CN1271429A - Volume phase hologram and method for producing the same - Google Patents
Volume phase hologram and method for producing the same Download PDFInfo
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- CN1271429A CN1271429A CN98809312A CN98809312A CN1271429A CN 1271429 A CN1271429 A CN 1271429A CN 98809312 A CN98809312 A CN 98809312A CN 98809312 A CN98809312 A CN 98809312A CN 1271429 A CN1271429 A CN 1271429A
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Images
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
- G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0005—Production of optical devices or components in so far as characterised by the lithographic processes or materials used therefor
- G03F7/001—Phase modulating patterns, e.g. refractive index patterns
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/04—Chromates
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/40—Treatment after imagewise removal, e.g. baking
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
- G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
- G03H1/0272—Substrate bearing the hologram
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
- G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
- G03H1/024—Hologram nature or properties
- G03H1/0248—Volume holograms
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
- G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
- G03H2001/026—Recording materials or recording processes
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
- G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
- G03H2001/026—Recording materials or recording processes
- G03H2001/0264—Organic recording material
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H2270/00—Substrate bearing the hologram
- G03H2270/53—Recording material dispersed into porous substrate
Abstract
The hologram comprises: a porous transparent sileceous body having a plurality of mutually interconnected microcavities or pores, the mean radius of which is lower than the wavelength of the hologram recording light and the wavelength of the hologram reading light, a photolysis product of a photolysable material, said product being attached to walls of certain microcavities and being spatially distributed in accordance with the recorded interference pattern, and a solid transparent polymeric material filling said microcavities, said polymeric material exhibiting local variations of refractive index, said variations being spatially modulated in conformity with the recorded interference pattern, said photolysis product being a polymerization modifier for a composition polymerizable into said polymeric filling material.
Description
The present invention relates to holography, be specifically related to volume phase hologram.
The volume phase hologram of being made by the polymkeric substance of refractive index localized variation is well-known.Hologram is recorded in (referring to R.J.Collier, C.B.Burckhardt, L.H.Lin " optical holography method " 1971, Academic press, New York and London) on photosensitive polymer layer or the dichromated gelatin film.These recording materials are made by organic material usually, and the mechanical property of described organic material is low, poor heat stability, so reliability is low, poor durability.In addition, can not use thick photosensitive material layer, because it can limit the obtainable spectrum level of hologram and the angular selectivity of record.
The also known volume phase hologram of making by the photolytic product of high silicon materials matrix of porous and organic or inorganic photosensitive substrate, the spatial modulation of hologram refractive index be the photolytic product concentration by suitable modulation matrix structure or spatial variations photosensitive substrate realize (referring to V.Sukhanov, heterogeneous recording medium, In SPIE, 1989, V.1238, p.226-230. UNESCO is about the international symposium of the science of volume hologram method, culture, education, Ed.Tung H.Jeorg, 1989, Kiev, USSR).The physical thickness of this hologram is up to 103 microns.In addition, they have the very high feature of thermal stability, and have anti-shrinkability in practice.But this hologram has porous structure, can produce the height scattering in indigo plant-green light spectrum district.For preventing this scattering, can fill with filler by the hole of dip treating to hologram.But the refractive index of this filler is more near the refractive index of matrix, then the diffraction efficiency of this hologram just low more (referring to " the formation principles of hologram in the capillary compound substance " such as S.A.Kuchinskii, Laser Physics, 1993, V3, n6, p.1114-1123).Therefore, it can not take into account low scattering and good diffraction efficiency.
The objective of the invention is a kind of volume phase hologram, it has the hologram diffraction efficient that significantly improves, and can reduce the loss that scattering causes.For reaching this purpose, in matrix pores, insert the solid polymer of refractive index with spatial modulation, the cycle of described index modulation is identical with the refractive index spatial of the volume phase hologram distribution cycle, and the hole of the porous matrix of described hologram is filled with the identical organic filler of refractive index.
