CN1811528A - MEMS liquid crystal light attenuator array and producing method thereof - Google Patents

MEMS liquid crystal light attenuator array and producing method thereof Download PDF

Info

Publication number
CN1811528A
CN1811528A CNA2006100165226A CN200610016522A CN1811528A CN 1811528 A CN1811528 A CN 1811528A CN A2006100165226 A CNA2006100165226 A CN A2006100165226A CN 200610016522 A CN200610016522 A CN 200610016522A CN 1811528 A CN1811528 A CN 1811528A
Authority
CN
China
Prior art keywords
liquid crystal
array
optical fiber
crystal material
light
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CNA2006100165226A
Other languages
Chinese (zh)
Other versions
CN100367082C (en
Inventor
陈维友
张歆东
刘彩霞
董玮
阮圣平
仲志成
周敬然
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jilin University
Original Assignee
Jilin University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jilin University filed Critical Jilin University
Priority to CNB2006100165226A priority Critical patent/CN100367082C/en
Publication of CN1811528A publication Critical patent/CN1811528A/en
Application granted granted Critical
Publication of CN100367082C publication Critical patent/CN100367082C/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The present invention belongs to the field of photoelectronic device, in the concrete, it relates to a kind of MEMS liquid crystal optical attenuator array and its making method. Said MEMS liquid crystal optical attenuator array is formed from single crystal silicon substrate, incidence optical fibre and emergence optical fibre coupling array and liquid crystal microgroove for filling polymer dispersed liquid crystal material. The polymer dispersed liquid crystal material in the liquid crystal microgroove is made up by using 30-90 wt% of liquid crystal material, 5-65 wt% of mixture of polymer monomer and proper quantity of diluting agent and 1-5 wt% of photoinitiator through the processes of fully stirring and UV curing treatment, in which the weight ratio of polymer monomer and diluting agent is 1:5-5:1, and on the electrode pair of single crystal silicon substrate an electric field is applied, so that the invented MEMS liquid crystal photoattenuator array can be obtained.

