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CN101907739B - Additional electric field-assisted ion exchange device - Google Patents

Additional electric field-assisted ion exchange device Download PDF

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Publication number
CN101907739B
CN101907739B CN 201010240159 CN201010240159A CN101907739B CN 101907739 B CN101907739 B CN 101907739B CN 201010240159 CN201010240159 CN 201010240159 CN 201010240159 A CN201010240159 A CN 201010240159A CN 101907739 B CN101907739 B CN 101907739B
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pottery
exchange
ceramic
potsherd
glass sheet
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CN101907739A (en
Inventor
周自刚
李静
罗小英
孙光春
陈文强
邓宗权
周航成
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Southwest University of Science and Technology
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Southwest University of Science and Technology
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Abstract

The invention discloses manufacturing technology and a using method for an additional electric field-assisted ion exchange device. The additional electric field-assisted ion exchange device comprises inner ceramic, outer ceramic, a ceramic rod, a ceramic wafer and an exchange K9 glass sheet, wherein the outer ceramic is used for containing fused salt for exchange; the inner ceramic, the ceramic wafer and the exchange K9 glass sheet are superimposed fixedly and sequentially; the inner ceramic is fixedly connected with the ceramic rod, and is hung in the outer ceramic through the ceramic rod; and the bottom of the inner ceramic and the ceramic wafer are provided a through hole for fixing a negative electrode respectively, and the negative electrodes are closely contacted with one surface of an exchange K9 glass nickel plating membrane through the through hole of the ceramic wafer.