More particularly, the present invention relates to a kind of volume phase hologram, it is with the form record interference figure of refractive index localized variation, and it comprises:
-porous silicon-containing residuite, it has many interconnected micropores or hole, and the mean radius of hole reads light wavelength less than holographic recording light wavelength and holography;
But the photolytic product of-photodissociation material on the wall of described product attached to some micropore, and carries out space distribution according to the interference figure that is write down; And
One inserts the solid transparent polymeric material of described micropore, the refractive index localized variation that it is characterized in that described polymeric material, the spatial modulation of described variation conforms to the interference figure that is write down, and described photolytic product is the polymeric modifier that composition aggregates into described polymer filler.
The invention still further relates to the method for making hologram, it comprises the following steps:
A) provide a kind of porous silicon-containing residuite, it has many interconnected micropores or hole, and the mean radius of hole reads light wavelength less than holographic recording light wavelength and holography;
B) but with the wall of photodissociation coated materials described micropore, the photolytic product of this photodissociation material is the polymeric modifier of at least a predetermined polymerisable compound;
C) recording holographic interference figure in described material, make described photolytic product according to described pattern distribution on the wall of some described micropore;
D) but remove the photodissociation material that does not change;
E) in the residue space of described micropore, insert described at least a polymerisable composition; With
F) the described composition of polymerization, thus the volume phase hologram that obtains is made by the have living space residuite of solid polymeric material of refractive index of modulation of filling agent, and the index modulation cycle of described polymkeric substance is identical with the space distribution cycle of described photolytic product.
When term " polymeric modifier " refers to that this material exists, when the refractive index of the polymkeric substance that the polymerisable compound polymerization forms and this material do not exist, the different material of refractive index of the polymkeric substance that described polymerisable compound polymerization forms.
Can understand other advantage of the present invention and feature by describing below with accompanying drawing.In the accompanying drawing,
Fig. 1 is the synoptic diagram of volume phase hologram of the present invention;
Fig. 2 is the curve of the grating efficiency (grating power) of diffraction efficiency and transmission hologram photo, is used to illustrate the present invention.
Hologram shown in Figure 1 is made up of the high silicon matrix 1 of porous, and it comprises hole or the micropore of many mean radiuss less than visible wavelength (promptly less than about 0.4 micron).It is n that the wall of some micropore is coated with refractive index
cBut, comprise the coating 2 of the photolytic product of photodissociation material, and be positioned near maximum or the minimum interference figure that is write down.The residual volume of hole is filled with the filler 3 of the refractive index with spatial modulation, and the refractive index of this filler is n in uncoated hole
f, be n in the refractive index of other this filler of hole
f+ Δ.
Can see easily that the difference of the effective refractive index between exposure region in the hologram volume (A) and unexposed area (B) can be represented by the formula:
n
A-n
B=Ff (n
c-n
f)+F (1-f) Δ (1) wherein, the relative void content of F=;
First description in the relative positive displacement (1) of f=hole floating coat is with the amplitude modulation(PAM) of the porous holographic photo of same filler, if n
fEqual n
c, then this is 0.If but the refractive index of filler is carried out spatial modulation, even at n
f=n
cSituation under, this amplitude also is not equal to 0, but equals F (1-f) Δ.Under the situation of the filler of spatial modulation, the variations in refractive index amplitude of hologram than the high K of variations in refractive index amplitude under the situation of identical filler (Δ=0) doubly, K is defined as:
In addition, even for n
c-n
fReach the hologram (promptly not being with filler) of its peaked originally " doing ",, also can obtain grating and amplify by the filler of spatial modulation being added the residual volume of porous holographic photo.By formula (1) as seen, amplification coefficient is in this case determined by following formula:
By formula (2) and formula (3) as seen, under the situation of the variations in refractive index homophase of the index modulation of filler and unfilled hologram and under the anti-phase situation of the modulation of same parameter, the holographic amplification can be taken place all.Only require described modulation to be characterised in that the space periodic of modulation is identical with the space periodic of the interference figure that is write down, and require the absolute value that obtains by formula (2) and formula (3) | k|, | k ' | greater than 1.Knownly equaling corresponding to grating efficiency (x):
During this concrete holographic refractive index amplitude modulation(PAM) value, the diffraction efficiency of transmission hologram photo reaches its maximal value.