Description

MEMS liquid crystal light attenuator array and method for making
Technical field
The invention belongs to field of optoelectronic devices, be specifically related to a kind of based on the MEMS liquid crystal light attenuator array of polymer dispersion liquid crystal material and the method for making of this liquid crystal attenuator array.
Background technology
Optical attenuator is a kind of device that is intended to reduce the luminous power of transmitting in the waveguide.The market potential of optical attenuator is big at present, and in passive device, its output is only second to connector, coupling mechanism etc.Along with developing rapidly of broadband optical communication network, particularly all-optical network, for guaranteeing communication quality, in optical-fiber network, be necessary the luminous power of each wavelength to be carried out equilibrium at node, variable optical attenuator is exactly wherein important a solution.
Formed fixed at present, stepping is adjustable, four kinds of series of continuous adjustable and intelligent optical attenuator, but business-like optical attenuator almost is the mechanical type large volume optical attenuator that conventional art is made entirely both at home and abroad, utilize input, being subjected to displacement or inserting in light transmission path shelter during the output optical fibre butt joint comes the luminous power of transmission is decayed, and be subject to people's attention day by day based on the very little optical attenuator of the volume of MEMS technical matters manufacturing, be in conceptual phase, optical communication market is to present hyperchannel, integrated variable optical attenuator has good demand, high-performance, low-cost, the development of the novel changable light attenuator array of miniaturization obtains the very big concern of educational circles and industrial community.
Along with the widespread use of liquid crystal material in recent years, people have carried out a large amount of deep researchs to the various electrooptical effects of liquid crystal, on telecommunications is used, because liquid crystal material has high penetration to near-infrared wavelength, so its element has low insertion loss and hypopolarization dependent loss, and liquid crystal cell has very big operation frequency range and the advantage of making miniaturization, makes them quite be suitable for application in optical WDM communication.
Particularly this research field of Polymer Dispersed Liquid Crystal system (PDLC) more and more is subjected to people's attention in recent years, when applying extra electric field, the behavior of liquid crystal molecule is subjected to the effect of polymer network, to tend to be orientated along direction of an electric field, because the ordinary refractive index of liquid crystal molecule and the refractive index of matrix are complementary, light can be through state; Remove extra electric field, liquid crystal particle recovers initial scattering state again under the effect of matrix.
Summary of the invention
The method for making that the purpose of this invention is to provide a kind of MEMS liquid crystal light attenuator array based on polymer dispersion liquid crystal material.
Device has made full use of the electro-optical characteristic of polymer liquid crystal material uniqueness and the crystallographic characteristics of Si monocrystalline, and with body bulk silicon process and the combination of polymer liquid crystal technique, novel structure, the traditional optical attenuator volume that has overcome present application is big, complex process, be not easy to deficiencies such as integrated.Compare with common liquid crystal type optical attenuator, the polymer liquid crystal optical attenuator need not polaroid, does not need liquid crystal material is carried out special orientation process, and structural design is simple.
MEMS liquid crystal light attenuator based on polymer dispersion liquid crystal material of the present invention is made up of the liquid crystal microflute of monocrystalline substrate, incident optical and outgoing optical fiber coupling array, filled polymer dispersed liquid crystal material, it is characterized in that:
(1) self aligned V-type groove array is arranged on silicon substrate, on the silicon substrate that comprises V-type groove array, be deposited with silicon dioxide layer and conductive metal layer successively, wherein silicon dioxide layer plays the insulation buffer action, and the conductive metal layer insulation between V-type groove array disconnects, and forms driving electrode array;
(2) be deposited with the ITO transparent conductive film in the end face and the side of incident optical and emergent light fibre array, incident optical and outgoing optical fiber are placed in the self aligned V-type groove of the silicon substrate array, the conductive film of its end face and side links to each other with metal level on being deposited on silicon substrate, disconnect with the metal level that incident optical links to each other with outgoing optical fiber, form the both positive and negative polarity electrode pair of drive electrode;
(3) on the light-path of incident optical that is coupled and the formation of outgoing optical fiber, with the silicon substrate of incident optical and outgoing optical fiber vertical direction on be carved with square type liquid crystal microflute, in square type liquid crystal microflute, be filled with the polymer dispersion liquid crystal material for preparing, be coated with the incident optical of ITO transparent conductive film and the end face of outgoing optical fiber coupling array and be close to liquid crystal material, thereby prepare the MEMS liquid crystal light attenuator array.
