far higher than the deep ultraviolet stability of the conventional organic liquid crystal (decay >50% at the same time).
Comparative example 1
This comparative example, which differs from example 1 in that a magnetic element doped titanium dioxide liquid crystal was prepared: in this comparative example, the operation of step S3 in example 1 was omitted, and the other operations were the same as in example 1, to produce a magnetic element-doped titania liquid crystal, i.e., a cobalt-doped titania liquid crystal.
In this comparative example, the first intercalation product was not mixed with the tetrabutylammonium hydroxide solution, the solution lacked TBA + ions with larger ionic radius, the first intercalation product layer was H + ions, and the sample was difficult to be peeled into two-dimensional material during mechanical peeling, and the final sample was cobalt doped titanium dioxide liquid crystal. The ratio of the diameter to the thickness of the cobalt-doped titanium dioxide liquid crystal prepared by the comparative example is below 10 2, which is far smaller than the ratio of the diameter to the thickness of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared by the example 1 (more than 10 3).
The cobalt-doped titanium dioxide liquid crystals prepared in example 1 and the comparative example were subjected to magnetic sensitivity characterization, magneto-optical Keton-Mu Du coefficient test and comparison, and the obtained results are shown in FIG. 7. From the magneto-optic response characterization test results, the small diameter-thickness ratio of the cobalt-doped titanium dioxide liquid crystal obtained in the comparative example causes low magneto-optic response sensitivity, the birefringence value is low, the magneto-optic Ketone-Mu Du coefficient is 2.4X10 5T-2m-1, and the magneto-optic Ketone-Mu Du coefficient (3.9X10 6T-2m-1) of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in the embodiment 1 is far smaller than that of the cobalt-doped two-dimensional titanium dioxide liquid crystal, so that the importance of the magneto-optic response characteristic of the material by stripping the cobalt-doped two-dimensional material is demonstrated.
Comparative example 2
This comparative example, which is different from example 1 in that a two-dimensional titanium dioxide liquid crystal was prepared: the preparation raw materials of the comparative example were not added with cobalt oxide, and the other operations were the same as in example 1, and the final product was a two-dimensional titania liquid crystal without cobalt doping.
Experiments show that the two-dimensional titanium dioxide liquid crystal prepared by the comparative example has extremely weak magnetism, cannot cause a double refraction effect under the action of a magnetic field, and cannot be used for preparing the double refraction adjustable deep ultraviolet optical hydrogel, so that the important significance of doping of the magnetic element cobalt can be seen, the two-dimensional titanium dioxide liquid crystal can provide larger magnetism for the double refraction adjustable deep ultraviolet optical hydrogel material, and can cause a strong double refraction effect under a small magnetic field.
Comparative example 3
This comparative example a cobalt doped two-dimensional titania liquid crystal was prepared, the difference between this comparative example and example 1 being that: in this comparative example, the cobalt doping concentration was Co/Ti (element molar ratio) =12%, higher than that in example 1 (Co/ti=6%), and the operation was the same as in example 1, and the final product was a high-concentration cobalt-doped two-dimensional titania liquid crystal.
The low concentration cobalt-doped two-dimensional titania liquid crystal prepared in example 1 and the high concentration cobalt-doped two-dimensional titania liquid crystal prepared in this comparative example were subjected to transmittance test and comparison using an ultraviolet-visible light spectrophotometer, and the results are shown in fig. 8. As shown by test results, when the proportion of cobalt element is high, the transmissivity of the deep ultraviolet region is reduced, the average transmissivity of the cobalt doped two-dimensional titanium dioxide liquid crystal prepared by the comparative example in the deep ultraviolet band of 300-350 nm is less than 50%, and the cobalt doped two-dimensional titanium dioxide liquid crystal is difficult to prepare a transmissive deep ultraviolet birefringent element. It can be seen that the concentration of cobalt doping cannot be too high.
