CN115558130A - Optical hydrogel with adjustable birefringence and preparation method and application thereof - Google Patents
Optical hydrogel with adjustable birefringence and preparation method and application thereof Download PDFInfo
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- CN115558130A CN115558130A CN202211199024.5A CN202211199024A CN115558130A CN 115558130 A CN115558130 A CN 115558130A CN 202211199024 A CN202211199024 A CN 202211199024A CN 115558130 A CN115558130 A CN 115558130A
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 239000004408 titanium dioxide Substances 0.000 claims abstract description 80
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- 150000002500 ions Chemical class 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
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- 229910017052 cobalt Inorganic materials 0.000 claims description 8
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 8
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- 230000009471 action Effects 0.000 claims description 7
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- 238000005516 engineering process Methods 0.000 claims description 6
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- 238000001354 calcination Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000000203 mixture Substances 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
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- 238000005259 measurement Methods 0.000 claims description 2
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims 1
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- 238000002834 transmittance Methods 0.000 description 15
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- 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
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- 239000010410 layer Substances 0.000 description 5
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- 239000010936 titanium Substances 0.000 description 5
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- 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
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 238000000016 photochemical curing Methods 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
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- GJKGAPPUXSSCFI-UHFFFAOYSA-N 2-Hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone Chemical compound CC(C)(O)C(=O)C1=CC=C(OCCO)C=C1 GJKGAPPUXSSCFI-UHFFFAOYSA-N 0.000 description 1
- 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
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- 230000001678 irradiating effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 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
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- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012876 topography 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
-
- 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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- 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 a birefringence-adjustable optical hydrogel and a preparation method and application thereof. The optical hydrogel can control parameters such as optical path, arrangement order degree of 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, and has the advantages of simpler modulation operation, easy control, accurate control, quick response time and no crosstalk to surrounding devices.
Description
Technical Field
The invention relates to the technical field of optical materials, in particular to birefringence-adjustable optical hydrogel and a preparation method and application thereof.
Background
By quantitatively regulating and controlling parameters such as amplitude, phase, frequency and polarization state of optical waves, an additional signal carrying information can be superposed on carrier optical waves by an optical modulation technology, and then information transmission is carried out by using an optical signal. The most important component of the optical modulation system is a birefringent optical element, but the working wavelength range of the birefringent optical element is mainly concentrated in the visible light and near infrared band (355 nm-1800 nm), and the related reports in the deep ultraviolet band (lambda <350 nm) are less, and the working wavelength range is mostly concentrated in the inorganic optical single crystal.
With the development of science and technology, the modulation of deep ultraviolet light becomes more and more important, and a transmissive birefringent element is urgently needed to be developed, so that the continuous modulation of the shape, polarization and phase of the deep ultraviolet pulse is realized under the condition of not changing the light propagation direction. In recent years, relevant research on the method is carried out at home and abroad, and Ca (BO) is prepared 2 ) 2 And alpha-SnF 2 And the like. However, when the shape and size of the material are fixed, the birefringence of the single crystal material is fixed, and continuous control of deep ultraviolet light is difficult, which limits practical application.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides an optical hydrogel with adjustable birefringence and a preparation method and application thereof.
The invention provides birefringence-adjustable optical hydrogel, which comprises a hydrogel matrix and magnetic element-doped two-dimensional titanium dioxide liquid crystals, wherein the hydrogel matrix is provided with a network cross-linking structure, and the magnetic element-doped two-dimensional titanium dioxide liquid crystals are filled in the network cross-linking structure and are arranged in an oriented manner.
The birefringence-adjustable optical hydrogel provided by 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 the optical hydrogel can control parameters such as optical path and arrangement order of the magnetic element-doped two-dimensional titanium dioxide liquid crystals through compression or stretching, so that continuous and stable modulation of deep ultraviolet light can be realized.