Extraction electrode on the conductive layer of MEMS liquid crystal light attenuator array silicon substrate, apply on the polymer dispersion liquid crystal material of electric field action in the liquid crystal microflute, just can utilize the variation of the scattering of light effect that Polymer Dispersed Liquid Crystal causes under different electric field intensity, but realize controlling attenuation, thereby reach the purpose of the described preparation optical attenuator of this patent the light path energy.
Polymer dispersion liquid crystal material in the liquid crystal microflute is by the potpourri of the liquid crystal material that accounts for general assembly (TW) 30%~90%, 5%~65% polymer monomer and proper amount of diluting, 1%~5% light trigger ultra-violet curing and forming after abundant stirring, and wherein the weight ratio of polymer monomer and thinning agent is 1: 5~5: 1.
As preferred version, polymer dispersion liquid crystal material in the liquid crystal microflute is by the potpourri of the liquid crystal material that accounts for general assembly (TW) 50%~90%, 5%~45% polymer monomer and an amount of thinning agent, 1%~5% light trigger ultra-violet curing and forming after abundant stirring, and wherein the weight ratio of polymer monomer and thinning agent is 1: 3~3: 1.
As further preferred version, polymer dispersion liquid crystal material in the liquid crystal microflute is by the potpourri of the liquid crystal material that accounts for general assembly (TW) 65%~90%, 5%~30% polymer monomer and an amount of thinning agent, 1%~5% light trigger ultra-violet curing and forming after abundant stirring, and wherein the weight ratio of polymer monomer and thinning agent is 1: 2~2: 1.
MEMS liquid crystal light attenuator based on polymer dispersion liquid crystal material of the present invention is the method that adopts body silicon Micrometer-Nanometer Processing Technology, make full use of the crystallographic characteristics of silicon, the autoregistration fiber orientation groove of liquid crystal light attenuator device performance requirement is satisfied in making, liquid crystal microflute and transparency conductive electrode, the modulation process and the parameter of research polymer dispersion liquid crystal material, utilize the variation of the scattering of light effect that Polymer Dispersed Liquid Crystal causes under different electric field intensity, realize controllable continuous decay to the light path energy, thereby design and produce out the variable Polymer Dispersed Liquid Crystal type MEMS optical attenuator of a kind of new continuous, by to the adjustment of Polymer Dispersed Liquid Crystal modulation parameter and the optimization of device architecture, for the practicability of liquid crystal light attenuation device creates conditions with technical in theory.
MEMS liquid crystal light attenuator making step based on polymer dispersion liquid crystal material of the present invention is as follows:
The making of A, optical fiber autoregistration V-type groove: adopt body silicon Micrometer-Nanometer Processing Technology, utilize the crystallographic characteristics of silicon, on monocrystalline substrate 10, produce optical fiber autoregistration V-type groove 1 by photoetching, mask, etching and employing anisotropic wet corrosion technology;
The making of B, conductive electrode: on (100) silicon chip of making optical fiber autoregistration V-type groove, deposit SiO by magnetically controlled sputter method successively 2 Insulation course 3 and metal level 2 are made multi-channel electrode array structure 7 as shown in Figure 2; Simultaneously come deposit ITO transparent conductive film by magnetically controlled sputter method in the end face and the side of incident optical and emergent light fibre array 5, make the end face and the side of the fiber array 5 of putting into V-type groove array 1 have electric conductivity, and link to each other with electrode array configurations 7 electricity that the metal level 2 of deposition on silicon substrate 10 forms, on electrode array configurations 7, draw lead formation driving electrode array;
The making of C, liquid crystal microflute: utilization ICP dry etching technology, on silicon substrate, joint at incident optical and emergent light fibre array 5, make and the perpendicular rectangle liquid crystal microflute of optical fiber autoregistration V-type groove array, the metal electrode of producing electrode array configurations 7 simultaneously is right, utilize microscope and infrared thermoviewer that the coupling of device is observed again, when reaching coupling when requiring, with the ultraviolet glue solidification method incident optical and outgoing optical fiber are fixed in the V-type groove, liquid crystal light attenuation structure and its optical fiber self-alignment structure are become one;
The preparation of D, polymer dispersion liquid crystal material:
What the preparation method of polymer dispersion liquid crystal material (Polymer dispersed liquid crystals is called for short PDLC) adopted is the photopolymerization split-phase method, low molecular weight liquid crystal and polymer monomer carried out again being separated after mixing by required proportioning with proper amount of diluting, light trigger, to be nematic liquid crystal be present in the transparent polymer matrix with the form of droplet the result that PDLC is separated.The light-operated attenuation characteristic of Polymer Dispersed Liquid Crystal system is to rely on extra electric field that the orientation of liquid crystal droplet is regulated, and becomes in various degree scattering to realize thereby reach to ambient light.