Obviously the χ value is improved k doubly, this means that in practice exposure need be reduced k times (but the response of the photodissociation material of supposition hologram is linear) obtains η=100%.
Therefore, the present invention can obtain the efficient phase hologram photo of low scattering degree by the refractive index of spatial modulation filler.
But the realization of described holographic amplification method is based on when the photolytic product of photodissociation material during as the polymeric modifier of described method, the difference of monomer filler between the polymerization mechanism of the exposure region of hologram and unexposed area.As a result, distribute according to the optical density that is write down, thereby the density of polymer filler and refractive index thereof are subjected to spatial modulation.The porous silicon-containing residuite can be that the fritted glass that forms of for example borosilicate glass lixiviate is (referring to V.I.Sukhanov. " fritted glass is as storage medium " Optica Applicata, 1994, v.24, n.1-2, pp.13-26), the fritted glass that makes with so-called sol-gel process (referring to: V.I.Sulhanov etc. " porous sol-gel derived bioglass; a kind of recording medium of holograph ", the preface speech of the 8th glass that international gel is made and ceramic symposial, 1995, Faro, Portugal, September 18-22, p331).
In both cases, this porous matrix contains interconnected micropore or hole, and its mean radius is significantly less than the wavelength of work light (be recording light and read light), and has high surface area.This structure guarantees that on the one hand light scattering is relatively low, can flood described light degradable material effectively on the other hand, and the result can apply the wall of described microporosity well with described photodissociation material.
But the present invention is used for the photodissociation material of hologram record can be that for example but its photolytic product can obviously cause the photodissociation material of complicated free radical polymerization.
But the illustrative example of suitable photodissociation material is the inorganic salts of some transition metal, as (NH
4)
2Cr
2O
7, Na
2Cr
2O
7, K
2Cr
2O
7With the organometallics of some transition metal, as Mn
2(CO)
10, Cr (CO)
6, Co
2(CO)
8, Mo (CO)
6Or the dichloride bicyclopentadiene closes titanium, referring to N.F.Borelly and D.L.Morse " fritted glass of photosensitive dipping " Appl.Phys.Lett.1983, v.43, n.pp.992-993; " light sensitive metal-organic system: mechanical principle and purposes " Ed.Ch.Kutal, N.Serpone.Advances inChemistry, Ser.238,1994, Am.Chem.Soc., Washington, DC 449p..
But available simple method is immersed in porous matrix in the solution bath of photodissociation material, and subsequent drying applies.If necessary, vacuum-pumping is to help dipping.
The photodissociation that is noted that transition metal salt has been used to holographic recording, especially the photodissociation of Cr (VI) salt (referring to: G.Manivannan etc. " main optics processing " polyvinyl alcohol (PVA) of dichromic acid salinization " J.Phys.Chem. of Cr (VI) in the real-time holography record; 1993; v.97; pp.7228-7233 n.28). at the exposure region of hologram, Cr (VI) ion is reduced into Cr (III) ion.
After photodissociation takes place in light degradable transistion metal compound in porous silicon-containing matrix in the holographic recording step, the functional group that contains own existence on the silicon face of its photolytic product and micro-pore wall (as-the SiOH group) react, form complex molecule coating with porous matrix wall chemical bonding.
Perhaps, as N.F.Borelly etc. at " in glass, making waveguide " IEEE.J.OfQuantum Electronics.1986 with photochemical method, v.QE-22, n.6, described in the pp896-901, can use the coating of the transition-containing metal ion of the organometallics manufacturing of transition metal and fritted glass wall chemical bonding.