The working waveband range of the optical hydrogel with adjustable birefringence is in a deep ultraviolet waveband (lambda is less than 350 nm), particularly in a wavelength range of 300 nm-350 nm, the optical hydrogel belongs to stress response type optical hydrogel, particularly can realize continuous and stable modulation of the deep ultraviolet birefringence through compressive or tensile stress, has a large phase adjustable range, can control the phase retardation within a range of 10-30 degrees, and can overcome the problem of photophysical or photochemical recession of organic liquid crystals under ultraviolet light.
In some embodiments of the present invention, the magnetic element doped two-dimensional titanium dioxide liquid crystal is doped with at least one magnetic element selected from cobalt, manganese and nickel; cobalt is preferred.
In order to ensure the deep ultraviolet transmittance and the 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 to 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 elements in the relatively low proper range, the material can be ensured to have high deep ultraviolet transmittance and sensitive magnetic response, so that the phenomenon that the birefringence value is small due to too low concentration of the magnetic elements, and the transmittance is too low due to too high concentration of the magnetic elements to influence the performance of the material is avoided.
In some embodiments of the present invention, the magnetic element doped two-dimensional titanium dioxide liquid crystal has an aspect ratio (i.e. lateral dimension to thickness) of 10 3 As described above. Under the large radius-thickness ratio, the magnetic element doped two-dimensional titanium dioxide liquid crystal has sensitive magnetic response characteristics, can complete orientation control under a small magnetic field and causes larger birefringence.
In some embodiments of the invention, the mass ratio of the magnetic element doped two-dimensional titanium dioxide liquid crystal to the optical hydrogel is 10 -4 ～10 -3 wt%. By controlling the content of the magnetic element doped two-dimensional titanium dioxide liquid crystal in the optical hydrogel to be in the above range, the optical hydrogel can be ensured to have higher birefringence value and high deep ultraviolet transmittance, and the transmission-type deep ultraviolet optical hydrogel with adjustable birefringence is obtained.
In a second aspect of the present invention, a method for preparing a birefringence-tunable optical hydrogel according to the first aspect of the present invention is provided, which comprises 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;
and S2, transferring the mixed solution into a mold, and carrying out ultraviolet curing under the action of a magnetic field.
In the preparation method, a mixed solution is prepared by mixing a magnetic element doped two-dimensional titanium dioxide liquid crystal with sensitive magnetic response and high deep ultraviolet transmittance with a polymer monomer, a photosensitizer and a solvent, the mixed solution is transferred into a mold, the two-dimensional titanium dioxide liquid crystal is cured into optical hydrogel under the action of a magnetic field by adopting a magnetic assisted photo-curing 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 birefringence, and the ordered structure arranged along the magnetic field by the magnetic element doped two-dimensional titanium dioxide liquid crystal is completely stored in the curing process, so that the deep ultraviolet optical hydrogel with adjustable birefringence is prepared, and particularly, the continuous and stable regulation and control of deep ultraviolet light can be realized by controlling parameters such as optical path, ordered arrangement degree of the magnetic element doped two-dimensional titanium dioxide liquid crystal and the like through compression or stretching.
In some embodiments of the invention, step S1 comprises: firstly, mixing a magnetic element doped two-dimensional titanium dioxide liquid crystal and a solvent to prepare a mixture with the concentration of 10 -4 ～10 -3 Adding polymer monomer accounting for 3-5 wt% of the liquid crystal solution and photosensitizer accounting for 0.3-1 wt% of the liquid crystal solution, and mixing to prepare mixed solution. By diluting the magnetic element doped two-dimensional titanium dioxide liquid crystal to the specific concentration, sensitive magnetic response and high deep ultraviolet light transmittance can be ensured at the same time. Wherein, the polymer monomer can specifically adopt at least one of poly (ethylene glycol) diacrylate and N-isopropyl acrylamide; the photosensitizer can adopt at least one of potassium persulfate and 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone.