The selection of a, material
Therefore the physicochemical property of liquid crystal material self play decisive influence to Polymer Dispersed Liquid Crystal (PDLC) device.Liquid crystal material must have positive specific inductive capacity, and is solvable in selected polymer monomer, and solubleness is very little aggregate into polymkeric substance under ultraviolet lighting after, perhaps is dissolved in polymkeric substance hardly, so that liquid crystal can be separated into little liquid crystal droplet.Reasonable liquid crystal material is the liquid crystal compound that contains aerobic base xenyl, and the liquid crystal compound that contains cyclohexyl, phenyl, a dihydrobenzene and cyano-phenyl also can be used.
In the polymer dispersion liquid crystal material system, the main body of photocuring is the potpourri of polymer monomer or monomer and an amount of monomer diluent.Its performance plays a decisive role to the speed of photocuring reaction and the main performances such as pattern, driving voltage of solidifying the back material.Polymer monomer is the low polymer that contains unsaturated functional group, and majority is the oligomer of acrylate.In general, polymer monomer material molecule amount is big more, and volumetric contraction is more little during curing, and curing rate is also very fast, but molecular weight is big more, and viscosity raises, and needs more monomer diluent to dilute.The prepolymer that is suitable for this patent has epoxy acrylate, polyurethane acrylate and some other unsaturated polyester (UP)s.
The monomer diluent material also is the key factor of decision curing system fundamental property.Monomer diluent links together the polymer monomer molecule in curing reaction, also plays a part crosslinking chemical.Need consider following character when selecting thinning agent: the viscosity of monomer diluent self, dilution capacity, to the dissolving power of light trigger, with the mutual compatibility of other component of system, volatility, the shrinkage factor of activity, functionality, polymerization and surface tension etc. to light source.What should particularly point out is: for what need among the present invention is transmission mould liquid crystal device, requires the refractive index of polymkeric substance to be complementary with liquid-crystal refractive-index, could be when extra electric field be arranged, and the transmittance maximum of liquid crystal composite film.Relatively Shi Yi diluent materials is an esters of acrylic acid, as methyl acrylate, ethyl acrylate, butyl acrylate, acrylic acid 2-hydroxypropyl acrylate, acrylic acid 2-hydroxyl ethyl ester etc., acrylic acid methoxyl ethyl ester etc.; Methacrylate, as methyl methacrylate, Jia Jibingxisuanyizhi, two propylene glycol diacrylate (TPGDA), trimethylolpropane triacrylate (TMPTA), the trimethylolpropane tris basic acrylate (TMPTM), 1 early that contracts, 6-hexanediol diene acid esters (HDDA); Methacrylate, as zinc methacrylate etc., and the methacrylic acid acid amides, these materials all can be by the ultraviolet lighting polymerization in the quite short time.
Under the certain situation of light source, can light trigger to PDLC device photopolymerization reaction decisive role take place.Light trigger is meant and can itself chemical change takes place after the portion of energy of absorbed radiation, is decomposed into free radical or kation, thus initiated polymerization.It is the material that produces the reactive intermediate with initiated polymerization ability.Whether the light-initiated efficient of light trigger has suitable absorption spectrum (with the coupling of optical source wavelength) with the relevant 1. light trigger of following three factors; 2. cause quantum efficiency; 3. light trigger and its fracture material do not participate in chain transfer and chain termination reaction, and the general concentration of light trigger in system is no more than 10%.Irgacure-184 is the non-yellowing light trigger of a kind of free radical type efficiently, can be used for UV ultraviolet polymerization simple function or multi-functional polymeric acrylic acid salt monomer and oligomer; Tiger red (Rose bengal) RB has good solubleness in multiple monomer resin matrix, it is not subjected to solvent effect substantially to the high absorption efficiency of light, and has higher active body (free radical or kation) quantum yield down light absorbing exciting, but itself is not enough to cause photopolymerization reaction, so how to make coinitiator with N-phenylglycine (NPG), play the H donor, finish polyreaction with RB.
The mixed solution of b, preparation liquid crystal, light trigger and polymer monomer and thinning agent;
After liquid crystal, polymer monomer, an amount of monomer diluent and light trigger take by weighing by certain weight ratio, heating under the shading condition, stir,, it is under isotropic state, fully stir again and make its even mixing mixture heated to 60~80 ℃; Liquid crystal material accounts for 30%~90% in the mixed solution, and prepolymer and monomer account for 5%~65%, and wherein prepolymer is 1: 5~5: 1 with the ratio of monomer, and light trigger accounts for 1%~5%;
The realization of E, attenuation function: the composite material in the above-mentioned steps is injected in the liquid crystal microflute, carrying out the UV-irradiation polymerization reaction take place induces it to be separated, the ultraviolet source wavelength available is the mercury vapor lamp of 300~500nm, and the time of light initiation polymerization is 1~10 minute; Like this polymer dispersion liquid crystal material on the optical transmission pathway is applied certain effect of electric field, can realize controllable continuous decay the light path energy.