Also can apply the photoresist layer that contains transistion metal compound on the described porous wall and forming coating on the wall in described hole, be used to replace making the pore wall direct chemical bonding of transition metal ion and fritted glass.In this case, photoresist layer takes place crosslinkedly after illumination, and the result forms the coating of transition-containing metal ion on pore wall.Can use photoresist layer based on synthetic polymer, especially polyvinyl alcohol (PVA) is (referring to: G.Manivanna etc. " the main optics processing of Cr (VI) in the real-time holography record: the polyvinyl alcohol (PVA) of dichromic acid salinization " J.Phys.Chem., 1993, v.97, pp.7228-7233 n.28).Also can use photoresist layer, especially gelatin or shellac based on the natural polymerization product.
Can use visible range laser to carry out holographic recording in the mode of routine.Only require the amount of the photolytic product that irradiation energy produces be enough to make this photolytic product in step (f) as effective polymeric modifier, and between the irradiated region of matrix and non-irradiated region, produce refractive index difference.
Can after step (c), remove the light degradable material that does not change by washing.
Can with described matrix impregnation in the lean solution of described polymerisable compound, this polymerisable compound be inserted in the residual volume of micropore, can use conventional method to carry out described polymerization, for example, can in autoclave, heat the matrix that is impregnated with polymerisable compound.
The transition metal ion of quovis modo (as Cr (III) ion), their all polymerizations of the composition of modification free redical polymerization by influencing stereoselectivity.
As a result, the packing density of the polymer chain that forms in this polymerization process is different with the packing density of the polymer chain that common radical polymerization process (not having described ion) forms, thereby obtains the polymkeric substance of different refractivity.
The illustrative example that is applicable to polymerizable compositions of the present invention has the polymerisable compound based on many alcohol (allyl carbonate), as commodity CR-39 by name
Diglycol two (allyl carbonate), but and with the potpourri of the monomer of copolymerization (as vinyl acetate or have the oligourethane of dimethylacrylate end group); (methyl) alkyl acrylate is as methyl methacrylate (MMA); The monomer that contains vinyl, as vinyl acetate (VA), but the potpourri of the monomer of styrene and styrene and copolymerization (as MMA, VA or vinyl cyanide).Except monomer, these compositions also comprise radical initiator usually, as superoxide or azo-compound.
With embodiment the possibility that the inventive method realizes is described below.
In experimentation, the diffraction efficiency of hologram (η) is to measure in the different step of making the fritted glass hologram.Measure (η for first group
Em) carry out in exposure with after developing, in the residual volume of hologram, have air.Measure (η for second group
Rf) corresponding to the hologram that is filled with liquid filler, the refractive index of described liquid filler equals the refractive index of polymer filler, it will be used for the manufacturing of the 3rd step holograph.Measure (η for the 3rd group
Mf) after polymerization is finished, carry out.The amplification coefficient of holograph is defined as:
With
This coefficient obtains according to the data computation that experiment obtains.
Fig. 2 represents the relation of diffraction efficiency and grating efficiency (χ): round dot () is corresponding to the hologram that has poly-diglycol two allyl carbonates (PCR-39) filler, and square () is corresponding to the hologram that has polymethylmethacrylate (PMMA) filler.K in maximum
1And k
2Being worth these data conforms to experiment.
Table 1 has been listed the amplification coefficient under two kinds of situations.By table as seen, with respect to same hologram of the liquid filler that has same refractive index, the polymer filler of usage space refraction index modulation can obtain 5-70 amplification coefficient k doubly
2Should note filling hologram,, fill the amplification coefficient k of the hologram of PCR-39 filler with respect to same the hologram of filling air with the polymer filler of spatial modulation
1Be about 2.0, fill the k of the photo of PMMA filler
1Be 4.5.
