CN101186446B - Method for preparing photosensitive germanium dioxide base organic-inorganic composite material - Google Patents
Method for preparing photosensitive germanium dioxide base organic-inorganic composite material Download PDFInfo
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- CN101186446B CN101186446B CN2007100190788A CN200710019078A CN101186446B CN 101186446 B CN101186446 B CN 101186446B CN 2007100190788 A CN2007100190788 A CN 2007100190788A CN 200710019078 A CN200710019078 A CN 200710019078A CN 101186446 B CN101186446 B CN 101186446B
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Abstract
The invention relates to a preparation method of organic-inorganic composite material of germanium dioxide, and is low temperature organic-inorganic composite photosensitive material by employing germanium dioxide as inorganic matrix, and modification silicate (containing photosensitive group) as organic matrix, which produces the organic- inorganic composite photoelectron material with dual properties of photosensitive and optical waveguide through the organic photosensitive function group. The invention, by adopting the technique of improving sol-gel process combining the low-temperature synthesis process, has the advantages of low synthesis temperature and simple technique requirement and good repeatability, and so on. The invention can produce low cost optical waveguide devices and other micro optical devices by making use of the uv photosensitive characteristic of the materials and combining mask technology and other laser techniques. More particularly, by utilizing the monolayer optical-quality waveguide film which is only a plurality of microns and has an adjustable refractive index and uv photosensitive characteristic, the micro-nano integrated optoelectronic devices and bulk production can be easily realized.
Description
Technical field
The present invention relates to a kind of preparation method of germanium dioxide base organic-inorganic composite material, be specifically related to a kind of preparation method of germanium dioxide base organic-inorganic composite material of light sensitive characteristic.
Technical background
In recent years based on the organic modified silicate based composites in the application aspect the integrated optoelectronics, caused that in the world scientists pays close attention to greatly.Particularly the so-gel integrated optics based on organic modified silicate is just demonstrating potential photoelectronics application prospect.Compare with the unorganic glass substrate material, composite organic-inorganic material not only can improve physics, chemistry and the mechanical characteristics of material along with the adding of organic group, but also can improve the structure of inorganic matrix, make that isomerization has bigger space to the organic photosensitive molecular radical.For example contain the polymerisable hydrocarbon polymer that is not full of or the epoxy material of comprising and the composite organic-inorganic material of organic group such as substitute by extensive studies and exploitation, because this class matrix material can write technology, laser holography or electron beam lithography etc. in conjunction with mask technique, laser according to the light sensitive characteristic of its UV-light, directly carry out develop then and fall the making that is not realized fiber waveguide device and micro-optic device by illumination (not polymerization) zone.This shows,, can save etching process necessary in the inorganic materials, thereby can reduce the element manufacturing cost greatly and carry out simple and batch making based on the optical device making processes of such photosensitive matrix material.So up to the present, be widely used in waveguide and micro-optic device, comprised that silicon-dioxide, zirconium dioxide, the photosensitive matrix material of titanium dioxide base organic-inorganic are in the news and study based on the compound photochromics of low temperature organic and inorganic of sol-gel technique.
On the other hand, consider that the germanium silex glass has high light transmission in visible and near-infrared region, be widely used as to be the fiber cores material.This shows that germanium dioxide-organic modified silicate composite material will have huge potential application as the matrix material that matrix adds the organic photosensitive group for photonics and integrated optics, because it not only has good compatibility with single-mode fiber, and with silicon-dioxide as substrate and germanium dioxide as the optical waveguides of the adulterated material of core, will have the characteristic that is equal to single-mode fiber in itself.Like this in conjunction with the light sensitive characteristic and the laser mask technology of organic group, thereby this matrix material is expected to carry out the making of low-cost and simple micro-nano opto-electronic device in batches, this has huge potential application to integrated optoelectronics.So in conjunction with improved sol-gel technique and low temperature organic and inorganic compounding technology realize its research with good light guide properties and UV photosensitive characteristic compound photochromics of germanium dioxide base organic-inorganic for the development of photonics and integrated optics with significant.