Description of drawings
Fig. 1: the V-type fiber orientation groove synoptic diagram of on silicon substrate, making of the present invention;
Fig. 2: the multi-channel electrode structural design synoptic diagram of on silicon substrate, making of the present invention;
Fig. 3: of the present invention on silicon substrate etching liquid crystal micro groove structure synoptic diagram;
Fig. 4: integrated multichannel MEMS variable optical attenuator part-structure synoptic diagram of the present invention;
Fig. 5: (100) of the present invention silicon optical fiber autoregistration V-type groove manufacture craft schematic flow sheet;
(1) forms the photoresist mask;
(2) form silicon nitride mask;
(3) preparation V-type groove.
As shown in Figure 1, the autoregistration fiber orientation groove of on (100) monocrystalline substrate 10, making 1;
As shown in Figure 2, deposition comprises SiO on autoregistration fiber orientation groove 1 2 Insulation course 3 and metal level 2, further make discrete each other electrode array configurations 7 again.
As shown in Figure 3, utilization ICP dry etching technology, on silicon substrate 10, make and the perpendicular square type liquid crystal microflute 4 of optical fiber autoregistration V-type groove (light-path), be less than metal electrode to 7 distance at the width of light-path direction liquid crystal microflute 4, the metal electrode of having prepared electrode array configurations 7 simultaneously is right.
As shown in Figure 4, be the integrated multichannel MEMS variable optical attenuator part-structure synoptic diagram that is prepared into, its each component names is respectively: monocrystalline substrate 10 has the right electrode array configurations of metal electrode 7, SiO 2Insulation course 3, with the perpendicular liquid crystal microflute 4 of optical fiber autoregistration V-type groove, the Polymer Dispersed Liquid Crystal dispersion 6 that in liquid crystal microflute 4, injects, end face and side are coated with the incident optical and the emergent light fibre array 5 of the coupling of ITO transparent conductive film.
As shown in Figure 5, manufacture craft flow process for (100) silicon chip wet etching optical fiber autoregistration V-type groove, autoregistration fiber orientation groove figure 1 is transferred on the silicon chip 10 from mask, through gluing, preceding baking, exposure, development, post bake with after removing photoresist, the silicon chip cross section is shown in Fig. 5 (1), and photoresist 8 is made mask layer, further comes the silicon nitride layer 9 of etching silicon chip surface again, form the mask of anisotropic wet corrosion silicon, shown in Fig. 5 (2); With corrosive liquid silicon substrate is corroded, and then prepare V-type groove array, shown in Fig. 5 (3).
Add different electric fields for each electrode pair, in liquid crystal microflute 4, adopt the different polymer liquid crystal dispersions and the different component proportionings of material, the optical transmission rate of same light-path or different light-pathes is not quite similar, thereby realizes the function of the multi-path MEMS light attenuator array of this patent.
Embodiment
Embodiment 1:
A: make single pass optical fiber autoregistration V-type groove:
Select n type (100) silicon chip for use, 200~500 microns of thickness, resistivity is 4~6 Ω cm, utilizes silicon single crystal anisotropic wet corrosive property to make single pass optical fiber autoregistration V-type groove:
1) adopts Si 3N 4As insulation and etching mask layer, with low-pressure chemical vapor deposition LPCVD method growth Si 3N 4Mask layer, concrete technological parameter condition is as shown in table 1, the Si of growth 3N 4Film thickness be 150nm.
Table 1 LPCVD grown silicon nitride technological parameter
Reacting gas Gas flow Reaction velocity Chamber pressure Reaction chamber temperature
SiH 2Cl 2 29.2sccm 7nm/min 0.25Torr 800℃
NH 3 156sccm
2) photoetching, locating slot figure (as shown in Figure 1) is transferred on the silicon chip from mask, photoetching process comprises gluing, preceding baking, exposure, development, post bake and removes photoresist, after the photoetching, the silicon chip cross section is shown in Fig. 5 (1), with Beijing chemical reagent BP212 type photoresist make mask, viscosity is (37 ± 2) * 10 -3Pas, the thickness of photoresist is about 1~2 micron in experiment.
3) come the silicon nitride film of etching silicon chip surface with photoresist as mask layer, etching gas uses CF 4, form the mask that anisotropic wet corrodes silicon, as Fig. 5 (2), the reaction process parameter is as shown in table 2;
The parameter of table 2 reactive ion etching silicon nitride
Reacting gas Gas flow Base vacuum (Pa) Reaction chamber pressure Radio-frequency power Etch rate
CF 4 60sccm 2.0×10 -1 3.0Pa 150W 40nm/min
O 2 30sccm
4) working concentration is 40% KOH solution, and temperature is 70 ℃, and wet etching is made the autoregistration optical fiber duct, and shown in Fig. 5 (3), the width of optical fiber duct is 200 microns, and the angle of exposure and surface level is about 35.26 °
B: on (100) silicon chip of making optical fiber autoregistration V-type groove,, deposited the SiO of insulating effect successively by magnetically controlled sputter method 2Thin layer and the aluminum metal layer of doing electrode, concrete process conditions are as shown in table 3:
Table 3 splash-proofing sputtering process parameter
Sputtered layer Base vacuum Working gas Gas flow Operating air pressure Sputtering power Sputter rate
Silicon dioxide
2×10 -3Pa High-purity argon gas 60sccm 1.8×10 0Pa 200W 10nm/min
Aluminium
