CN102173599A - Acid induction liquid phase deposition preparation method for germanium dioxide hollow-core optical wave guide - Google Patents
Acid induction liquid phase deposition preparation method for germanium dioxide hollow-core optical wave guide Download PDFInfo
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Abstract
The invention relates to an acid induction liquid phase deposition preparation method for germanium dioxide hollow-core optical wave guide and belongs to the field of optical material application. In the preparation method, germanium dioxide is dissolved in alkaline solution to form precursor solution, and acid is added into the precursor solution to ensure that a germanium dioxide film is generated by acid induction homogeneous phase liquid phase deposition and the germanium dioxide film is subjected to densified thermal treatment to form the germanium dioxide hollow-core optical wave guide. The preparation method comprises the steps of: (1) preparing germanium dioxide deposition solution; (2) growing the germanium dioxide film; and (3) performing densified thermal treatment on the germanium dioxide film. Compared with a chemical vapor deposition method, the preparation method has the advantages that: the adopted precursor solution is stable and has low synthesis cost, the reaction temperature is low, the reaction conditions are mild and the method can be easy to control. Compared with a sol-gel method, the preparation method has the advantages that: the precursor solution generated by reacting germanium dioxide and ammonia water has high stability in the air and can be stored for a long period, and the used raw materials have low price, and the germanium dioxide reflection film of which the thickness can reach the micron can be prepared on the inner wall of a quartz glass tube.
Description
Technical field
Liquid deposition preparation method is induced in the acid that the present invention relates to a kind of germanium dioxide hollow core optical waveguide, belongs to the optical material Application Areas.
Background technology
Carbon dioxide laser is a kind of important mid-infrared laser, and its wavelength is 10.6 microns, just in time is in atmospheric window, and atmosphere absorbs little to it, but tissue and metal etc. have big uptake factor to it.Therefore carbon dioxide laser has important application in infrared optoelectronic information technology, laser medicine and forming materials processing and other fields.Transmission media makes carbon dioxide laser be subjected to bigger restriction in these Application for Field owing to lack effectively at present.The carbon dioxide laser wavelength has determined it not transmit with traditional quartzy communication optical waveguides.Hollow core optical waveguide as transmission medium, can avoid in the real core optical waveguides heat to be difficult to scatter and disappear and problem such as foreign ion absorption loss height with air, has higher energy damage threshold.Therefore hollow core optical waveguide is considered to transmit the better selection of carbon dioxide laser.The hollow core optical waveguide of laboratory study at present has leakage type and fully-reflected type two classes.Leakage type optical waveguides is restricted its application owing to the metallic mirror surface reflection can cause problems such as dispersing of light spread modes and mixed mould phenomenon and hot spot focusing quality be relatively poor.The fully-reflected type hollow core optical waveguide realizes the transmission of carbon dioxide laser according to the total reflection principle of light, good optical transmission mode makes it have advantage at aspects such as focusing, sensing, imaging, signal loading, so it can be applied to a plurality of fields such as optoelectronic information, infrared sensing, environmental monitoring, laser medicine and military infrared viewing device.
In the research of fully-reflected type hollow core optical waveguide, material and preparation technology are the emphasis that the various countries investigator pays close attention to always.How selecting specific optical waveguide material and it is had more low-loss hollow core optical waveguide by rational prepared one-tenth, is the important topic that people face.Discover that germanium dioxide is located anomalous dispersion takes place and made its specific refractory power less than 1 10.6 microns of carbon dioxide laser wavelength, can realize that carbon dioxide laser is the total reflection mode transfer of transmission medium by air.In the preparation process of germanium dioxide fully-reflected type hollow core optical waveguide, most important is exactly preparation one deck germanium dioxide reflectance coating on the parent tube internal surface.The main method of preparation germanium dioxide hollow wave guide reflectance coating has chemical vapour deposition and sol-gel method at present.The presoma GeCl that uses in the chemical Vapor deposition process
4More expensive and very easily hydrolysis, the thousands of degree of chemical vapour deposition reaction temperature, the fierce difficult control of the gas-phase chemical reaction in the elongated small space of parent tube, it is too fast and cause kapillary and stop up to occur local germanium dioxide deposition easily, can set off an explosion when serious.Expensive and the very easily hydrolysis of the germanium alkoxide precursor that uses in the sol-gel method, the difficult control of colloidal sol building-up reactions, the monofilm thickness of preparation is low excessively.Therefore explore a kind of simple and can on the parent tube internal surface, prepare evenly, fine and close, germanium dioxide reflectance coating that thickness reaches the total reflection requirement, be the key point of preparation germanium dioxide fully-reflected type hollow wave guide.The solution of this key issue is transmitted and is widened its application in fields such as optoelectronic information, infrared sensing, environmental monitoring, laser medicine and infrared night visions for the total reflection that realizes carbon dioxide laser and is significant.