Summary of the invention
The object of the present invention is to provide that a kind of synthesis temperature is low, processing requirement is simple and the preparation method of the light sensitive characteristic germanium dioxide base organic-inorganic composite material of good reproducibility.
For achieving the above object, the present invention adopts technical scheme to be: 1) at first by 1: 4 mol ratio Virahol germanium and 2-methyl cellosolve are mixed and stir as solution A; By 1: 3: 3 mol ratio with 3-(Trimethoxy silane base) propyl methyl acid esters, Virahol and the hydrolysis of deionized water mixing and stirring after as solution B; By 1: 4: 4 mol ratio Union carbide A-162, ethanol and deionized water are mixed, then in mixed solution by Union carbide A-162: hydrochloric acid is that 100: 1 mol ratio adds hydrochloric acid and stirs afterwards as solution C as catalyzer;
2) then the solution A of 20-40 molfraction, the solution B of 30-60 molfraction and the solution C of 0-40 molfraction are mixed stirring at room temperature, evenly contained the low temperature organic-inorganic composite ground mass mother liquor of SiGe;
3) two (2,4, the 6-trimethylbenzoyl) the phenyl phosphine oxide light triggers with organic-inorganic composite ground mass mother liquor gross weight 3.0-4.5% join in the organic-inorganic composite ground mass mother liquor, and stir under darkroom and room temperature and obtain suspension liquid;
4) utilize spin coating technology under the situation that rotating speed changes for per minute 2500-4000, the above-mentioned suspension liquid that obtains to be deposited on the glass substrate, to deposit good film sample then and be placed under the 80-120 ℃ of temperature and handled 10-20 minute, can obtain the germanium dioxide base organic-inorganic composite material of light sensitive characteristic.
The present invention adopts and improves that sol-gel technique has in conjunction with the preparation of low temperature organic and inorganic synthetic technology that synthesis temperature is low, processing requirement simple and advantage such as good reproducibility.The present invention is the compound photochromics of low temperature organic and inorganic of organic substrate with germanium dioxide as inorganic matrix and organic modified silicate (containing photosensitive group), by having light sensitive characteristic light harvesting guide properties organic and inorganic complex light electronics material simultaneously based on its organic photosensitive functional group with realization.UV photosensitive characteristic by such low-temperature composite material can be carried out the making of fiber waveguide device cheaply or other micro-optic device in conjunction with mask technique or other laser technology simultaneously.Particularly can be in harmonious proportion the single layer optical quality waveguide film of UV photosensitive characteristic based on having several micron thickness, specific refractory power at low temperatures, so be beneficial to very much the integrated and batch making of realizing the micro-nano opto-electronic device, and the integrated of opto-electronic device will be the important trend of photoelectron development undoubtedly.
Description of drawings
The Fourier transform infrared spectroscopy graphic representation of the compound photochromics of germanium dioxide base organic-inorganic that obtains under Fig. 1 different heat treatment temperature, wherein X-coordinate is wave number (cm
-1), ordinate zou is a specific absorption;
Fig. 2 is based on the ridge optical waveguide array (a) that laminated film substrate material UV photosensitive characteristic that preparation method of the present invention obtains is made: two dimensional image; (b): the ridge waveguide height and the width distribution of WYKO interferometer measurement, wherein X-coordinate is a distance (micron) between the waveguide, ordinate zou is duct height (micron);
The ridge optical waveguide (a) that Fig. 3 makes based on the laminated film substrate material light sensitive characteristic that preparation method of the present invention obtains: 3-D view; (b): the corresponding figures a duct height and the width distribution of WYKO interferometer measurement, X-coordinate duct width (micron) wherein, ordinate zou is duct height (micron);
The ridge optical waveguide that the laminated film substrate material light sensitive characteristic that Fig. 4 obtains based on preparation method of the present invention is made and Fig. 3 are than the result with longer time shutter (a): 3-D view; (b): the ridge waveguide height and the width distribution of WYKO interferometer measurement, X-coordinate duct width (micron) wherein, ordinate zou is duct height (micron).