2×10 -3Pa High-purity argon gas 60sccm 1.8×10 0Pa 300W 30nm/min
The making of metal aluminium electrode: make electrode array configurations 7 as shown in Figure 2, mask is made in the corrosion of aluminium with photoresist, makes corrosive liquid with phosphoric acid, composition such as table 4.
The parameter of table 4 phosphoric acid corrosion aluminium
Solution Composition Temperature Corrosion rate
Phosphoric acid+water H 3PO 4 100ml DIH 2O 100ml 80℃ 50nm/s
C, utilization ICP dry etching technology, make and the perpendicular square type liquid crystal microflute of optical fiber autoregistration V-type groove, the width of microflute is 30 microns, utilize its conductive layer to disconnect fully with incident optical and outgoing optical fiber both sides, adopt simultaneously and carry out magnetically controlled sputter method in fiber end face and side and come deposit ITO transparent conductive film, make fiber end face and the side of putting into the V-type groove have electric conductivity, and link to each other with aluminium electrode that silicon substrate is made, on the silicon plane of incident optical and outgoing optical fiber both sides, draw lead, apply electric field thereby can finish attenuation performance for the polymer dispersion liquid crystal material in the square type liquid crystal microflute;
By result's contrast to the repetition test of incident optical and outgoing optical fiber deposition ITO transparent conductive film, as sputtering power 80W, when argon flow amount is 20sccm, can produce even aura, and the sputtered film homogeneous quality is better, the thickness of ito thin film is 80nm.Have good permeability at the ito thin film that makes under this sputtering condition under optical communication 1550nm wavelength, mean transmissivity is more than 80%, thereby the influence of device optical attenuation is dwindled.
D:
Our used liquid crystal material is the low molecular mixing liquid crystal E7 of biphenyl base system in a, the experiment, it is that four kinds of nematic liquid crystals mix in proportion and obtain, these four kinds of liquid crystal weight ratios are respectively 51% n-pentylcyanobiphenyl (5CB), 25% n-hyptylcyanobiphenyl (7CB), 16% n-octyloxyc yanobiphenyl (8CB), and 8% n-pentylcyanoterphenyl (5CT), its molecular structure is shown below respectively:
The Δ n=0.2246 of E7, n e=1.7462, n o=1.5216;
Liquid crystal material is provided by German Merck company:
Adopting polymer monomer in the experiment is the bisphenol-A epoxy acrylate, and its structural formula is as shown below:
Figure A20061001652200112
The monomer diluent of selecting for use is a methyl methacrylate, and methyl methacrylate has the effect of extraordinary reduction viscosity, and volatile grade is lower, and laser curing velocity is also than higher.The refractive index of methyl methacrylate is 1.4142, and structural formula is as shown below:
Figure A20061001652200113
Under the certain situation of light source, can light trigger polymerization take place to the PDLC system and polymerization speed plays decisive influence.We adopt the 1-hydroxycyclohexylphenylketone (Irgacure-184) that is provided by Jkchemical company as light trigger in this experiment, its optimal absorption scope 250-310nm, and molecular structural formula is as shown below:
B, in the darkroom, take by weighing liquid crystal, polymer monomer, an amount of thinning agent and light trigger, liquid crystal material content is 73% in the mixed solution, photoinitiator levels is 3.4%, polymer monomer and monomer diluent content are 23.6%, monomer and diluent materials ratio are 1: 1, heating under the shading condition, stir, ° it is under isotropic state, fully stir again and make its even mixing;
C, the composite material in the above-mentioned steps is injected under isotropic state in the T type liquid crystal groove, when it is cooled to 40~50 ℃, adopt the ultraviolet source of philips 300w, it is separated to carry out the UV-irradiation polymerisation induced, the 5 minutes time of light initiation polymerization, 40 ℃ of polymerization temperatures.
At liquid crystal content is 73%, and photoinitiator levels is 3.4%, and monomer and diluent materials ratio are 1: 1, solidification temperature prepares polymer dispersion liquid crystal material when being 40 ℃, the threshold voltage of material is less than 4V, and minimum light transmission rate is about 0.67%, and the working range of voltage is 2-35V.The material for preparing under this condition can be realized the extraordinary good electro-optical characteristic that is separated, has, and it is as shown in table 5 that experiment records data.
Table 5:73% liquid crystal, 3.4% light trigger, monomer are 1: 1 with the diluent materials ratio, the electro-optical characteristic under electric field action
Institute's making alive (V) 0 3.4 29.9 31.6 32.7 33.3 34.4 35.4 36.6
Light transmission rate (%) 0.67 0.69 76.3 78.2 79.07 81.24 83.61 85.34 87.2
The realization of E, attenuation function: pass through fiber adjusting mount, the optical fiber that end face and side are coated with the ITO conductive film is put into autoregistration optical fiber V type groove and is aimed at, utilize microscope and infrared thermoviewer that the coupling of device is observed, when reaching coupling when requiring, optical fiber is fixed on the silicon substrate with the ultraviolet glue solidification method; On electrode structure, draw lead and form drive electrode; With regard to having realized the polymer dispersion liquid crystal material on the optical transmission pathway is applied certain effect of electric field like this, the performance parameter of measurement is: attenuation range 14.68dB, insert loss 1.1dB, Polarization Dependent Loss 0.97dB.

