CN101942058A - Infrared photodeformable liquid crystal high-polymer nano composite material and preparation method thereof - Google Patents
Infrared photodeformable liquid crystal high-polymer nano composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of nano composite materials, and particularly relates to an infrared photodeformable liquid crystal high-polymer nano composite material and a preparation method thereof. The composite material comprises liquid crystal high polymers containing azobenzene and derivatives thereof, and rare-earth light-emitting nano particles, wherein the liquid crystal high polymers are prepared from polymer monomers and a cross-linking agent through photopolymerization or thermal polymerization in the presence of a photoinitiator or a thermal initiator. The composite material can realize photoinduced deformation under the irradiation of infrared light, and can restore after stopping irradiation. The liquid crystal high-polymer nano composite material can be used in the fields of micro actuators, artificial muscles, biochips and the like.
Description
Technical field
The invention belongs to the nano composite material technical field, be specifically related to a kind of photo-deformable liquid crystal polymer nano composite material and preparation method thereof.
Background technology
Photo-induced deformation liquid crystal macromolecular material is a kind of intelligent shape-changing material by light guide, be embodied in: when material is subjected to rayed, (be generally UV-light and visible light), its inner photoisomerization that takes place reacts the dimensional change that causes corresponding section, and by between liquid crystal molecule and the intersegmental synergy of macromolecular chain this micro-variations is passed to molecular chain, the state generation significance of molecular chain is changed, and material shows as photo-deformable on macroscopic view.After illumination stopped, the reaction of reversible photoisomerization took place again in material, and the form of molecular chain is correspondingly restored, and material then restores to the original state, and also can quicken its recovery process by heating or with the rayed (being generally visible light) of other wavelength certainly., can constantly realize, and tangible fatigue phenomenon does not appear in material to recovering whole process from photo-deformable.Only a kind of clean energy, Environmental Safety can realize that by photo-deformable luminous energy arrives the direct conversion of mechanical energy, avoids energy through repeatedly transforming the loss that causes, and has improved the utilising efficiency of luminous energy.Photo-induced deformation liquid crystal macromolecular material is widely used, at artificial-muscle, and Photoinduction device, the miniature instrument field, and in aviation, all have suitable application potential and development prospect.
Photo-induced deformation liquid crystal macromolecular material should have the group that reversible photoisomerization reaction can take place on the chemical structure, have by the cis-trans isomerism reaction, as nitrogen benzide, toluylene; Have by the dipole ion formation reaction, as the benzo spiro-pyrans; Have by cyclization, as fulgide; Have by the ion pair formation reaction, as triarylmethane derivatives; Realize by some other reaction in addition.Simultaneously material also must have liquid crystal liquid crystal property, and mesomorphic unit can be on main chain, also can be on side chain.Because the ordered arrangement characteristic of liquid crystal makes mesomorphic unit under the light action of specific wavelength, and more consistent variation takes place, again by with the coupling of macromolecular chain, thereby the deformation of realization microcosmic on the macroscopic view.
Relevant in the past containing in nitrogen benzide and the chromophoric crosslinked fluid polycrystalline macromolecule research of derivative thereof it has been found that this material has a kind of special photoresponse performance, and the contraction and the three-dimensional crooked deformation of one dimension, two dimension can take place after absorbing luminous energy.
But, can only realize photo-deformable (200710038100.3,200810032771.3,200910045903.0) by utilizing absorption UV-light or visible light energy at present.Yet, utilize infrared luminous energy to realize that photo-deformable has prior meaning, because infrared light not only has lower energy, and have Noninvasive and dark penetrativity, thereby the controlled photic shape-changing material of infrared light will have more wide application prospect.
On the other hand, nano material is the very important basic substance of Future Social Development, and the breakthrough of many scientific and technological frontiers presses for nano material and nanosecond science and technology support, and nano material and technical support also are badly in need of in the skill upgrading of conventional industries.The application of rare earth nano material is to relate to every field, has a wide range of applications in machinery, electronics, optics, magnetics, chemistry and biology field.
Rare earth luminous nano material has unique up-conversion luminescence character, can absorb the long wavelength light of near-infrared region, and emission is positioned at the short-wavelength light in ultraviolet-visible district.Rare earth luminous nano material has advantages such as emission is narrow, life-span length, bleach-resistant.The method for preparing rare earth nano material has Pintsch process, hydro-thermal (solvent thermal) method etc., and the rare earth nano material periphery of these method preparations is alkyl chains, for hydrophobic, can be scattered in the organic solvent.