Summary of the invention
The object of the present invention is to provide a kind of acid of germanium dioxide hollow core optical waveguide to induce liquid deposition preparation method, this method cost is low, simple to operate, convenient preparation thick film.
Liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide of the present invention, germanium dioxide is dissolved in basic solution generates precursor liquid, in precursor liquid, add acid realization acid and induce homogeneous phase liquid deposition growth germanium dioxide film, and make through the germanium dioxide film is carried out densification thermal treatment, comprise the steps:
(1) preparation germanium dioxide deposit fluid: the germanium dioxide powder is dissolved in the basic solution, obtains the germanium dioxide mass concentration after fully stirring and be 1～12% precursor liquid; Make inductor and it is joined in the precursor liquid to mix with acid, obtain the germanium dioxide deposit fluid;
(2) growth germanium dioxide film: the germanium dioxide deposit fluid is injected quartz glass tube, and quartz glass tube is supported on the support and grows the germanium dioxide film after 20～240 hours in the rotary state deposit on inside pipe wall;
(3) the densification thermal treatment of germanium dioxide film: after the quartz glass tube drying of germanium dioxide film is arranged on the inwall, heat-treat densification, make the germanium dioxide hollow core optical waveguide.
Among the present invention:
Selected basic solution is sodium hydroxide solution and ammoniacal liquor.
The precursor liquid acid for adjusting pH is 0～5.
In germanium dioxide film process of growth, quartz glass tube horizontally rotates.
The densification thermal treatment temp is 1100～1160 ℃, and the time is 10～60 minutes.Preferably in electric tube furnace, carry out.
The germanium dioxide hollow core optical waveguide that the present invention makes can be transmitted carbon dioxide laser.
Thereby the present invention can by control deposit fluid concentration, induce acid kind, pH value, depositing time and conditions such as number of times, thermal treatment temp and time make the different germanium dioxide reflectance coating of thickness.
The present invention induces liquid deposition and has obtained the germanium dioxide hollow core optical waveguide through subsequent heat treatment by acid, and compare the precursor liquid that is adopted with chemical Vapor deposition process stable and synthetic cost is low, and temperature of reaction is low, and reaction conditions is comparatively gentle and be easy to control.Compare the precursor solution property stable in the air that generates with germanium dioxide and ammoniacal liquor reaction among the present invention with sol-gel method good, can prolonged preservation, employed raw material is compared cheap with traditional germanium alkoxide, can be implemented in to make thickness on the inwall of quartz glass tube and reach micron-sized germanium dioxide reflectance coating.
Description of drawings
Fig. 1 is the digital photograph in kind after silica glass parent tube interior deposition germanium dioxide film and the densification thereof.
Fig. 2 is the SEM photo of inducing the germanium dioxide film that the liquid phase deposition process grows under the room temperature by acid.
Fig. 3 is the SEM photo of acid being induced the germanium dioxide film thermal treatment densification caudacoria that the liquid phase deposition growing goes out.
Fig. 4 is the SEM photo of inducing the germanium dioxide film that the liquid phase deposition process grows under the room temperature by acid,
Concrete mode of deposition is: hydrochloric acid is for inducing acid, the mass concentration 5% of germanium dioxide in the precursor liquid, and pH=1 deposits 48h, and frequency of depositing is once.
Fig. 5 is the SEM photo of inducing the germanium dioxide film that the liquid phase deposition process grows under the room temperature by acid,
Concrete mode of deposition is: sulfuric acid is for inducing acid, the mass concentration 5% of germanium dioxide in the precursor liquid, and pH=1 deposits 48h, and frequency of depositing is once.
Fig. 6 induces section SEM photo after the germanium dioxide film thermal treatment densification that the liquid phase deposition process grows with acid,
Concrete mode of deposition is: sulfuric acid is for inducing acid, germanium dioxide mass concentration 6% in the precursor liquid, and pH=4 deposits 72h, and frequency of depositing is once.
Fig. 7 induces section SEM photo after the germanium dioxide film thermal treatment densification that the liquid phase deposition process grows with acid,
Concrete mode of deposition is: sulfuric acid is for inducing acid, germanium dioxide mass concentration 6% in the precursor liquid, pH=4, deposition 72h, frequency of depositing three times.
Fig. 8 induces the liquid phase deposition process to grow the digital photograph in kind of the quartz glass tube of germanium dioxide film in pipe by acid under the condition of different pH.