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1: at first by 1: 4 mol ratio Virahol germanium and 2-methyl cellosolve are mixed and stir as solution A; By 1: 3: 3 mol ratio with 3-(Trimethoxy silane base) propyl methyl acid esters, Virahol and the hydrolysis of deionized water mixing and stirring after as solution B; By 1: 4: 4 mol ratio Union carbide A-162, ethanol and deionized water are mixed, then in mixed solution by Union carbide A-162: hydrochloric acid be 100: 1 mole add hydrochloric acid stir as catalyzer after as solution C;
Then the solution A of 20 molfractions, the solution B of 40 molfractions and the solution C of 40 molfractions are mixed stirring at room temperature, evenly contained the low temperature organic-inorganic composite ground mass mother liquor of SiGe;
Two (2,4, the 6-trimethylbenzoyl) phenyl phosphine oxide light triggers of organic-inorganic composite ground mass mother liquor gross weight 3% are joined in the organic-inorganic composite ground mass mother liquor, and under darkroom and room temperature, stir and obtain suspension liquid;
Utilize spin coating technology under the situation that rotating speed changes for per minute 2500, the above-mentioned suspension liquid that obtains to be deposited on the glass substrate, to deposit good film sample then is placed under 80 ℃ of temperature and handled 10 minutes, can obtain individual layer and have about 2 micron thickness, and smooth surface is smooth and have a germanium dioxide base organic-inorganic composite film material of UV photosensitive characteristic and waveguide properties.
Embodiment 2: at first by 1: 4 mol ratio Virahol germanium and 2-methyl cellosolve are mixed and stir as solution A; By 1: 3: 3 mol ratio with 3-(Trimethoxy silane base) propyl methyl acid esters, Virahol and the hydrolysis of deionized water mixing and stirring after as solution B; By 1: 4: 4 mol ratio Union carbide A-162, ethanol and deionized water are mixed, then in mixed solution by Union carbide A-162: hydrochloric acid be 100: 1 mole add hydrochloric acid stir as catalyzer after as solution C;
Then the solution A of 30 molfractions, the solution B of 50 molfractions and the solution C of 20 molfractions are mixed stirring at room temperature, evenly contained the low temperature organic-inorganic composite ground mass mother liquor of SiGe;
Two (2,4, the 6-trimethylbenzoyl) phenyl phosphine oxide light triggers of organic-inorganic composite ground mass mother liquor gross weight 3.5% are joined in the organic-inorganic composite ground mass mother liquor, and under darkroom and room temperature, stir and obtain suspension liquid;
Utilize spin coating technology under the situation that rotating speed changes for per minute 3000, the above-mentioned suspension liquid that obtains to be deposited on the glass substrate, to deposit good film sample then is placed under 80 ℃ of temperature and handled 15 minutes, can obtain individual layer and have about 2 micron thickness, and smooth surface is smooth and have a germanium dioxide base organic-inorganic composite film material of UV photosensitive characteristic and waveguide properties.
Embodiment 3: at first by 1: 4 mol ratio Virahol germanium and 2-methyl cellosolve are mixed and stir as solution A; By 1: 3: 3 mol ratio with 3-(Trimethoxy silane base) propyl methyl acid esters, Virahol and the hydrolysis of deionized water mixing and stirring after as solution B; By 1: 4: 4 mol ratio Union carbide A-162, ethanol and deionized water are mixed, then in mixed solution by Union carbide A-162: hydrochloric acid be 100: 1 mole add hydrochloric acid stir as catalyzer after as solution C;
Then the solution A of 35 molfractions, the solution B of 30 molfractions and the solution C of 35 molfractions are mixed stirring at room temperature, evenly contained the low temperature organic-inorganic composite ground mass mother liquor of SiGe;
Two (2,4, the 6-trimethylbenzoyl) phenyl phosphine oxide light triggers of organic-inorganic composite ground mass mother liquor gross weight 4% are joined in the organic-inorganic composite ground mass mother liquor, and under darkroom and room temperature, stir and obtain suspension liquid;
Utilize spin coating technology under the situation that rotating speed changes for per minute 3500, the above-mentioned suspension liquid that obtains to be deposited on the glass substrate, to deposit good film sample then is placed under 100 ℃ of temperature and handled 10 minutes, can obtain individual layer and have about 2 micron thickness, and smooth surface is smooth and have a germanium dioxide base organic-inorganic composite film material of UV photosensitive characteristic and waveguide properties.