Example 2
The embodiment prepares the deep ultraviolet optical hydrogel material with adjustable birefringence, and the preparation method comprises the following steps:
S1, adding deionized water into the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in the embodiment 1 to dilute the liquid crystal to obtain a liquid crystal solution with the concentration of 5 multiplied by 10 -4 wt%, adding a poly (ethylene glycol) diacrylate monomer with the concentration of 4wt% of the liquid crystal solution and a potassium persulfate photosensitizer accounting for 0.5wt% of the liquid crystal solution, and uniformly stirring and mixing to obtain a mixed solution;
S2, as shown in FIG. 9, transferring the mixed solution into a container (or a die), wherein the size of the container is 8cm 3, then generating a magnetic field of 0.8T by utilizing an electromagnet, placing the container filled with the mixed solution into the magnetic field, and enabling the bottom of the container to be parallel to the direction of the magnetic field; at this time, the cobalt-doped two-dimensional titanium dioxide in the mixed solution tends to be arranged in the magnetic field direction under the action of an external magnetic field due to the intrinsic magnetic anisotropy of the cobalt-doped two-dimensional titanium dioxide, so that double refraction is caused; and then, the mixed solution is irradiated by ultraviolet light with the wavelength of 365nm for 10min, at the moment, the poly (ethylene glycol) diacrylate monomer and the photosensitizer cause gelation, the cobalt-doped two-dimensional titanium dioxide which is directionally arranged is solidified in the hydrogel, and the birefringence value of the cobalt-doped two-dimensional titanium dioxide is kept even under the condition of removing an external magnetic field, so that the deep ultraviolet optical hydrogel with adjustable birefringence is prepared, as shown in figure 10.
The birefringence-adjustable deep ultraviolet optical hydrogel is compressed or stretched to carry out deep ultraviolet light modulation. Specifically, first, the above birefringence-adjustable deep ultraviolet optical hydrogel was subjected to stress-strain test, and the results are shown in fig. 11 and 12, and it is known from the test results that only a small force (< 6 kPa) is required to compress or stretch the optical hydrogel to 50% of the initial state.
Subsequently, a 45℃polarizer was added after the exit laser light having a wavelength of 303nm, and this deep ultraviolet polarized light was irradiated onto the above birefringence-tunable optical hydrogel. The optical hydrogel is compressed or stretched along the optical path, and the ordered arrangement state of the optical path and the cobalt doped two-dimensional titanium dioxide can be changed, so that the quantitative regulation and control of the deep ultraviolet phase delay are realized. Because the ordered structure of the cobalt doped two-dimensional titanium dioxide liquid crystal is completely stored in the optical hydrogel, the optical hydrogel has double refraction in an initial state and causes 22 DEG phase delay of deep ultraviolet light; when the hydrogel is compressed to 50% from the initial state, the optical path and the arrangement state of the cobalt-doped two-dimensional titanium dioxide liquid crystal material are changed simultaneously, so that the phase retardation is changed, and the initial 22 DEG is regulated to 11 DEG, as shown in fig. 13; when 50% strain is caused by stretching, the optical path length increases, and the amount of phase retardation increases to 30 °, as shown in fig. 14. It can be seen that the optical hydrogel can be used as a novel optical element with adjustable birefringence, and realizes the force-light modulation performance through the force-induced birefringence effect, thereby realizing quantitative continuous modulation of deep ultraviolet light.
Regarding the stability of the deep ultraviolet optical hydrogel, as shown in fig. 15, the difference rate of the deep ultraviolet phase differences from each other under the same deformation is not more than 2% in 10 repeated compression processes of the hydrogel; meanwhile, the phase difference error caused by repeated stretching light modulation for 10 times is not more than 2%, as shown in fig. 16, which proves that the optical hydrogel with adjustable birefringence has good stability.
Comparative example 4
This comparative example produced an optical hydrogel with adjustable birefringence, which differs from example 2 in that: in this comparative example, the dilution concentration of the cobalt-doped two-dimensional titania liquid crystal in step S1 of example 2 was adjusted from 5X 10 -4 wt% to 5X 10 -5 wt%, and the other operations were the same as in example 2.
The birefringence-tunable optical hydrogels prepared in example 2 and this comparative example were characterized according to the characterization method of the magnetic response of the liquid crystal material in example 1, and the results are shown in fig. 17. As shown by test results, the cobalt-doped two-dimensional titanium dioxide liquid crystal pair concentration in the comparative example is too low, the birefringence value of the optical hydrogel of the product is extremely small, and practical application is difficult to realize.
Comparative example 5
This comparative example produces an optical hydrogel, which differs from example 2 in that: in this comparative example, the dilution concentration of the cobalt-doped two-dimensional titania liquid crystal in step S1 of example 2 was adjusted from 5X 10 -4 wt% to 5X 10 -2 wt%, and the other operations were the same as in example 2.