Concrete mode of deposition is: nitric acid is for inducing acid, germanium dioxide mass concentration 6% in the precursor liquid, and pH is respectively 2,3,4 and 5, deposits 96h, and frequency of depositing is once.
Fig. 9 is the SEM photo of inducing the germanium dioxide film that the liquid phase deposition process grows under the room temperature by acid,
Concrete mode of deposition is: nitric acid is for inducing acid, the mass concentration 9% of germanium dioxide in the precursor liquid, and pH=2 deposits 72h, and frequency of depositing is once.
Embodiment
The present invention is further detailed explanation below in conjunction with embodiment and accompanying drawing.
Can find out clearly that from Fig. 1 inducing homogeneous phase liquid deposition process by acid can be the silica glass inside pipe wall deposition layer of even germanium dioxide film of 1mm at internal diameter.Comparison diagram 2 and Fig. 3, as can be seen the germanium dioxide film of room temperature deposition be by approximate cubical particle inlay each other, tightly packed forming, the particle diameter of cubes particle is about 4～5 microns, after Overheating Treatment, formed the germanium dioxide reflectance coating of one deck densification on the inwall of quartz glass tube, its thickness is about 10 microns.Mostly between 3dB/m～7dB/m, through-put power can reach tens watts to the prepared germanium dioxide total reflection of this patent hollow core optical waveguide to the transmission loss of carbon dioxide laser, and the transmission loss of some sample is lower, reaches 0.65dB/m.Under equal test condition, find when carrying out the Laser Transmission experiment that through-put power is zero with the silica glass parent tube that does not have the germanium dioxide reflectance coating.This shows that the germanium dioxide film for preparing with this patent method brought into play keying action to the transmission of laser on the silica glass inside pipe wall.Power requirement to the transmission carbon dioxide laser in a lot of practical applications arrives watt level in the milliwatt level, so the germanium dioxide hollow wave guide that the present invention prepares has actual application value.
Embodiment 1
Liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide of the present invention, comprises the following steps:
(1) the 0.5g germanium dioxide being dissolved into mass concentration is to obtain transparent precursor liquid in 2% the ammoniacal liquor, and the germanium dioxide mass concentration is 5%;
(2) regulate precursor liquid pH to 1 with hydrochloric acid and obtain the germanium dioxide deposit fluid;
(3) the germanium dioxide deposit fluid injection internal diameter with (2) gained is the quartz glass tube of 1.5mm, port with thermoplastic tube sealing quartz glass tube, and quartz glass tube is placed on the support, keeping Glass tubing to horizontally rotate state deposit 48h, the SEM photo of the germanium dioxide film that grows on inside pipe wall as shown in Figure 4;
(4) with after inwall has the quartz glass tube drying of germanium dioxide film in (3), 1130 degree thermal treatments made the film densification in 15 minutes in tube type resistance furnace, obtained the germanium dioxide hollow core optical waveguide;
Repeat above-mentioned steps, the SEM photo that changes the hydrochloric acid in (2) into germanium dioxide film that sulfuric acid grows on inside pipe wall as shown in Figure 5.
When using hydrochloric acid to make inductor as can be seen from Figure 4, all growth is incomplete for germanium dioxide particulate hexahedron wedge angle major part, and particle size is bigger.When using sulfuric acid to make inductor as can be seen from Figure 5, germanium dioxide particulate hexahedron wedge angle is partly grown more complete, and particle size is less, and particle packing is tight, and the thickness of the germanium dioxide film of growing on inwall after the thermal treatment densification is about 2.5 μ m.Induce the grain diameter of the germanium dioxide film that the liquid phase deposition process grows little by acid under the room temperature, pile up closely, help to improve the surface flatness of germanium dioxide film after the thermal treatment densification, and after the thermal treatment densification on the silica glass inside pipe wall surface of germanium dioxide film smooth more, the loss that laser transmits in hollow core optical waveguide is low more.
Liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide of the present invention, comprises the following steps:
(1) the 0.6g germanium dioxide being dissolved into mass concentration is to obtain transparent precursor liquid in 9% the ammoniacal liquor, and the germanium dioxide mass concentration is 6%;
(2) regulate precursor liquid pH to 4 with sulfuric acid and obtain the germanium dioxide deposit fluid;
(3) the germanium dioxide deposit fluid injection internal diameter with (2) gained is the quartz glass tube of 1.5mm, port with thermoplastic tube sealing quartz glass tube, and quartz glass tube is placed on the support, at rotary state deposit 72h, discharge the solution in the quartz glass tube, repeating step 1,2,3 carries out three depositions of quartz glass tube;
(4) with after inwall has the quartz glass tube drying of germanium dioxide film in (3), 1120 degree thermal treatments made the film densification in 30 minutes in tube type resistance furnace, obtain the germanium dioxide hollow core optical waveguide, the section SEM photo of the germanium dioxide film that primary depositing grows on inside pipe wall as shown in Figure 6, the section SEM photo that is deposited on the germanium dioxide film that grows on the inside pipe wall for three times is as shown in Figure 7.