Therefore, photo-induced deformation liquid crystal macromolecular material and rare earth luminous nano material is compound, can realize that matrix material absorbs infrared luminous energy and photo-deformable takes place.
Summary of the invention
The objective of the invention is to propose a kind ofly can realize liquid crystal polymer nano composite material of photo-deformable and preparation method thereof by infrared light control.
The infrared photo-deformable liquid crystal polymer nano composite material that the present invention proposes is made up of liquid crystal polymer that contains nitrogen benzide and derivative thereof and rare earth luminous nanoparticle.
The used liquid crystal polymer of the present invention is by monomer X and linking agent Y, under the condition that light trigger or thermal initiator exist, obtains by photopolymerization reaction or heat polymerization.
The general structure of described monomer X is:
D
1——A
1——R
The general structure of described linking agent Y is:
D
2——A
2——D
3
Wherein R is H, or C
1-C
18Replacement or unsubstituted alkyl (can be saturated or unsaturated) or alkoxyl group, or have the polar end group, selectable have cyano group, isocyano-, hydroxyl, halogen (F, Cl, Br, I), ester group, carboxyl, nitro, amino or an amide group etc.
A
1, A
2Be selected from a kind of in the following structure (1-12) or two kinds or three kinds (two kinds or three kinds situation is with pairing structure keyed jointing, and the mode of keyed jointing can be chosen arbitrarily) from about counter structure, can be the same or different.And A
1, A
2In have one at least for containing the conjugated structure of nitrogen benzide, infinite example such as structure 13-15.
B, B among the structure 5-12
1, B
2Be replacement or unsubstituted aliphatics ring, aromatic ring, condensed ring, heterocycle, or their corresponding derivatives, can be the same or different.
D
1～D
3Be the group that contains the polyreaction structure of functional groups, selectable have carbon-carbon double bond structure, an ethylene oxide structure, the group of isocyanic ester structure etc., they can independently be selected from a kind of in the following structure, can be the same or different infinite example such as structure 16-21.
R wherein
1Be H or CH
3R
2Be H, perhaps in the monomer general formula, do not occur, or C
1-C
18Replacement or unsubstituted alkyl or alkoxyl group, alkylthio, alkylamino, dialkylamino, alkyloyl, alkanoyloxy, alkyl amide, alkane alkylsulfonyl, or their corresponding derivatives.
In an optimized technical scheme, R is C preferably
1～C
12Replacement or unsubstituted alkyl or alkoxyl group, or have the polar end group, described have the polar end group preferably from F, Cl, Br, I or ester group.
In an optimized technical scheme, R
2C preferably
1～C
12Replacement or unsubstituted alkyl, described alkyl can be saturated or unsaturated, or is selected from alkoxyl group.
Wherein, light trigger of the present invention is selected from organic carbonyl complex and organo-metallic compounds, and preferably from Irgacure 784, Irgacure 819, their structural formula is as follows:
The thermal initiator that the present invention relates to is selected from azo compound, preferably from Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile).
Wherein, the selected light trigger or the consumption of thermal initiator are the 0.1%-10% of monomer and linking agent mole number sum, preferably 1%-5%.
The rare earth ion that rare earth luminous nanoparticle of the present invention uses is fluorochemical or fluorochemical sodium salt or oxide compound or the phosphoric acid salt or the vanadate of rare-earth elements of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), scandium (Sc) and yttrium (Y); The Er that perhaps mixes, Yb/Er, Yb/Ho, Yb, the fluorochemical of the rare earth element of Tm or fluorochemical sodium salt, oxyhydroxide, oxide compound, composite oxides, carbonate, titanate, borate, phosphoric acid salt, tungstate or vanadate.This type of rare earth luminous nano material can prepare by the synthetic method of routine, for example, hydrothermal method (Li YD, Nature 2005,437, and 121; Inorganic Chemistry 2006,45,6661, Chemistry of Materials, 2007,19,727) or pyrolysis method (Capobianco J A, Journal of the American Chemical Society, 2006,128,7444; Yan CH, Journal of the American Chemical Society 2005,127,3260) or other method.And the rare earth luminous nano material for preparing has the character of up-conversion luminescence, can absorb the near infrared long wavelength light and launch the UV, visible light short-wavelength light.The rare earth luminous nanoparticle size is 10-1000nm.