Embodiment 4: at first by 1: 4 mol ratio Virahol germanium and 2-methyl cellosolve are mixed and stir as solution A; By 1: 3: 3 mol ratio with 3-(Trimethoxy silane base) propyl methyl acid esters, Virahol and the hydrolysis of deionized water mixing and stirring after as solution B; By 1: 4: 4 mol ratio Union carbide A-162, ethanol and deionized water are mixed, then in mixed solution by Union carbide A-162: hydrochloric acid be 100: 1 mole add hydrochloric acid stir as catalyzer after as solution C;
Then the solution A of 40 molfractions and the solution B of 60 molfractions are mixed stirring at room temperature, evenly contained the low temperature organic-inorganic composite ground mass mother liquor of SiGe;
Two (2,4, the 6-trimethylbenzoyl) phenyl phosphine oxide light triggers of organic-inorganic composite ground mass mother liquor gross weight 4.5% are joined in the organic-inorganic composite ground mass mother liquor, and under darkroom and room temperature, stir and obtain suspension liquid;
Utilize spin coating technology under the situation that rotating speed changes for per minute 4000, the above-mentioned suspension liquid that obtains to be deposited on the glass substrate, to deposit good film sample then is placed under 120 ℃ of temperature and handled 20 minutes, can obtain individual layer and have about 2 micron thickness, and smooth surface is smooth and have a germanium dioxide base organic-inorganic composite film material of UV photosensitive characteristic and waveguide properties.
The UV photosensitive characteristic of the germanium dioxide base organic-inorganic composite material of prepared light sensitive characteristic according to the present invention, in conjunction with mask technique or other laser technology (laser writes technology, laser holography etc.) or electron beam lithography, be placed directly in ethanolic soln then and develop, can realize the making of fiber waveguide device cheaply or other micro-optic device.
Fig. 1 is the Fourier transform infrared spectroscopy graphic representation that has the quick material of germanium dioxide base organic-inorganic composite ultraviolet that obtains under the different heat treatment temperature in the above-mentioned example.As seen from the figure; under 400 degree temperature, handle the thin-film material that obtains; the C-C that is about corresponding carbonic acyl radical ester group peak in 1718cm-1 and 1632cm-1 place and vinyl groups in wave number can be known and is observed, and the intensity at these peaks reduces along with the rising of temperature.These results show that the matrix material that obtains has the UV photosensitive characteristic under the thermal treatment temperature below 300 degree.
Fig. 2 is based on laminated film substrate material UV photosensitive characteristic in the above-mentioned example 3 in conjunction with photomask technology, and chemical development then (being placed on ethanolic soln) is removing not by the ultraviolet lighting part, thus the ridge optical waveguide array X-Y scheme and the distribution plan thereof that make.Distance between the waveguide is about about 122 microns as seen from the figure, about 0.4 micron of the waveguide degree of depth.The structural cycle of waveguide depends primarily on template, and the waveguide degree of depth is mainly by time shutter and development time decision.Obviously the compound photochromics of such organic and inorganic writes etc. in conjunction with laser technology (writing as laser), electron beam, is expected to be used for the low cost and the batch making of micro-optic devices such as grating, binary optical lens.