The listed data of table 1 also show k
1And k
2But value and the kind of porous matrix and the cation type (Na in the photodissociation material
+Or NH
+ 4) irrelevant substantially.In addition, under the situation of PMMA filler, K
1And K
2Value increases with the minimizing of exposure.Therefore the present invention's method of making hologram can significantly increase the light sensitivity of hologram recording medium.
In addition, after polymer filler filling hologram, the scattering degree obviously descends.Therefore, penetrability τ=0.75 of packless hologram when λ=488nm, but after inserting polymkeric substance in the hologram volume, τ increases to 0.90.
1. use diameter 40mm, the discoid porous high silica glass of thick 1.5mm (average pore radius is about the 60-70 dust, and the volume fraction in hole is about 30+1%) (1 type glass in the table 1).This glass is to obtain with the borosilicate glass that acidleach puts the percentage composition of column weight amount: SiO
2-61.12%, B
2O
3-28.03%, Na
2O-7.65%, Al
2O
3-3.17%.
2. with the (NH of 1.25 weight %
4)
2Cr
2O
7Aqueous solution is flooded this fritted glass and is strengthened its light sensitivity, the many 5-6 of volume ratio fritted glass volume of ammonium dichromate solution doubly, 20 ℃ of dippings to the fritted glass of dipping till the optical density of the optical wavelength of 488nm reaches 0.25-0.30.This fritted glass of air drying at room temperature is immersed in the aqueous isopropanol with the filling pore volume, prevents that steam from damaging this glass.
3. adopt argon laser (488nm) with the angle recordings transmission hologram photo between 9.2 ° of record bundles.Irradiation energy is 0.5J/cm
2Behind the record, to remove isopropyl alcohol, it was washed 15 hours with distilled water at 20 ℃ subsequently, again 70 ℃ of washings 30 minutes at this porous matrix of air drying.Then, anhydrate from matrix, to remove at air drying; Drying is 4 hours in 120 ℃ baking oven.
4. measure this dry porous matrix (η with λ=633nm (He-Ne laser)
Em) and be filled with the not filler of polymerizable (o-xylene) (η
Rm) the diffraction efficiency (η) of hologram.
The grating efficiency of hologram (χ) is following to be calculated:
The relation of diffraction efficiency and grating efficiency is shown in Fig. 2, χ
EmAnd χ
RfValue is listed in table 1.After the measurement, in vacuum (10
-2MmHg) descend dry this matrix in room temperature (3 hours) and 100 ℃ (3 hours) in.
5. with following method polymer filler is inserted in the porous holographic photo:
Soak the matrix that records hologram of this drying with methyl methacrylate (MMA) solution of the radical polymerization initiator (azoisobutyronitrile) of 2 weight % in room temperature.
Make special equipment to carry out polymerization.This equipment comprises two silicate glass disks, and this disk has the working face of the horizontal parallel on band optical quality surface, is wound with cellophane film (3-4 layer) in the periphery on plane.Anticipate the working surface of disk with dichlorodimethylsilane, with the viscosity of the silicate surfaces that reduces polymkeric substance and equipment.The dipping matrix that records hologram is put into this equipment.Pour extra initiating agent-monomer (MMA) solution in this equipment into, made matrix be immersed in fully in this solution.This equipment is put into autoclave, and apply 8 atmospheric inert gas (Ar or N
2) pressure.
In the liquid automatic temperature-regulator, heat reactor according to following temperature order, so that carry out polymerization:
Placed 24 hours at 0 ℃;
With 10 ℃/hour speed temperature is risen to 100 ℃;
Placed 2.0 hours at 100 ℃; And
Speed with 10 ℃/hour reduces to room temperature with temperature.
After the pressure of autoclave reduced to atmospheric pressure, open autoclave, from described equipment, take out matrix.