The molar ratio of contained monomer of liquid crystal polymer and linking agent is 99 among the present invention: 1-1: 99.In an optimized technical scheme, be preferably 90: 10-10: 90.
The quality ratio of liquid crystal polymer nano composite material middle-weight rare earths luminescent nanoparticle of the present invention and liquid crystal polymer is 20: 80-0.1: 99.9.In an optimized technical scheme, be preferably 10: 90-1: 99.
Liquid crystal polymer nano composite material of the present invention is made up of liquid crystal polymer and rare earth luminous nanoparticle, it is characterized in that, as body material, rare earth luminous nanoparticle is as packing material by liquid crystal polymer.Can adopt the in-situ polymerization method of forming or two one-step forming legal systems to be equipped with the liquid crystal polymer nano composite material.Wherein:
The in-situ polymerization method of forming: at first with high molecular polymerization monomer X, linking agent Y, initiator and rare earth luminous nanoparticle melting mixing or dissolving dispersing and mixing are even.Then the mixture that obtains is injected in the reaction mould of definite shape, by heating (or illumination) polyreaction is taken place, the demoulding more just can obtain the liquid crystal polymer nano composite material.Also mixture can be filmed, pass through photopolymerization (thermopolymerization) again and form the liquid crystal polymer nano composite material.
Two one-step forming methods: at first prepare linear polymer by photopolymerization or thermopolymerization, with linking agent Y, initiator and rare earth luminous nanoparticle mix, as Preblend again.Then Preblend is prepared difform liquid crystalline polymers nano composite material by further forming process, method for processing forming can be selected methods such as injection molding, hot-forming, vacuum compression molding, injection moulding, extrusion moulding for use.
The matrix material of method for preparing needs further to solidify.And, can adopt photopolymerization for curing process, wherein, selected wavelength region is 300nm-800nm when carrying out photopolymerization, preferably 400nm-600nm; The light intensity scope is 0.1mW/cm
2-20mW/cm
2, 1mW/cm preferably
2-10mW/cm
2Carrying out photopolymerisable polymerization time scope is 0.5h-48h, preferably 2h-20h; The polymerization temperature scope is 50 ℃-200 ℃, preferably 80 ℃-150 ℃.Also can adopt thermopolymerization, the polymerization time scope of carrying out thermopolymerization is 1h-100h, preferably 3h-50h; The polymerization temperature scope is 20 ℃-200 ℃, preferably 40 ℃-150 ℃.
The present invention also provides the method that makes described liquid crystal polymer nano composite material generation deformation and recovery, specifically is, makes matrix material produce deformation under the irradiation of infrared light, stops can be returned to original state again after infrared light shines.In this method, the infrared light wavelength scope of the photo-deformable of control matrix material is the near-infrared band of 800-2000nm, and luminous power is 1-10W.After stopping illumination, because the heat effect of infrared light intensity can make deformation recovery.
This liquid crystal polymer nano composite material can be used for fields such as microactrator spare, artificial-muscle, biochip.
Description of drawings
Fig. 1 is the Experimental equipment of synthetic liquid crystal polymer nano composite material.Wherein the implication of mark is: the 1-radiating light source, and the 2-interval insulant, the 3-frictional direction, 4-heats supervisory control desk, 5-substrate, 6-liquid crystal cell.
Fig. 2 is the macroscopic deformation behavior synoptic diagram that occurs of liquid crystal polymer nano composite material under the near infrared light effect.
Number in the figure: the 1-radiating light source, the 2-interval insulant, the 3-frictional direction, 4-heats supervisory control desk, 5-substrate, 6-liquid crystal cell;
The 7-substrate, 8-liquid crystal polymer nano composite material, the 9-frictional direction, the 10-infrared light, the liquid crystal polymer nano composite material of deformation takes place in 11-, and 12-recovers the liquid crystal polymer nano composite material of initial state.
Embodiment
According to accompanying drawing, the present invention will be further described.Select monomer vinylformic acid-9-{4-[(4 '-(4 "-ethoxyl phenenyl ethynyl)-2 '-methyl for use) phenylazo] phenoxy group } ester in the ninth of the ten Heavenly Stems (A9ABT), [4-(11-acryloxy) undecane oxygen base-4 '-oxygen base] just nitrogen benzide (A11AB6) and linking agent DA9ABT, 4,4 '-two [11-(acryloxy) undecane oxygen base] nitrogen benzide (DA11AB) preparation liquid crystal high polymer material.Select NaLaF for use
4: 1-5mol%Tm, 20-50mol%Yb is as rare earth luminous nanoparticle.