The optical hydrogel prepared in this comparative example was tested by using a transmission spectrometer, and the transmittance of deep ultraviolet light of the liquid crystal in the optical hydrogel prepared in this comparative example was extremely low, and the average transmittance was less than 10% in the deep ultraviolet band of 300nm to 350nm, which was difficult to be practically used.
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.
Claims (6)
1. The optical hydrogel with adjustable birefringence is characterized by comprising a hydrogel matrix and magnetic element doped two-dimensional titanium dioxide liquid crystals, wherein the hydrogel matrix is provided with a network crosslinking structure, and the magnetic element doped two-dimensional titanium dioxide liquid crystals are filled in the network crosslinking structure and are arranged in an oriented manner; the magnetic element doped in the magnetic element doped two-dimensional titanium dioxide liquid crystal is cobalt, the doping amount of the magnetic element in the magnetic element doped two-dimensional titanium dioxide liquid crystal is controlled to be 3-9% of the molar ratio of the magnetic element to the titanium element, and the diameter-thickness ratio of the magnetic element doped two-dimensional titanium dioxide liquid crystal is more than 10 3;
The optical hydrogel is prepared by the following steps:
s1, firstly mixing a magnetic element doped two-dimensional titanium dioxide liquid crystal with a solvent to prepare a liquid crystal solution with the concentration of 10 -4~10-3 wt%, and then adding a polymer monomer accounting for 3-5 wt% of the liquid crystal solution and a photosensitizer accounting for 0.3-1 wt% to prepare a mixed solution;
S2, transferring the mixed solution into a mold, and performing ultraviolet curing under the action of a magnetic field.
2. A method of preparing a birefringent tunable optical hydrogel according to claim 1, comprising the steps of:
s1, firstly mixing a magnetic element doped two-dimensional titanium dioxide liquid crystal with a solvent to prepare a liquid crystal solution with the concentration of 10 -4~10-3 wt%, and then adding a polymer monomer accounting for 3-5 wt% of the liquid crystal solution and a photosensitizer accounting for 0.3-1 wt% to prepare a mixed solution;
S2, transferring the mixed solution into a mold, and performing ultraviolet curing under the action of a magnetic field.
3. The method for preparing a birefringent tunable optical hydrogel according to claim 2, further comprising, prior to step S1: s0, preparing the magnetic element doped two-dimensional titanium dioxide liquid crystal by an ion intercalation method.
4. The method of preparing a birefringent tunable optical hydrogel according to claim 3, wherein step S0 comprises:
(1) Mixing preparation raw materials comprising titanium dioxide, a magnetic element source and carbonate, and calcining to obtain a calcined product;
(2) Mixing the calcined product with protonic acid, and performing a first intercalation reaction to obtain a first intercalation product;
(3) Mixing the first intercalation product with organic base, and performing a second intercalation reaction to obtain a second intercalation product;
(4) And mechanically stripping the second intercalation product in a liquid phase to obtain the magnetic element doped two-dimensional titanium dioxide liquid crystal.
5. Use of the birefringent tunable optical hydrogel of claim 1 in the fields of optical communications, laser polarization technology, polarization information processing or precision measurement.
6. An optical device comprising the birefringence-tunable optical hydrogel of claim 1.
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| CN103170357A (en) * | 2013-03-27 | 2013-06-26 | 天津大学 | High-activity two-dimensional doped modified titanium dioxide nanometer powder photocatalytic material and preparation method thereof |
| CN113429530A (en) * | 2021-06-04 | 2021-09-24 | 清华-伯克利深圳学院筹备办公室 | Two-dimensional material composite hydrogel and preparation method and application thereof |
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| CN103170357A (en) * | 2013-03-27 | 2013-06-26 | 天津大学 | High-activity two-dimensional doped modified titanium dioxide nanometer powder photocatalytic material and preparation method thereof |
| CN113637180A (en) * | 2020-05-11 | 2021-11-12 | 清华-伯克利深圳学院筹备办公室 | Optically anisotropic hydrogel, preparation method thereof, production system thereof and optical device |
| CN113429530A (en) * | 2021-06-04 | 2021-09-24 | 清华-伯克利深圳学院筹备办公室 | Two-dimensional material composite hydrogel and preparation method and application thereof |
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