The germanium dioxide mass concentration is that 6% precursor liquid is about 4 μ m through the germanium dioxide film thickness that primary depositing obtains as can be seen from Figure 6, and the loss of the hollow core optical waveguide that makes is 11.8dB/m.The germanium dioxide mass concentration is that the germanium dioxide film thickness that 6% precursor liquid obtains after through three depositions is about 10 μ m as can be seen from Figure 7.Along with the increase of frequency of depositing, the thickness of germanium dioxide film becomes big on the parent tube inwall.
Liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide of the present invention, comprises the following steps:
(1) the 2.4g germanium dioxide being dissolved into mass concentration is to obtain transparent precursor liquid in 2% the ammoniacal liquor, and the mass concentration of germanium dioxide is 6%;
(2) solution with (1) gained is divided into 4 parts, regulates 4 parts of precursor liquid pH with nitric acid, and the pH of 4 parts of precursor liquids is respectively 2,3, and 4 and 5, obtain the germanium dioxide deposit fluid;
(3) quartz glass tube that the germanium dioxide deposit fluid of (2) gained is injected 4 internal diameters respectively is 1mm, port with thermoplastic tube sealing quartz glass tube, and quartz glass tube is placed on the support, at rotary state deposit 96h, obtain inwall length have germanium dioxide quartz glass tube digital photograph in kind as shown in Figure 8;
(4) with after inwall has the quartz glass tube drying of germanium dioxide film in (3), 1125 degree thermal treatments made the film densification in 40 minutes in tube type resistance furnace, obtained the germanium dioxide hollow core optical waveguide.
The pH that from Fig. 8, can find precursor liquid clearly not simultaneously, through the thickness difference of the germanium dioxide film of growing on the identical depositing time silica glass inside pipe wall.The pH of precursor liquid is that the thickness of the germanium dioxide film of growing on the silica glass inside pipe wall in 2 o'clock is the thickest.
Liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide of the present invention, comprises the following steps:
(1) the 0.5g germanium dioxide being dissolved into mass concentration is to obtain transparent precursor liquid in 8% ammoniacal liquor, and the germanium dioxide mass concentration is 5%;
(2) regulate precursor liquid pH to 3 with phosphoric acid and obtain the germanium dioxide deposit fluid;
(3) the germanium dioxide deposit fluid injection internal diameter with (2) gained is the quartz glass tube of 1.5mm, port with thermoplastic tube sealing quartz glass tube, and quartz glass tube is placed on the support, keeping Glass tubing to horizontally rotate state deposit 72h, repeating step 1,2,3 carries out quartz glass tube secondary and three depositions;
(4) with in (3) once, after secondary and three times deposition back inwalls have the quartz glass tube drying of germanium dioxide film, 1120 degree thermal treatments made the film densification in 15 minutes in tube type resistance furnace, obtained the germanium dioxide hollow core optical waveguide;
Once, secondary and three times deposition back inwall has the loss of the hollow core optical waveguide that makes after the quartz glass tube thermal treatment densification of germanium dioxide film to be respectively 19dB/m, 6.2dB/m and 3.1dB/m.We know that frequency of depositing increases by example 2 and example 4, and it is big that the thickness of the germanium dioxide film on the silica glass inside pipe wall becomes, and loss reduces, hollow core optical waveguide the best that three depositions make.The thickness of this explanation germanium dioxide film is the important factor that influences the hollow core optical waveguide loss.
Liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide of the present invention, comprises the following steps:
(1) the 0.7g germanium dioxide being dissolved into mass concentration is to obtain transparent precursor liquid in 5% the ammoniacal liquor, and the germanium dioxide mass concentration is 7%;
(2) regulate precursor liquid pH to 2 with sulfuric acid and obtain the germanium dioxide deposit fluid;
(3) the germanium dioxide deposit fluid of (2) gained being injected internal diameter is the quartz glass tube of 1.5mm, with the port of thermoplastic tube sealing quartz glass tube, and quartz glass tube is placed on the support, is keeping Glass tubing to horizontally rotate state deposit 120h;
(4) with after inwall has the quartz glass tube drying of germanium dioxide film in (3), 1140 degree thermal treatments made the film densification in 35 minutes in tube type resistance furnace, and the loss of prepared hollow core optical waveguide is 0.65dB/m.