This embodiment has illustrated the process for preparing the liquid crystal polymer nano composite material according to the in-situ polymerization method of forming of the present invention.See also shown in Figure 1ly, at first A11AB6 and DA11AB are pressed 90: 10 proportionings of mole number, add the light trigger of A11AB6 and DA11AB mole number sum 5% then, add the rare earth luminous nanoparticle of A11AB6 and DA11AB quality sum 10% again.Mix the back fusion and inject two liquid crystal cells 6 that substrate 5 is made, two 5 of substrates have been placed the certain interval insulant 2 of diameter makes the certain interval of maintenance between the two substrates 5 to control the thickness of prepared liquid crystal polymer nano composite material, the internal surface of substrate 5 is directed and rubbed, so that mesomorphic unit aligns along frictional direction, frictional direction 3 is seen shown in the figure, then use warm table 4 control reaction temperature at 80 ℃, and the wavelength that is sent at light source 1 is greater than 545nm, and light intensity is 3mW/cm
2The following reaction 8h of illumination, open liquid crystal cell 6 and obtain the liquid crystal polymer nano composite material.
This embodiment has illustrated the process for preparing the liquid crystal polymer nano composite material according to the in-situ polymerization method of forming of the present invention.See also shown in Figure 1, at first A9ABT and DA9ABT are pressed 90: 10 proportionings of mole number, the thermal initiator 2,2'-Azobis(2,4-dimethylvaleronitrile) that adds A9ABT and DA9ABT mole number sum 5% then adds the rare earth luminous nanoparticle of A9ABT and DA9ABT quality sum 10% again.Mix the back fusion and inject two liquid crystal cells 6 that substrate 5 is made, two 5 of substrates have been placed the certain interval insulant 2 of diameter makes the certain interval of maintenance between the two substrates 5 to control the thickness of prepared liquid crystal polymer nano composite material, the internal surface of substrate 5 is directed and rubbed, in order that mesomorphic unit is aligned along frictional direction, frictional direction 3 is seen shown in the figure, then with 100 ℃ of warm table 4 control reaction temperature, reaction 24h opens liquid crystal cell 6 and obtains the liquid crystal polymer nano composite material.
This embodiment has illustrated the control of the photo-deformable of liquid crystal polymer nano composite material.Ask for an interview shown in Figure 2, the liquid crystal polymer nano composite material 8 that obtains among embodiment 1 or the embodiment 2 is placed on the substrate 7, starting wavelength above perpendicular to described liquid crystal polymer nano composite material 8 then is 980nm, power is the laser apparatus 10 of 3W, can observe liquid crystal polymer nano composite material 8 this moment and bend towards the liquid crystal polymer nano composite material 11 that light source has formed generation deformation along frictional direction 9.After stopping laser apparatus 10 irradiations, the liquid crystal polymer nano composite material 11 that can be observed described generation deformation has again become the liquid crystal high polymer material 12 of replying original state, the multi-pass operations that can circulate of this process, and liquid crystal high polymer material 8 itself obvious fatigue do not occur.
This embodiment has illustrated the process for preparing the liquid crystal polymer nano composite material according to the in-situ polymerization method of forming of the present invention.At first A11AB6 and DA11AB are pressed 90: 10 proportionings of mole number, the light trigger that adds A11AB6 and DA11AB mole number sum 5% then, the rare earth luminous nanoparticle that adds A11AB6 and DA11AB quality sum 10% again, with the chloroform is that dispersion solvent mixes, then the rotating speed of mixing solutions by 1000-10000 rev/min is spin-coated on the substrate, selects different rotating speeds to control coating thickness.Then with the warm table control reaction temperature at 80 ℃, and at wavelength greater than 545nm, light intensity is 3mW/cm
2The following reaction 8h of illumination, obtain the liquid crystal polymer nano composite material.
This embodiment has illustrated the process for preparing the liquid crystal polymer nano composite material according to the in-situ polymerization method of forming of the present invention.At first A9ABT and DA9ABT are pressed 90: 10 proportionings of mole number, the thermal initiator 2,2'-Azobis(2,4-dimethylvaleronitrile) that adds A9ABT and DA9ABT mole number sum 5% then, the rare earth luminous nanoparticle that adds A9ABT and DA9ABT quality sum 10% again, with the chloroform is that dispersion solvent mixes, then the rotating speed of mixing solutions by 1000-10000 rev/min is spin-coated on the substrate, selects different rotating speeds to control coating thickness.Then with 100 ℃ of warm table control reaction temperature, reaction 24h obtains the liquid crystal polymer nano composite material.