Fig. 3 is ridge optical waveguide three-dimensional picture and the cross-sectional distribution figure thereof that makes in conjunction with photomask technology based on laminated film substrate material UV photosensitive characteristic in the example 3.As can be seen from the figure the width of ridge waveguide is about 10 microns, about 0.4 micron of the degree of depth.What be worth emphasizing is that the thickness of laminated film is 1.6 microns, but the degree of depth of ridge waveguide has only 0.4 micron, much smaller than 1.6 microns, this be because the waveguide degree of depth mainly by time shutter and development time decision.
Fig. 4 is that the ridge optical waveguide made based on this laminated film substrate material UV photosensitive characteristic and Fig. 3 are than ridge optical waveguide three-dimensional picture with longer time shutter and cross-sectional distribution figure thereof.As can be seen from the figure the width of ridge waveguide is about 10 microns, but the degree of depth only is 0.3 micron, and a small rut occurs on the top, top of waveguide, and these are owing to overexposure causes.
Claims (1)
1. the preparation method of the germanium dioxide base organic-inorganic composite material of light sensitive characteristic is characterized in that:
1) at first Virahol germanium and 2-methyl cellosolve are mixed and stir as solution A by 1: 4 mol ratio; By 1: 3: 3 mol ratio with 3-(Trimethoxy silane base) propyl methyl acid esters, Virahol and the hydrolysis of deionized water mixing and stirring after as solution B; By 1: 4: 4 mol ratio Union carbide A-162, ethanol and deionized water are mixed, then in mixed solution by Union carbide A-162: hydrochloric acid is that 100: 1 mol ratio adds hydrochloric acid and stirs afterwards as solution C as catalyzer;
2) then the solution A of 20-40 molfraction, the solution B of 30-60 molfraction and the solution C of 0-40 molfraction are mixed stirring at room temperature, evenly contained the low temperature organic-inorganic composite ground mass mother liquor of SiGe;
3) two (2,4, the 6-trimethylbenzoyl) the phenyl phosphine oxide light triggers with organic-inorganic composite ground mass mother liquor gross weight 3.0-4.5% join in the organic-inorganic composite ground mass mother liquor, and stir under darkroom and room temperature and obtain suspension liquid;
4) utilize spin coating technology under the situation that rotating speed changes for per minute 2500-4000, the above-mentioned suspension liquid that obtains to be deposited on the glass substrate, to deposit good film sample then and be placed under the 80-120 ℃ of temperature and handled 10-20 minute, can obtain the germanium dioxide base organic-inorganic composite material of light sensitive characteristic.
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| GB201202128D0 (en) | 2012-02-08 | 2012-03-21 | Univ Leeds | Novel material |
| CN102540333B (en) * | 2012-02-22 | 2013-07-10 | 西安交通大学 | Method for preparing functional strip waveguides from silicon-titanium organic-inorganic composite material with ultraviolet photosensitivity characteristics |
| CN103744250B (en) * | 2013-12-23 | 2016-06-29 | 西安交通大学 | The preparation method with the low-temperature germanium dioxide-organic modified silicate composite material improving optics third-order non-linear quality factor |
| CN112034637B (en) * | 2020-08-21 | 2023-01-31 | 南京邮电大学 | Germanium dioxide based photosensitive composite film and preparation and application thereof |
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| CN1975465A (en) * | 2006-12-05 | 2007-06-06 | 西安交通大学 | Method for producing low-temperature germanium dioxide-organic modified silicate composite material |
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| JPS6255645A (en) * | 1985-09-04 | 1987-03-11 | Takeda Chem Ind Ltd | Photosensitive material |
| JPS63121854A (en) * | 1986-11-11 | 1988-05-25 | Matsushita Electric Ind Co Ltd | Electrophotographic sensitive body |
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| US4990423A (en) * | 1988-06-30 | 1991-02-05 | Sharp Kabushiki Kaisha | Photosensitive member for electrophotography |
| CN1975465A (en) * | 2006-12-05 | 2007-06-06 | 西安交通大学 | Method for producing low-temperature germanium dioxide-organic modified silicate composite material |
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