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 the preparation raw materials including titanium dioxide, a magnetic element source and carbonate, and calcining to obtain a calcined product;
(2) Mixing the calcined product with protonic acid to perform a first intercalation reaction to prepare a first intercalation product;
(3) Mixing the first intercalation product with organic base, and carrying out a second intercalation reaction to prepare a second intercalation product;
(4) And mechanically stripping the second intercalation product in a liquid phase to prepare the magnetic element doped two-dimensional titanium dioxide liquid crystal.
The two-dimensional titanium dioxide liquid crystal doped with the magnetic element with the large diameter-thickness ratio can be effectively stripped and prepared by adopting the ion intercalation method, and the obtained two-dimensional titanium dioxide liquid crystal doped with the magnetic element has excellent magneto-optical response characteristics, high magneto-optical response sensitivity and high birefringence value.
In some embodiments of the invention, step (1) specifically comprises: mixing the raw materials including titanium dioxide, magnetic element source and carbonateCalcining at 800-1200 deg.c for 5-6 hr, grinding, and calcining at 800-1200 deg.c for 20-24 hr. Wherein, the first time of calcination is to fully react the raw materials; a second calcination to grow grains; taking the grind out between two calcines can improve the homogeneity of the material. The carbonate can be at least one of sodium carbonate, potassium carbonate and lithium carbonate, and metal ions in the carbonate can provide positive charges and are inserted into the titanium dioxide layer to facilitate the subsequent stripping of the titanium dioxide layer into a single-layer material; in addition, compared with Na + And Li + Ion, K + The radius of the ion is larger, and the titanium dioxide in the layer cannot be replaced by Ti 4+ As the carbonate, potassium carbonate is preferably used. The magnetic element source can adopt at least one of cobalt oxide, manganese oxide and nickel oxide; specifically, the preparation raw material may include the following elements in a molar ratio of K: ti Li Co O =0.8 [ (5.2-x)/3 ]]:[(0.8-2x)/3]Titanium dioxide, cobalt oxide, potassium carbonate and lithium carbonate with x of 4 and x of = 0.05-0.15.
In some embodiments of the present invention, in the 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, magnetic stirring is carried out continuously for 4-5 days, then the mixture is stood still, precipitate is collected, and then deionized water is used for cleaning and drying.
In the step (3), the organic base is generally organic base with large-particle-size positive ions, so that the positive ions in the organic base are inserted into the titanium dioxide layer, and the stripping preparation of the 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 and the organic amine salt solution are mixed and kept stand for 5 to 6 hours to carry out the second intercalation reaction.
In some embodiments of the present invention, in the step (4), the mechanical peeling 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, an application of any one of the birefringence-tunable optical hydrogels proposed in the first aspect of the present invention in optical communication, laser polarization technology, polarization information processing or precision measurement is proposed.
In a fourth aspect of the present invention, an optical device is provided, which comprises any one of the birefringence-tunable optical hydrogels set forth in the first aspect of the present invention. The optical device includes 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 following figures and examples, in which:
FIG. 1 is a diagram showing the statistical results of the lateral dimensions of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1;
FIG. 2 is a graph showing the statistical results of the thickness 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 light transmittance test of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1;
FIG. 4 is a graph showing the results of the magnetic anisotropy test of the cobalt-doped two-dimensional titania liquid crystal prepared in example 1;
FIG. 5 is a graph showing the results of the magnetic response test of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1;
FIG. 6 is a graph showing the UV stability of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1;
FIG. 7 is a graph showing the results of magnetic response tests of cobalt-doped two-dimensional titania liquid crystals prepared in example 1 and cobalt-doped titania liquid crystals prepared in comparative example 1;
FIG. 8 is a graph showing the results of deep ultraviolet light transmittance test of cobalt-doped two-dimensional titania liquid crystals prepared in example 1 and comparative example 3;
FIG. 9 is a schematic diagram of the preparation of an optical hydrogel with adjustable birefringence according to example 2;