Claims (7)

1, the MEMS liquid crystal light attenuator array is made up of the liquid crystal microflute (4) of monocrystalline substrate (10), incident optical and outgoing optical fiber coupling array (5), filled polymer dispersed liquid crystal material, it is characterized in that:
A) self aligned V-type groove array (1) is arranged on silicon substrate, be deposited with silicon dioxide layer (3) and conductive metal layer (2) on the silicon substrate (10) of V-type groove array (1) successively comprising, wherein silicon dioxide layer (3) plays the insulation buffer action, conductive metal layer (2) insulation between V-type groove array (1) disconnects, and forms driving electrode array;
B) be deposited with the ITO transparent conductive film in the end face and the side of incident optical and emergent light fibre array (5), incident optical and outgoing optical fiber (5) are placed in the self aligned V-type groove of the silicon substrate array (1), the conductive film of its end face and side links to each other with metal level (2) on being deposited on silicon substrate, disconnect with the metal level that incident optical links to each other with outgoing optical fiber, form the both positive and negative polarity electrode pair (7) of drive electrode;
C) on the light-path of incident optical that is coupled and outgoing optical fiber (5) formation, with be carved with square type liquid crystal microflute (4) on the silicon substrate of incident optical and outgoing optical fiber vertical direction, in square type liquid crystal microflute, be filled with the polymer dispersion liquid crystal material (5) for preparing, be coated with the incident optical of ITO transparent conductive film and the end face of outgoing optical fiber coupling array and be close to polymer dispersion liquid crystal material, thereby prepare the MEMS liquid crystal light attenuator array.
2, MEMS liquid crystal light attenuator array as claimed in claim 1, it is characterized in that: the polymer dispersion liquid crystal material of filling in the square type liquid crystal microflute (4) is by the potpourri of the liquid crystal material that accounts for general assembly (TW) 30%~90%, 5%~65% polymer monomer and proper amount of diluting, 1%~5% light trigger ultra-violet curing and forming after abundant stirring, and wherein the weight ratio of polymer monomer and thinning agent is 1: 5~5: 1.
3, MEMS liquid crystal light attenuator array as claimed in claim 2, it is characterized in that: the polymer dispersion liquid crystal material of filling in the square type liquid crystal microflute (4) is by the potpourri of the liquid crystal material that accounts for general assembly (TW) 50%~90%, 5%~45% polymer monomer and an amount of thinning agent, 1%~5% light trigger ultra-violet curing and forming after abundant stirring, and wherein the weight ratio of polymer monomer and thinning agent is 1: 3~3: 1.
4, MEMS liquid crystal light attenuator array as claimed in claim 3, it is characterized in that: the polymer dispersion liquid crystal material of filling in the square type liquid crystal microflute (4) is by the potpourri of the liquid crystal material that accounts for general assembly (TW) 65%~90%, 5%~30% polymer monomer and an amount of thinning agent, 1%~5% light trigger ultra-violet curing and forming after abundant stirring, and wherein the weight ratio of polymer monomer and thinning agent is 1: 2~2: 1.
5, as any one described MEMS liquid crystal light attenuator array of claim 2-4, it is characterized in that: liquid crystal material is the liquid crystal compound that contains aerobic base xenyl, cyclohexyl, phenyl, a dihydrobenzene or cyano-phenyl.
6, as any one described MEMS liquid crystal light attenuator array of claim 2-4, it is characterized in that: polymer monomer is epoxy acrylate or polyurethane acrylate, monomer diluent is a methyl acrylate, ethyl acrylate, butyl acrylate, acrylic acid 2-hydroxypropyl acrylate, acrylic acid 2-hydroxyl ethyl ester, acrylic acid methoxyl ethyl ester or methyl methacrylate, Jia Jibingxisuanyizhi, two propylene glycol diacrylates that contract, trimethylolpropane triacrylate, trimethylolpropane tris is basic acrylate early, 1,6-hexanediol diene acid esters or zinc methacrylate, the methacrylic acid acid amides.
7, the preparation method of the described MEMS liquid crystal light attenuator array of claim 1, its step is as follows:
The making of A, optical fiber autoregistration V-type groove: adopt body silicon Micrometer-Nanometer Processing Technology, utilize the crystallographic characteristics of silicon, on monocrystalline substrate (10), produce optical fiber autoregistration V-type groove (1) by photoetching, mask, etching and employing anisotropic wet corrosion technology;
The making of B, conductive electrode: making on the silicon substrate (10) of optical fiber autoregistration V-type groove (1) successively by magnetically controlled sputter method deposition SiO 2Insulation course (3) and metal level (2) use the method for acid corrosion that the metal level (2) between adjacent V-type groove (1) is disconnected, and produce multi-channel electrode array structure (7); Simultaneously come deposit ITO transparent conductive film by magnetron sputtering in the end face and the side of incident optical and emergent light fibre array (5), make fiber end face and the side of putting into V-type groove (1) have electric conductivity, and link to each other with electrode array configurations (7) that silicon substrate (10) go up to be made, on electrode array configurations (7), draw lead formation drive electrode;
The making of C, liquid crystal microflute: ICP is in the method lithographic technique in utilization, on silicon substrate, be positioned at incident optical and outgoing optical fiber joint, make and the perpendicular rectangle liquid crystal microflute (4) of optical fiber autoregistration V-type groove, the metal electrode of producing electrode array configurations (7) simultaneously is right, utilize microscope and infrared thermoviewer that the coupling of device is observed again, when reaching coupling when requiring, with the ultraviolet glue solidification method incident optical and emergent light fibre array (5) are fixed in the V-type groove array (1), liquid crystal light attenuation structure and its optical fiber self-alignment structure are become one;
D, with liquid crystal material, polymer monomer, an amount of monomer diluent and light trigger, Hybrid Heating to 60 under the shading condition~80 ℃, it is under isotropic state, make it evenly mix the mixed solution of preparation liquid crystal, light trigger and polymer monomer and thinning agent thereby fully stir again, it is polymer dispersion liquid crystal material, calculate with weight ratio in the mixed solution, liquid crystal material accounts for 30%~90%, prepolymer and monomer account for 5%~65%, wherein prepolymer is 1: 5~5: 1 with the ratio of monomer, and light trigger accounts for 1%~5%; Under 60~80 ℃ of conditions, be filled into mixed solution in the rectangle liquid crystal microflute (4), when it is cooled to 40~50 ℃, carry out UV-irradiation, polymerization reaction take place induces it to be separated, thereby aggregate into liquid crystal composite material, it is the mercury vapor lamp of 300~500nm that ultraviolet source adopts wavelength, and the time of light initiation polymerization is 1~10 minute.
CNB2006100165226A 2006-01-13 2006-01-13 MEMS liquid crystal light attenuator array and producing method thereof Expired - Fee Related CN100367082C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2006100165226A CN100367082C (en) 2006-01-13 2006-01-13 MEMS liquid crystal light attenuator array and producing method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2006100165226A CN100367082C (en) 2006-01-13 2006-01-13 MEMS liquid crystal light attenuator array and producing method thereof