6. measure the diffraction efficiency (η of the matrix of filled polymer
Mf), calculate χ
MfValue (is seen step 4), is calculated amplification coefficient (K by formula (4)
1, K
2), the results are shown in table 1.
Repeat the step 1-6 of embodiment 1, but the irradiation energy that is used for the recording holographic photo is 3J/cm
2
All experimental datas are all listed in table 1.
Repeat the step 1-6 of embodiment 1, still:
-the irradiation energy that is used for the recording holographic photo is 3J/cm
2(step 3).
-use CR-39 (monomer) solution of 2 weight % initiating agents (peroxidating benzoic acid) to soak fritted glass, and be used for forming polymer filler (step 5) in void content.In the liquid automatic temperature-regulator, heat reactor according to following temperature order, so that carry out polymerization:
Placed 24 hours at 60 ℃;
Placed 65 hours at 80 ℃;
With 10 ℃/hour speed temperature is risen to 100 ℃;
Placed 1.5 hours at 100 ℃; And
Speed with 10 ℃/hour reduces to room temperature with temperature.
All experimental datas are all listed in Fig. 2 and table 1.
Embodiment 4
Repeat the step 1-6 of embodiment 1, still:
-(average pore radius is about the 40-50 dust to use the porous high silica glass; The about 26+1% of the volume fraction of hole) (the II type glass in the table 1).It is to carry the borosilicate glass with following percentage composition with acidleach to obtain: SiO
2-67.5%; B
2O
3-24.6%; Na
2O-7.9%; Al
2O
3-0.5% (step 1).
-fritted glass is immersed the Na of 10 weight %
2Cr
2O
7Aqueous solution in the light sensitivity (step 2) of reinforcing glass.
All experimental datas are all listed in table 1.
Table 1
| Embodiment | Fritted glass | Photoactive substance | Irradiation energy (J/cm 2) | Polymer filler | Grating efficiency (χ) | Amplification coefficient | |||
| ????χ cm | ?????χ rf | ?????χ mf | ??K 1＝χ mf/χ cm | ????K 2＝χ mf/χ rf | |||||
| Embodiment 1 | The I type | ???(NH 4) 2Cr 2O 7 | ????0.5 | ??PMMA | ????0.275π | ????0.015π | ?????1.05π | ?????3.8 | ????70 |
| Embodiment 2 | The I type | ???(NH 4) 2Cr 2O 7 | ????3.0 | ??PMMA | ????0.9π | ????0.07π | ?????2.65π | ?????2.9 | ????37 |
| Embodiment 3 | The I type | ???(NH 4) 2Cr 2O 7 | ????3.0 | ??PCR-39 | ????0.36π | ????0.125π | ?????0.65π | ?????1.8 | ????5.2 |
| Embodiment 4 | The II type | ???Na 2Cr 2O 7 | ????0.5 | ??PMMA | ????0.275π | ????0.02π | ?????1.245π | ?????4.5 | ????62 |
Claims (21)
1. volume phase hologram, it is with the form record interference figure of refractive index localized variation, and it comprises:
One porous silicon-containing residuite, it has many interconnected micropores or hole, and the mean radius of hole reads light wavelength less than holographic recording light wavelength and holography;
But the photolytic product of a photodissociation material on the wall of described product attached to some micropore, and carries out space distribution according to the interference figure that is write down;
One inserts the solid transparent polymeric material of described micropore, the refractive index localized variation that it is characterized in that described polymeric material, the spatial modulation of described variation conforms to the interference figure that is write down, and described photolytic product is the polymeric modifier that composition aggregates into described polymer filler.
2. hologram as claimed in claim 1 is characterized in that described polymeric material is many alcohol (allyl carbonate) polymer of monomers or multipolymer.
3. hologram as claimed in claim 2 is characterized in that described many alcohol (allyl carbonate) monomers are diglycol two allyl carbonates.
4. hologram as claimed in claim 1 is characterized in that described polymeric material is the polymkeric substance of at least a alkyl acrylate.