FIG. 10 is a diagram of an example of a birefringence tunable optical hydrogel prepared in example 2;
FIG. 11 is a graph showing the pressure-strain curves of the birefringence tunable optical hydrogels prepared in example 2;
FIG. 12 is a graph showing the tensile stress-strain curves of the birefringence-tunable optical hydrogel prepared in example 2;
FIG. 13 is a graph showing the modulation test results of the birefringence-tunable optical hydrogel obtained in example 2 on deep ultraviolet light;
FIG. 14 is a graph showing the modulation test results of the birefringence-tunable optical hydrogel obtained in example 2 on deep ultraviolet light;
FIG. 15 is a graph showing the results of testing the repeated compression stability of the birefringence tunable optical hydrogel obtained in example 2;
FIG. 16 is a graph showing the results of testing the repetitive tensile stability of the birefringence-tunable optical hydrogel obtained in example 2;
FIG. 17 is a graph showing the results of the magnetic response test of the birefringence-tunable optical hydrogels obtained in example 2 and comparative example 4.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
The embodiment prepares the magnetic element doped two-dimensional titanium dioxide liquid crystal, and the preparation method comprises the following steps:
s1, uniformly mixing titanium dioxide, cobalt oxide, potassium carbonate and lithium carbonate in a corundum crucible according to the molar ratio of elements, namely K, ti, li, co, O =0.8, 0.1; taking out the sample obtained by heat treatment, placing the sample in a corundum crucible at room temperature, uniformly mixing, fully grinding, heating to 1000 ℃ at a speed of 10 ℃/min in a muffle furnace, and keeping the heat treatment for 20 hours to obtain a calcined product K 0.8 Ti 1.7 Li 0.2 Co 0.1 O 4 Having a layered structureAnd has good crystallinity;
s2, mixing the calcined product prepared in the step S1 with 200mL of hydrochloric acid (2 mol/L), and continuously carrying out magnetic stirring for 4 days to carry out a first intercalation reaction so as to protonate the calcined product and enable Li + Ions and K + The ions can react with H + Carrying out sufficient ion exchange on ions; standing, collecting precipitate, washing with deionized water for 3 times, and drying in oven to obtain first intercalation product HTi 1.7 Co 0.1 O 4 ；
S3, subjecting the first intercalation product HTi 1.7 Co 0.1 O 4 Soaking in 200mL of tetrabutylammonium hydroxide solution with concentration of 10% (w/v), standing for 5H for second intercalation reaction to obtain H + Ion replacement to TBA of larger particle size + Ion to obtain a second intercalation product BA z H 1-z Ti 1.7 Co 0.1 O 4 ；
And S4, mixing the second intercalation product with deionized water, mechanically shaking for 48h, 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 investigate the characteristics of the prepared cobalt-doped two-dimensional titanium dioxide liquid crystal, the appearance, the transmissivity, the magnetic and magneto-optical response and the stability of the liquid crystal are characterized as follows:
(1) Topography characterization
Specifically, the prepared cobalt-doped two-dimensional titanium dioxide liquid crystal is diluted to 0.01g/L, and is dripped on a silicon wafer for spin coating and drying, and then an Atomic Force Microscope (AFM) is used for characterizing the transverse size and the thickness of the two-dimensional nanosheet, and the obtained results are shown in fig. 1 and fig. 2, wherein fig. 1 is a transverse size 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 μm, 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 cobalt-doped two-dimensional titanium dioxide liquid crystal prepared by the method can reach 10 3 The above.
(2) Transmission characterization
Specifically, a certain amount of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared above was taken, and transmittance was measured using an ultraviolet-visible spectrophotometer, and the obtained result is shown in fig. 3. As can be seen from the experimental results shown in FIG. 3, the two-dimensional liquid crystal prepared in this example has a high transmittance (average transmittance >70% in this range) in the deep ultraviolet range of 300nm to 350 nm; the high deep ultraviolet transmittance provides a foundation for preparing the transmission type double refraction adjustable deep ultraviolet optical element.
(3) Magnetic characterization
Specifically, a cobalt-doped two-dimensional titanium dioxide film is prepared by adopting a suction filtration method, and then a SQUID magnetic measuring instrument is used for 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 titania material is greater than the out-of-plane polarizability, and the cobalt-doped two-dimensional titania material exhibits significant magnetic anisotropy, and under the action of a magnetic field, the magnetic anisotropy causes the cobalt-doped two-dimensional titania material to align along the direction of the magnetic field, thereby causing birefringence.