Embodiment 6
Liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide of the present invention, comprises the following steps:
(1) the 0.9g germanium dioxide being dissolved into mass concentration is to obtain transparent precursor liquid in 1.5% the sodium hydroxide solution, and the germanium dioxide mass concentration is 9%;
(2) regulate precursor liquid pH to 2 with nitric acid and obtain the germanium dioxide deposit fluid;
(3) the germanium dioxide deposit fluid injection internal diameter with (2) gained is the quartz glass tube of 1.5mm, port with thermoplastic tube sealing quartz glass tube, and quartz glass tube is placed on the support, keeping Glass tubing to horizontally rotate state deposit 72h, the SEM photo of the germanium dioxide film that grows on inside pipe wall as shown in Figure 9;
(4) with after inwall has the quartz glass tube drying of germanium dioxide film in (3), 1140 degree thermal treatments made the film densification in 35 minutes in tube type resistance furnace.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment did, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (5)
1. liquid deposition preparation method is induced in the acid of a germanium dioxide hollow core optical waveguide, it is characterized in that germanium dioxide is dissolved in and generate precursor liquid in the basic solution, in precursor liquid, add acid realization acid and induce homogeneous phase liquid deposition growth germanium dioxide film, and make through the germanium dioxide film is carried out densification thermal treatment, comprise the steps:
(1) preparation germanium dioxide deposit fluid: the germanium dioxide powder is dissolved in the basic solution, obtains the germanium dioxide mass concentration after fully stirring and be 1～12% precursor liquid; Make inductor and it is joined in the precursor liquid to mix with acid, obtain the germanium dioxide deposit fluid;
(2) growth germanium dioxide film: the germanium dioxide deposit fluid is injected quartz glass tube, and quartz glass tube is supported on the support and grows the germanium dioxide film after 20～240 hours in the rotary state deposit on inside pipe wall;
(3) the densification thermal treatment of germanium dioxide film: after the quartz glass tube drying of germanium dioxide film is arranged on the inwall, heat-treat densification, make the germanium dioxide hollow core optical waveguide.
2. liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide according to claim 1, it is characterized in that the precursor liquid acid for adjusting pH is 0～5.
3. liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide according to claim 1 and 2, it is characterized in that quartz glass tube horizontally rotates.
4. liquid deposition preparation method is induced in the acid of germanium dioxide hollow core optical waveguide according to claim 1, it is characterized in that the densification thermal treatment temp is 1100～1160 ℃, and the time is 10～60 minutes.
5. the germanium dioxide hollow core optical waveguide that makes of the described method of claim 1 can be transmitted carbon dioxide laser.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103592719A (en) * | 2013-10-23 | 2014-02-19 | 华东师范大学 | Manufacturing method of metal capillary attenuated total reflection infrared hollow optical fiber and optical fiber obtained through the manufacturing method |
| CN107991733A (en) * | 2016-10-27 | 2018-05-04 | 华东师范大学 | Metal capillary germanium dioxide dielectric film mid and far infrared hollow-core fiber and preparation |
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| EP0249886A1 (en) * | 1986-06-19 | 1987-12-23 | 3M Fiber Optic Products, Inc. | Method of manufacturing hollow core optical fibers |
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| US4411678A (en) * | 1981-04-02 | 1983-10-25 | Nippon Electric Co., Ltd. | Method for fabricating an optical waveguide on a planar glass substrate |
| EP0249886A1 (en) * | 1986-06-19 | 1987-12-23 | 3M Fiber Optic Products, Inc. | Method of manufacturing hollow core optical fibers |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103592719A (en) * | 2013-10-23 | 2014-02-19 | 华东师范大学 | Manufacturing method of metal capillary attenuated total reflection infrared hollow optical fiber and optical fiber obtained through the manufacturing method |
| CN103592719B (en) * | 2013-10-23 | 2016-06-01 | 华东师范大学 | Metal capillary attenuated total reflectance attenuated total refraction infrared hollow optical fiber making method and optical fiber thereof |
| CN107991733A (en) * | 2016-10-27 | 2018-05-04 | 华东师范大学 | Metal capillary germanium dioxide dielectric film mid and far infrared hollow-core fiber and preparation |
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Address after: 200241 room 243, School of information, East China Normal University, 500 Dongchuan Road, Shanghai, Minhang District Applicant after: Jing Chengbin Address before: 266042 Qingdao University of Science & Technology, 53 Zhengzhou Road, Sifang District, Shandong, Qingdao Applicant before: Jing Chengbin |
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Application publication date: 20110907 |