5. hologram as claimed in claim 1 is characterized in that described polymeric material is at least a polymer of vinyl monomer or multipolymer.
6. hologram as claimed in claim 2, it is characterized in that described polymeric material be many alcohol (allyl carbonates) but the multipolymer of monomer and at least a other copolymeric material, but described copolymeric material mainly is selected from vinyl acetate and has the oligourethane of dimethylacrylate end group.
7. hologram as claimed in claim 1 is characterized in that described polymeric material is the multipolymer of styrene and at least a other copolymerisable monomer, and described copolymerisable monomer mainly is selected from methyl methacrylate, vinyl acetate and vinyl cyanide.
8. as any one described hologram among the claim 1-7, it is characterized in that described porous matrix is to make with the porous high silica glass that acid etching phase-splitting glass forms.
9. as any one described hologram among the claim 1-7, it is characterized in that described porous matrix is to be formed by the fritted glass that sol-gel process is made.
10. as any one described hologram among the claim 1-9, it is characterized in that described polymeric modifier comprises transition metal ion.
1. as any one described hologram among the claim 1-10, it is characterized in that described polymeric modifier is the product of light degradable organometallics.
12. hologram as claimed in claim 11 is characterized in that described organometallics is selected from Mn
2(CO)
10, Co
2(CO
8), Cr (CO)
6, Mo (CO)
6Or the dichloride bicyclopentadiene closes titanium.
13., it is characterized in that described polymeric modifier is Cr as any one described hologram among the claim 1-10
VIThe photolytic product of salt.
14. hologram as claimed in claim 13 is characterized in that described Cr
VISalt mainly is selected from (NH
4)
2Cr
2O
7, Na
2Cr
2O
7And K
2Cr
2O
7
15., it is characterized in that described polymeric modifier is attached directly on the micro-pore wall of described matrix as any one described hologram among the claim 1-14.
16., it is characterized in that described polymeric modifier is included in the coating that is coated on the described matrix micropores wall as any one described hologram among the claim 1-14.
17. hologram as claimed in claim 16 is characterized in that described coating comprises photoresist.
18. hologram as claimed in claim 17 is characterized in that described photoresist made by gelatin, described polymeric modifier is Cr
IIIIon.
19. hologram as claimed in claim 17 is characterized in that described photoresist made by polyvinyl alcohol (PVA).
20. hologram as claimed in claim 17 is characterized in that described photoresist made by shellac.
21. an optical device, it contains light source and at least a optical element, it is characterized in that described at least a optical element is any one described hologram among the claim 1-21.
22. the manufacture method as the described hologram of any one claim of front, it comprises the following steps:
A) provide a kind of porous silicon-containing residuite, it has many interconnected micropores or hole, and the mean radius of hole reads light wavelength less than holographic recording light wavelength and holography;
B) but with the wall of photodissociation coated materials described micropore, the photolytic product of this photodissociation material is the polymeric modifier of at least a predetermined polymerisable compound;
C) recording holographic interference figure in described material, make described photolytic product according to described pattern distribution on the wall of some described micropore;
D) but remove the photodissociation material that does not change;
E) in the residual volume of described micropore, insert described at least a polymerisable composition; With