(4) Magneto-optical response characterization
The magnetic sensitivity of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared by the method is characterized by a magneto-optical system, and the magneto-optical Keton-Mu Du coefficient is tested, and the result is shown in fig. 5. Combined with the experimental data in fig. 5, according to the formula C = Δ n/(λ × H) 2 ) The coefficient of the magneto-optic Kedun-Mu Du of the cobalt-doped two-dimensional titanium dioxide liquid crystal can be calculated to be 3.9 multiplied by 10 6 T -2 m -1 . The sensitive magnetic response shows that the small magnetic field can cause the ordered arrangement of two-dimensional liquid crystal molecules and birefringence, which lays a foundation for the preparation of the deep ultraviolet optical hydrogel by adopting the magnetic assisted photocuring technology.
(5) Characterization of stability
The cobalt-doped two-dimensional titanium dioxide liquid crystal prepared above was irradiated with 303nm laser for 5h to examine whether it has strong stability under deep ultraviolet light, and the obtained result is shown in fig. 6. As can be seen from FIG. 6, after 5h of irradiation, the light intensity attenuation in the "on" and "off" states of the magnetic field is within 5%, which is much higher than the deep UV stability of the conventional organic liquid crystal (with >50% attenuation in time).
Comparative example 1
The comparative example, which prepares a magnetic element-doped titanium dioxide liquid crystal, differs from example 1 in that: 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 obtain a magnetic element-doped titania liquid crystal, i.e., a cobalt-doped titania liquid crystal.
This comparative example lacks TBA with a larger ionic radius due to the absence of mixing the first intercalation product with tetrabutylammonium hydroxide solution + Ions, between layers of the first intercalation product being H + And ions are difficult to strip the sample into a two-dimensional material during mechanical stripping, and the finally obtained sample is cobalt-doped titanium dioxide liquid crystal. The diameter-thickness ratio of the cobalt-doped titanium dioxide liquid crystal prepared by the comparative example is 10 2 The ratio of the diameter to the thickness of the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1 is much smaller (more than 10) 3 )。
The cobalt-doped titanium dioxide liquid crystals prepared in example 1 and this comparative example were subjected to characterization of magnetic sensitivity and testing and comparison of magneto-optical Keton-Mu Du coefficient, and the results are shown in FIG. 7. The magneto-optic response characterization test result shows that the small diameter-thickness ratio of the cobalt-doped titanium dioxide liquid crystal obtained by the comparative example causes low magneto-optic response sensitivity, the birefringence value is low, and the magneto-optic Keton-Mu Du coefficient is 2.4 multiplied by 10 5 T -2 m -1 Magneto-optic Keton-Mu Du coefficient (3.9X 10) much smaller than that of cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in example 1 6 T -2 m -1 ) Therefore, the importance of the two-dimensional material stripping on the magneto-optical response characteristic of the material is illustrated.
Comparative example 2
This comparative example, which was different from example 1 in that a two-dimensional titanium dioxide liquid crystal was prepared, was: the preparation raw material of the comparative example is not added with cobalt oxide, other operations are the same as the example 1, and the final product is the two-dimensional titanium dioxide 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 birefringence effect under the action of a magnetic field, and further cannot be used for preparing the birefringence-adjustable deep ultraviolet optical hydrogel.
Comparative example 3
The comparative example, which prepares a cobalt-doped two-dimensional titania liquid crystal, differs from example 1 in that: in the comparative example, the cobalt doping concentration is Co/Ti (element molar ratio) =12%, which is higher than that in example 1 (Co/Ti = 6%), other operations are the same as in example 1, and the final product is a high-concentration cobalt-doped two-dimensional titania liquid crystal.