This embodiment has illustrated the process that is equipped with the liquid crystal polymer nano composite material according to two one-step forming legal systems of the present invention.At first prepare linear polymer: with monomer A 11AB6, light trigger (be monomer A 11AB6 mole number 5%) mixes, and greater than 545nm, light intensity is 3mW/cm at wavelength
2The following reaction 4h of illumination, obtain the linear polymer that molecular weight is the 5000-50000 scope.Then linear polymer and linking agent DA11AB6 are pressed 80: 20 proportionings of mass ratio, add the light trigger of linear polymer and linking agent quality sum 5% again, mix the back as Preblend.Utilize injection moulding machine-shaping then, earlier bed die is fixed, preheating, utilize injection machinery again under the pressure condition of 150-500Kpa, by an inlet Preblend is squeezed into and makes it moulding in the model.At last with moulding product at wavelength greater than 545nm, light intensity is 3mW/cm
2Illumination down reaction 8h carry out crosslinking curing, this method easily is automated and batch preparations.
This embodiment has illustrated the process that is equipped with the liquid crystal polymer nano composite material according to two one-step forming legal systems of the present invention.At first prepare linear polymer: with monomer A 9ABT, thermal initiator (be monomer A 9ABT mole number 5%) mixes, and at 100 ℃ of temperature reaction 24h down, obtains the linear polymer that molecular weight is the 5000-50000 scope.Then linear polymer and linking agent DA9ABT are pressed 80: 20 proportionings of mass ratio, add the thermal initiator of linear polymer and linking agent quality sum 5% again, mix the back as Preblend.Utilize injection moulding machine-shaping then, earlier bed die is fixed, preheating, utilize injection machinery again under the pressure condition of 150-500Kpa, by an inlet Preblend is squeezed into and makes it moulding in the model.At last moulding product is reacted 24h under 100 ℃ temperature condition and carry out crosslinking curing, this method easily is automated and batch preparations.
Claims (10)
1. one kind infrared photo-deformable liquid crystal polymer nano composite material is characterized in that by the liquid crystal polymer that contains nitrogen benzide and derivative thereof and rare earth luminous nanoparticle is compound forms; Described liquid crystal polymer, is obtained by photopolymerization reaction or heat polymerization under the condition of light trigger or thermal initiator existence by monomer X and linking agent Y; Wherein:
The general structure of described monomer X is: D
1---A
1---R
The general structure of described linking agent Y is: D
2---A
2---D
3
Wherein R is H, or C
1-C
18Replacement or unsubstituted alkyl or alkoxyl group, or have the polar end group;
A
1, A
2Be selected from following structural formula (1)--one or both or three kinds in the structural formula (12); And A
1, A
2In have one at least for containing the conjugated structure of nitrogen benzide;
B, B in structural formula (5)--the structural formula (12)
1, B
2Be to replace or unsubstituted aliphatics ring, aromatic ring, condensed ring or heterocycle, or their corresponding derivatives;
D
1～D
3Be the group that contains the polyreaction structure of functional groups, and be selected from following structural formula (16)--a kind of in the structural formula (21):
R wherein
1Be H or CH
3R
2Be H, perhaps in the monomer general formula, do not occur, or C
1-C
18Replacement or unsubstituted alkyl or alkoxyl group, alkylthio, alkylamino, dialkylamino, alkyloyl, alkanoyloxy, alkyl amide or alkane alkylsulfonyl, or their corresponding derivatives.
2. infrared photo-deformable liquid crystal polymer nano composite material according to claim 1 is characterized in that the described rare earth luminous particulate material of receiving is fluorochemical or fluorochemical sodium salt or oxide compound or the phosphoric acid salt or the vanadate of rare-earth elements of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium or yttrium; The Er that perhaps mixes, Yb/Er, Yb/Ho, Yb, the fluorochemical of the rare earth element of Tm or fluorochemical sodium salt, oxyhydroxide, oxide compound, composite oxides, carbonate, titanate, borate, phosphoric acid salt, tungstate or vanadate.
3. infrared photo-deformable liquid crystal polymer nano composite material according to claim 1 is characterized in that the molar ratio of monomer and linking agent is 99 in the described liquid crystal polymer: 1-1: 99.