F) the described composition of polymerization, thus the volume phase hologram that obtains is made by the have living space residuite of solid polymeric material of refractive index of modulation of filling agent, and the index modulation cycle of described polymkeric substance is identical with the space distribution cycle of described photolytic product.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU97115684 | 1997-09-19 | ||
| RU97115684/28A RU2168707C2 (en) | 1997-09-19 | 1997-09-19 | Volume phase hologram and process of its generation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1271429A true CN1271429A (en) | 2000-10-25 |
Family
ID=20197327
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98809312A Pending CN1271429A (en) | 1997-09-19 | 1998-09-10 | Volume phase hologram and method for producing the same |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP1023643A4 (en) |
| JP (1) | JP2001517812A (en) |
| KR (1) | KR20010024157A (en) |
| CN (1) | CN1271429A (en) |
| RU (1) | RU2168707C2 (en) |
| WO (1) | WO1999015939A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2002116488A (en) | 2002-06-18 | 2004-01-27 | Корнинг Инкорпорейтед (US) | Volumetric phase hologram and method of its creation |
| RU2378673C1 (en) | 2008-04-03 | 2010-01-10 | Владимир Исфандеярович Аджалов | Image visualisation method and device to this end |
Family Cites Families (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2315328A (en) * | 1938-11-04 | 1943-03-30 | Corning Glass Works | High silica glass article |
| US3860429A (en) * | 1973-03-16 | 1975-01-14 | Ici America Inc | Photopolymerization of ethylenically unsaturated organic compounds |
| US4187111A (en) * | 1977-05-31 | 1980-02-05 | Bell Telephone Laboratories, Incorporated | Sensitized porous bodies useful for producing thick refractive index recordings |
| US4173475A (en) * | 1977-05-31 | 1979-11-06 | Bell Telephone Laboratories, Incorporated | Latent image thick refractive index recordings |
| US4403031A (en) * | 1981-06-25 | 1983-09-06 | Corning Glass Works | Method for providing optical patterns in glass |
| US4488864A (en) * | 1983-08-04 | 1984-12-18 | Corning Glass Works | Integral optical device and method of making it |
| JPH0690589B2 (en) * | 1984-12-14 | 1994-11-14 | ソニー株式会社 | Hologram recording medium |
| GB2174692B (en) * | 1985-04-04 | 1989-06-28 | Canon Kk | Method for forming optical pattern |
| US4778744A (en) * | 1986-11-21 | 1988-10-18 | Corning Glass Works | Method for providing high-intensity optical patterns in glass |
| US4970129A (en) * | 1986-12-19 | 1990-11-13 | Polaroid Corporation | Holograms |
| GB8815966D0 (en) * | 1988-07-05 | 1988-08-10 | Marconi Gec Ltd | Optical elements |
| US5213915A (en) * | 1989-05-19 | 1993-05-25 | Agency Of Industrial Science & Technology, Ministry Of International Trade & Industry | Holographic recording material and method for holographic recording |
| EP0409396B1 (en) * | 1989-06-05 | 1995-09-06 | Nippon Sheet Glass Co. Ltd. | Process for producing light control plate having light-scattering pervious region |
| US5196282A (en) * | 1990-07-16 | 1993-03-23 | Hughes Aircraft Company | Glassy oxide network passivation of dichromated gelatin holograms |
| US5627217A (en) * | 1993-06-29 | 1997-05-06 | Minnesota Mining And Manufacturing Company | Interfacial polymerization in a porous substrate and substrates functionalized with photochemical groups |
-
1997
- 1997-09-19 RU RU97115684/28A patent/RU2168707C2/en active
-
1998
- 1998-09-10 JP JP2000513176A patent/JP2001517812A/en not_active Withdrawn
- 1998-09-10 EP EP98946901A patent/EP1023643A4/en not_active Withdrawn
- 1998-09-10 WO PCT/US1998/018778 patent/WO1999015939A1/en not_active Application Discontinuation
- 1998-09-10 CN CN98809312A patent/CN1271429A/en active Pending
- 1998-09-10 KR KR1020007002924A patent/KR20010024157A/en not_active Application Discontinuation
Also Published As
| Publication number | Publication date |
|---|---|
| RU2168707C2 (en) | 2001-06-10 |
| EP1023643A4 (en) | 2003-06-11 |
| KR20010024157A (en) | 2001-03-26 |
| EP1023643A1 (en) | 2000-08-02 |
| JP2001517812A (en) | 2001-10-09 |
| WO1999015939A1 (en) | 1999-04-01 |
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