Transmittance test and comparison were performed on 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 using an ultraviolet-visible spectrophotometer, and the obtained results are shown in fig. 8. The test result shows that when the proportion of the cobalt element is higher, the transmissivity of a deep ultraviolet region is reduced, and 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%, so that the cobalt-doped two-dimensional titanium dioxide liquid crystal is difficult to be used for preparing the transmission-type deep ultraviolet birefringent element. It can be seen that the concentration of cobalt doping cannot be too high.
Example 2
The embodiment prepares a birefringence-adjustable deep ultraviolet optical hydrogel material, and the preparation method comprises the following steps:
s1, adopting the cobalt-doped two-dimensional titanium dioxide liquid crystal prepared in the embodiment 1, adding deionized water to dilute the cobalt-doped two-dimensional titanium dioxide liquid crystal to obtain the liquid crystal with the concentration of 5 multiplied by 10 -4 Adding 4wt% of poly (ethylene glycol) diacrylate monomer and 0.5wt% of potassium persulfate photosensitizer into the liquid crystal solution with weight percent, and uniformly mixing to obtain a mixed solution;
s2, as shown in figure 9, transferring the mixed solution into a container (or a mold), wherein the size of the container is 8cm 3 Then, a 0.8T magnetic field is generated by an electromagnet, and the container filled with the mixed liquid is placed in the magnetic field, the bottom of the container is connected with the bottom of the containerThe magnetic field directions are parallel; at the moment, 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 intrinsic magnetic anisotropy, so that birefringence is caused; and then irradiating the mixed solution by using 365nm ultraviolet light for 10min, wherein at the moment, the poly (ethylene glycol) diacrylate monomer and the photosensitizer cause gelation, and the cobalt-doped two-dimensional titanium dioxide which is directionally arranged is cured in the hydrogel, so that the birefringence value is still maintained even under the condition of removing an external magnetic field, and the birefringence-adjustable deep ultraviolet optical hydrogel is prepared, as shown in figure 10.
The deep ultraviolet light modulation is carried out by compressing or stretching the deep ultraviolet optical hydrogel with adjustable birefringence. Specifically, first, the stress-strain test is performed on the above birefringence-tunable deep ultraviolet optical hydrogel, and the obtained results are shown in fig. 11 and 12, and it can be seen 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 outgoing laser light with a wavelength of 303nm, and this deep ultraviolet polarized light was irradiated on the above birefringence-adjustable optical hydrogel. The optical hydrogel is compressed or stretched along the optical path, so that the optical path and the ordered arrangement state of the cobalt-doped two-dimensional titanium dioxide can be changed, and the quantitative regulation and control of the deep ultraviolet phase delay can be 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 phase delay of 22 degrees of deep ultraviolet light; when the hydrogel is compressed to 50% from the initial state, the phase retardation changes along with the change of the optical path and the arrangement state of the cobalt-doped two-dimensional titanium dioxide liquid crystal material, and is regulated from the initial 22 degrees to 11 degrees as shown in fig. 13; when 50% strain is caused by stretching, the optical path length becomes large, and the phase retardation amount increases to 30 °, as shown in fig. 14. The optical hydrogel can be used as a novel birefringence-adjustable optical element, and the force-light modulation performance is realized through the force-induced birefringence effect, so that the quantitative continuous modulation of the deep ultraviolet light is realized.
Regarding the stability of the deep ultraviolet optical hydrogel, as shown in fig. 15, the difference rate of the deep ultraviolet phase difference between the hydrogels under the same deformation is not more than 2% in 10 repeated compression processes; meanwhile, the phase difference error caused by 10 times of repeated stretching light modulation does not exceed 2 percent, and as shown in FIG. 16, the optical hydrogel with adjustable birefringence has good stability.
Comparative example 4
This comparative example, which prepared an optical hydrogel with adjustable birefringence, differs from example 2 in that: this comparative example shows that the dilution concentration of the cobalt-doped two-dimensional titania liquid crystal in step S1 of example 2 is set to 5X 10 -4 The wt% is adjusted to 5X 10 -5 wt%, other operations were the same as in example 2.