4. infrared photo-deformable liquid crystal polymer nano composite material according to claim 1, the quality ratio that it is characterized in that described rare earth luminous nanoparticle and liquid crystal polymer is 20: 80-0.1: 99.9.
5. infrared photo-deformable liquid crystal polymer nano composite material according to claim 1 is characterized in that described light trigger is selected from organic carbonyl complex and organo-metallic compounds.
6. infrared photo-deformable liquid crystal polymer nano composite material according to claim 1 is characterized in that described
Thermal initiator is selected from azo compound.
7. according to claim 1,5 or 6 described infrared photo-deformable liquid crystal polymer nano composite materials, the consumption that it is characterized in that described light trigger or thermal initiator is the 0.1%-10% of monomer and linking agent mole number sum.
8. as the preparation method of the described infrared photo-deformable liquid crystal polymer nano composite material of one of claim 1-7, it is characterized in that, by liquid crystal polymer as body material, rare earth luminous nanoparticle adopts the in-situ polymerization method of forming or two one-step forming methods to be prepared into the liquid crystal polymer nano composite material as packing material; Wherein:
The in-situ polymerization method of forming: at first with high molecular polymerization monomer X, linking agent Y, initiator and rare earth luminous nanoparticle mix, and the mixture that obtains are injected in the reaction mould of definite shape or film, and by heating or illumination, carry out polyreaction; The demoulding again obtains the liquid crystal polymer nano composite material;
Two one-step forming methods: at first prepare linear polymer by photopolymerization or thermopolymerization, with linking agent Y, initiator and rare earth luminous nanoparticle mix, as Preblend again; Then Preblend is prepared difform liquid crystalline polymers nano composite material by further forming process.
9. preparation method according to claim 8 is characterized in that the composite material by adopting photopolymerization of gained or thermopolymerization method are cured; Wherein, when adopting light polymerization process, optical wavelength is 300nm-800nm, and light intensity is 0.1mW/cm
2-20mW/cm
2, the photopolymerization time is 0.5h-48h, the photopolymerization temperature is 50 ℃-200 ℃; When adopting the thermopolymerization method, the thermopolymerization time is 1h-100h, and the thermopolymerization temperature is 20 ℃-200 ℃.
10. as the using method of the described infrared photo-deformable liquid crystal polymer nano composite material of one of claim 1-7, it is characterized in that adopting the infrared light irradiation, selecting the infrared light wavelength is the near-infrared band of 800-2000nm, luminous power is 1-10W, makes liquid crystal polymer nano composite material generation deformation; Stop illumination, make liquid crystal polymer nano composite material deformation recovery.
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| CN103483495A (en) * | 2013-09-16 | 2014-01-01 | 复旦大学 | Photoinduced-deformation high polymer material based on triplet state-triplet state annihilation up-conversion luminescence |
| CN103483495B (en) * | 2013-09-16 | 2016-08-17 | 复旦大学 | Photo-deformable macromolecular material based on triplet state-triplet state annihilation up-conversion luminescence |
| CN103524678A (en) * | 2013-10-10 | 2014-01-22 | 湖北大学 | Liquid crystal elastomer composite material for optical actuator and preparation method thereof |
| CN104591253A (en) * | 2015-02-02 | 2015-05-06 | 首都师范大学 | Microemulsion synthesis method of porous water-soluble rare earth nano material |
| CN105124599A (en) * | 2015-08-13 | 2015-12-09 | 张德盛 | Life-nourishing and health-care material and production method thereof |
| CN111255778A (en) * | 2018-11-30 | 2020-06-09 | 西湖大学 | Light-operated liquid drop movement method, light-operated liquid drop movement microtube and manufacturing method thereof |
| CN111255778B (en) * | 2018-11-30 | 2021-06-01 | 西湖大学 | Light-operated liquid drop movement method, light-operated liquid drop movement microtube and manufacturing method thereof |
| CN109803524A (en) * | 2019-03-11 | 2019-05-24 | 京东方科技集团股份有限公司 | A kind of intelligent glass |
| CN109803524B (en) * | 2019-03-11 | 2020-07-28 | 京东方科技集团股份有限公司 | Intelligent glass |
| CN112321872A (en) * | 2020-10-29 | 2021-02-05 | 合肥乐凯科技产业有限公司 | Color optical film and preparation method thereof |
| CN112321872B (en) * | 2020-10-29 | 2022-04-15 | 合肥乐凯科技产业有限公司 | Color optical film and preparation method thereof |
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