Publications (2)

Publication Number Publication Date
CN1811528A true CN1811528A (en) 2006-08-02
CN100367082C CN100367082C (en) 2008-02-06

Family

ID=36844549

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB2006100165226A Expired - Fee Related CN100367082C (en) 2006-01-13 2006-01-13 MEMS liquid crystal light attenuator array and producing method thereof

Country Status (1)

Country Link
CN (1) CN100367082C (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012103663A1 (en) 2011-01-31 2012-08-09 Universidad De Chile In situ polymerisation process for obtaining an electro-optical apparatus, said polymer and electro-optical apparatus; and uses thereof
CN103197452A (en) * 2013-04-16 2013-07-10 浙江大学 Variable optical attenuator based on liquid crystal cladding polymer optical waveguide
CN101923243B (en) * 2009-04-27 2014-03-12 宝创有限公司 Polymeric dispersed liquid crystal light shutter device
CN104698668A (en) * 2015-03-30 2015-06-10 北京三五九投资有限公司 Nano conducting particle doped PDLC (polymer dispersed liquid crystal) membrane and preparation method thereof
CN105141332A (en) * 2015-09-16 2015-12-09 南京捷希科技有限公司 Pluggable radio frequency matrix
CN111879832A (en) * 2020-06-12 2020-11-03 宁波水表(集团)股份有限公司 Sensor for detecting residual chlorine in tap water and preparation method thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005189891A (en) * 1998-09-04 2005-07-14 Nippon Telegr & Teleph Corp <Ntt> Variable optical attenuator and method for manufacturing the same
CN1100843C (en) * 1999-12-07 2003-02-05 中国科学院广州化学研究所 Matrix structure controllable high polymer dispersed liquid crystal membrane and its preparing process
CN1232851C (en) * 2003-08-28 2005-12-21 上海交通大学 Adaptive microtype optical fibre connector

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101923243B (en) * 2009-04-27 2014-03-12 宝创有限公司 Polymeric dispersed liquid crystal light shutter device
WO2012103663A1 (en) 2011-01-31 2012-08-09 Universidad De Chile In situ polymerisation process for obtaining an electro-optical apparatus, said polymer and electro-optical apparatus; and uses thereof
CN103197452A (en) * 2013-04-16 2013-07-10 浙江大学 Variable optical attenuator based on liquid crystal cladding polymer optical waveguide
CN103197452B (en) * 2013-04-16 2015-08-05 浙江大学 A kind of adjustable optical attenuator based on liquid crystal clad polymer optical waveguide
CN104698668A (en) * 2015-03-30 2015-06-10 北京三五九投资有限公司 Nano conducting particle doped PDLC (polymer dispersed liquid crystal) membrane and preparation method thereof
CN104698668B (en) * 2015-03-30 2019-04-02 北京三五九投资有限公司 A kind of PDLC film and preparation method thereof for mixing nano conducting powders
CN105141332A (en) * 2015-09-16 2015-12-09 南京捷希科技有限公司 Pluggable radio frequency matrix
CN105141332B (en) * 2015-09-16 2017-08-22 南京捷希科技有限公司 A kind of pluggable radio frequency matrix
CN111879832A (en) * 2020-06-12 2020-11-03 宁波水表(集团)股份有限公司 Sensor for detecting residual chlorine in tap water and preparation method thereof

Also Published As

Publication number Publication date
CN100367082C (en) 2008-02-06

Similar Documents

Publication Publication Date Title
JP6332522B1 (en) Composition and method for producing the composition
CN100367082C (en) MEMS liquid crystal light attenuator array and producing method thereof
KR102112974B1 (en) Ink composition, film and display
CN110092875B (en) Preparation method of PDLC (polymer dispersed liquid crystal) film based on liquid crystal/polymer composite material system
CN110095896A (en) A kind of preparation method of the light modulation film based on Liquid Crystal/Polymer composite material
WO2018137262A1 (en) Display apparatus and preparation method therefor
Zhang et al. Fluorescence enhancement and encapsulation of quantum dots via a novel crosslinked vinyl-ether liquid crystals/polymer composite film
CN100368836C (en) Polymer dispersed liquid crystal optical attenuator array and its production method
CN111655818A (en) Composition, film, laminate structure, light-emitting device, and display
CN109917587B (en) Liquid crystal display device and manufacturing method thereof
CN108424537A (en) A kind of adjustable ultra-violet curing film of refractive index and preparation method thereof
CN105116665A (en) Method for realizing light amplification of optical waveguide device using up-conversion luminescent material
Zhu et al. Independent dispersed and highly water-oxygen environment stable FAPbBr3 QDs-polymer composite for down-conversion display films
Takei et al. Nanoparticle free polymer blends for light scattering films in liquid crystal displays
CN107817627A (en) SiO2The compound wide wave reflection film of aerogel/cholesteric liquid crystal and preparation method
KR20010047842A (en) Base coating composition for forming lcd reflector having diffusing properties
CN109188793B (en) Flexible three-dimensional electrode, preparation method thereof and liquid crystal display panel
TWI760591B (en) Composition, film, laminate structure, light emitting device and display
CN111690159A (en) Preparation method of liquid crystal/high-molecular full-polymerization quantum dot film based on vinyl ether
US9557609B2 (en) Method for manufacturing polymer dispersed liquid crystal (PDLC) panel
CN110066516A (en) A kind of preparation method of the composite package matrix for LED encapsulation
WO2022044759A1 (en) Composition containing semiconductor nanoparticles, color filter, and image display device
CN113025307B (en) Preparation method of quantum dot fluorescence enhancement film based on titanium dioxide/liquid crystal/polymer composite material
CN103881005B (en) A kind of photocuring preparation method of rare earth bonding type fluorescence gel glass
CN110308501B (en) Strong laser film and preparation method and application thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20080206

Termination date: 20110113