The birefringence-tunable optical hydrogels prepared in example 2 and this comparative example were subjected to characterization test according to the characterization method of the magnetic response of the liquid crystal material in example 1, and the obtained results are shown in fig. 17. According to the test results, the concentration of the cobalt-doped two-dimensional titanium dioxide liquid crystal pair in the comparative example is too low, the birefringence value of the optical hydrogel product is extremely small, and the practical application is difficult to realize.
Comparative example 5
This comparative example prepared an optical hydrogel, which differs from example 2 in that: this comparative example shows that the dilution concentration of the cobalt-doped two-dimensional titania liquid crystal in step S1 of example 2 is set to 5X 10 -4 The wt% is adjusted to 5X 10 -2 wt%, other operations were the same as in example 2.
The optical hydrogel prepared in the comparative example is tested by a transmission spectrometer, and the liquid crystal in the optical hydrogel prepared in the comparative example has extremely low deep ultraviolet transmittance, and the average transmittance within a deep ultraviolet band of 300-350 nm is less than 10%, so that the optical hydrogel is difficult to be practically applied.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. The birefringence-adjustable optical hydrogel 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 cross-linked structure, and the magnetic element-doped two-dimensional titanium dioxide liquid crystals are filled in the network cross-linked structure and are arranged in an oriented manner.
2. The birefringence-tunable optical hydrogel according to claim 1, wherein the magnetic element doped in the two-dimensional titania liquid crystal is selected from at least one of cobalt, manganese, and nickel.
3. The birefringence-tunable optical hydrogel according to claim 1, wherein the amount of the magnetic element doped in the magnetic-element-doped two-dimensional titanium dioxide liquid crystal is controlled to be 3 to 9% in terms of the molar ratio of the magnetic element to the titanium element.
4. The birefringence-tunable optical hydrogel of claim 1, wherein the aspect ratio of the magnetic element doped two-dimensional titanium dioxide liquid crystal is 10 3 The above.
5. The birefringence-tunable optical hydrogel according to any one of claims 1 to 4, wherein the mass ratio of the magnetic-element-doped two-dimensional titanium dioxide liquid crystal to the optical hydrogel is 10 -4 ～10 -3 wt％。
6. A method of preparing a birefringence-tunable optical hydrogel according to any one of claims 1 to 5, comprising the steps of:
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;
and S2, transferring the mixed solution into a mold, and carrying out ultraviolet curing under the action of a magnetic field.
7. The method for preparing an optical hydrogel with adjustable birefringence according to claim 6, wherein step S1 comprises: firstly, mixing a magnetic element doped two-dimensional titanium dioxide liquid crystal and a solvent to prepare a mixture with the concentration of 10 -4 ～10 -3 Adding polymer monomer accounting for 3-5 wt% of the liquid crystal solution and photosensitizer accounting for 0.3-1 wt% of the liquid crystal solution, and mixing to prepare mixed solution.
8. The method for preparing an optical hydrogel with adjustable birefringence according to claim 6, further comprising the steps of, before step S1: s0, preparing a magnetic element doped two-dimensional titanium dioxide liquid crystal by an ion intercalation method; preferably, step S0 includes:
(1) Mixing the preparation raw materials including titanium dioxide, a magnetic element source and carbonate, and calcining to obtain a calcined product;
(2) Mixing the calcined product with protonic acid to perform a first intercalation reaction to prepare a first intercalation product;
(3) Mixing the first intercalation product with organic base, and carrying out a second intercalation reaction to prepare a second intercalation product;
(4) And mechanically stripping the second intercalation product in a liquid phase to prepare the magnetic element doped two-dimensional titanium dioxide liquid crystal.
9. Use of the birefringence-tunable optical hydrogel of any one of claims 1 to 5 in the fields of optical communication, laser polarization technology, polarization information processing, or precision measurement.
10. An optical device comprising the adjustable-birefringence optical hydrogel according to any one of claims 1 to 5.
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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 |
| 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 |
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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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