Description

A kind of additional electric field-assisted ion exchange device
Technical field:
The invention belongs to the technical field of integrated light guide, is a kind of efficient, stable, equal even device that controllably prepares integrated light guide, particularly a kind of additional electric field-assisted ion exchange device.
Background technology:
Development along with photoelectron technology, be applied to the various transmission signals of needs in the optical communication, objectively require high photonic device integrated, microminiaturized, buried type to occur, and wherein fiber waveguide device is exactly the needs of adaptation optical communication and the photonic device that produces and grow up.Its basic thought is on the surface of same substrate, with the material optical waveguide of refractive index mutability, and makes array laser, modulator etc. based on this again.By this integrated, can realize the microminiaturization, stability of optical system, the purpose of easy of integration and homogenising.
In the active and passive photon preparation of devices of integrated optics, adopt prepared in various methods, but a kind of method simple, that cost is low is an ion exchange process.But the method need be tested control, in natural situation following Production Time oversize (generally more than 24 hours).
Having under the auxiliary situation of extra electric field, the self-diffusion coefficient of ion is just not only depended in the thermion exchange, also can be subjected to the influence of extra electric field.In ion exchange process, the Na in the fused salt +Ion enters into K9 glass by diffusion, the Cs in the K9 glass +Ions diffusion is come out, and the flux of every kind of ion can be used following formula:
φ ‾ ρ = - D Cs ▿ C ‾ Cs ∂ ln α ‾ Cs ∂ ln C ‾ Cs + μ ‾ Cs C ‾ Cs E ρ
In the formula Molar flow (mol/m for ion 2.s),
Figure BSA00000209783000013
Be Cs ion-conductance chemical transport rate (m 2/ V.s),
Figure BSA00000209783000014
Be the concentration (mol/m of Cs ion in K9 glass 3),
Figure BSA00000209783000015
Be external electric field intensity (V/cm).
Therefore, in the contemporary optics field, the important effect of the positive play more and more of a kind of added electric field ion interchange unit.
Summary of the invention:
Technical matters to be solved by this invention is:
1, in the exchange post anneal, K9 glass can well separate with fused salt, thereby avoids fused salt to push the K9 glass surface in process of setting, causes the exchange area fragmentation;
2, under need not any appendicular situation, make negative electrode and K9 glass contact stable;
3, assurance device fused salt in exchange process can not flow into negative electrode, causes short circuit.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of additional electric field-assisted ion exchange device comprises interior pottery, outer pottery, ceramic rod, potsherd and exchange K9 glass sheet; Described outer pottery is used to hold the employed fused salt of exchange; Pottery, described potsherd, described exchange K9 glass sheet fixedly are superimposed together successively in described; Pottery is fixedlyed connected with described ceramic rod in described, by described ceramic rod pottery in described is hung in the outer pottery; Pottery bottom and described potsherd all are provided with a through hole in described, are used for fixing negative electrode, and described negative electrode closely contacts with the one side of described exchange K9 glass plated nickel film by the through hole of described potsherd.
Described ion interchange unit, described two through holes are concentric settings.
Described ion interchange unit adopts high-temp glue that pottery, described potsherd, described exchange K9 glass sheet in described are bonded together successively.
Described ion interchange unit, potsherd size only are 20 * 20mm 2
Described ion interchange unit, outer ceramic length and width height is of a size of 75 * 75 * 50mm 3, interior ceramic length and width height is of a size of 50 * 40 * 25mm 3
Described ion interchange unit, the through-hole diameter of described interior pottery bottom is 5mm, the through-hole aperture of described potsherd is 10mm.
At home, the experiment condition of existing making optical waveguide still can only rest on the level that the fusion ion exchanges naturally; Form problems such as long, the difficult control of burying depth of waveguide time and waveguide region be inhomogeneous in order to solve, the present invention adopts new method that a kind of experimental provision is provided, can accelerate ion-exchange speed, thereby shorten experimental period (generally in 30 minutes), thereby reach the purpose of enhancing productivity.
The invention has the beneficial effects as follows: reduce all kinds of waveguide fabrication times, waveguide region burying depth easy to control and shape, can determine the waveguide region index distribution and guarantee advantages such as waveguide region is uniform and stable.
Description of drawings:
Fig. 1 is an additional electric field-assisted ion exchange device circuit theory synoptic diagram;
Fig. 2 is the additional electric field-assisted ion exchange device cut-open view;
Fig. 3 is the partial enlarged drawing of Fig. 2 corresponding position;
Fig. 4 is the additional electric field-assisted ion exchange device vertical view;
Reference numeral explanation: 1 negative electrode, 2 positive electrodes, 3 ceramic rods, 4 outer potteries, pottery in 5,6 exchange K9 glass sheet, 7 potsherds, 8 titanium films, 9 nickel films, ceramic bottom through-holes in 10,11 potsherd through holes, 12CsNO 3With NaNO 3Fused salt, 13 American Red Prince of the Devils high-temperature-resistant structure glue-lines (having another name called 538 ℃ of high-temperature plastics), 14 ceramic rod wire guides.
Embodiment:
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
As shown in Figure 1, be additional electric field-assisted ion exchange device circuit theory synoptic diagram of the present invention, with reference to figure 2, the capacitor C equivalence is exchange K9 glass sheet 6; The supply voltage scope is 0-80V; Range is that the reometer A of 300 μ A can detect under the high temperature whether short circuit of circuit; Resistance R plays the effect of protection power supply.
Present embodiment provides a kind of additional electric field-assisted ion exchange device, as shown in Figure 2, and pottery 5, outer pottery 4, ceramic rod 3, potsherd 7 and exchange K9 glass sheet 6 in comprising; Described outer pottery 4 is used to hold the employed fused salt of exchange; Pottery 5, described potsherd 7, described exchange K9 glass sheet 6 fixedly are superimposed together successively in described, for example adopt high-temp glue to be bonded together, preferably, as shown in Figure 3, adopt American Red Prince of the Devils high-temperature resistant structural adhesive (having another name called 538 ℃ of high-temperature plastics) layer 13 bonding; Pottery 5 is fixedlyed connected with described ceramic rod 3 in described, by described ceramic rod 3 will be described in pottery 5 hang on outside in ceramic 4; Ceramic 4 bottoms and described potsherd 7 are provided with a through hole 10 and through hole 11 respectively in described, be used for negative electrode 1 wherein ccontaining, fixedly negative electrode 1, and described negative electrode 1 closely contacts with the one side of described exchange K9 glass 6 plated nickel films 9 by the through hole 10 of described potsherd 7.
The using method of apparatus of the present invention is: exchange K9 glass sheet is carried out plated film and photoetching.Adopt ion sputtering after exchange area plates titanium film 8, on the zone, form 1 * 2 with the ultraviolet lithography method NThe exchange area of (N is any natural number) branch, N is 2 in the present embodiment, as shown in Figures 2 and 3, has formed the exchanging window of 4 branches in the titanium film 8.To exchange K9 glass sheet one side center 5 * 5mm 2Plated with nickel film in the zone forms negative electrode area.The potsherd of punching is bonded in interior pottery bottom with high-temp glue, negative electrode nickel sheet is passed from interior ceramic hole, and be fixed on the aperture place of potsherd.To exchange the K9 glass sheet and be bonded on the potsherd, the nickel sheet of negative electrode is contacted closely with the nickel film of exchange K9 glass sheet with high-temp glue.Fig. 1 connects circuit according to circuit theory, and voltage is set.Put into a certain amount of exchange fused salt outside in the pottery, inside and outside pottery is put into high temperature furnace (placed apart) respectively, just establishing temperature is 200 ℃.Be gradient with 40 ℃ subsequently, temperature one by one raises.When temperature was raised to 500 ℃ of left and right sides, the fused salt fusing utilized ceramic rod that interior pottery is suspended on outer ceramic top, and exchange K9 glass sheet is immersed in the fused salt.Open switch, under the added electric field situation, carry out ion-exchange, observe whether deflection of reometer.After exchange 30 minutes, interior pottery is taken out from outer pottery, be placed in the high temperature furnace, carry out annealing in process.With 40 ℃ be gradient, reduce temperature to 200 ℃ one by one after, close the high temperature furnace switch, make it be cooled to room temperature naturally.
For example, all to adopt purity be 99.99%Al for pottery 5 and outer pottery 4 in apparatus of the present invention 2O 3Material, pottery (high 75 * 75 * 50mm of length and width of its China and foreign countries 3) be used to hold the exchange employed fused salt, for example CsNO 3With NaNO 3Fused salt mixt 12; With interior pottery (high 50 * 40 * 25mm of length and width 3) bottom digs the aperture that a diameter is 5mm, so just can guarantee that nickel wire line passes aperture smoothly, and exchange the K9 glass sheet and contact.
Interior pottery hangs on the outer pottery by fixing bonding with ceramic rod.After can guaranteeing that like this exchange finishes, fused salt and K9 glass can separate rapidly, thus after solving exchange, in the annealing process because the cooled and solidified of fused salt, with the problem of bonding exchange K9 glass sheet attrition crushing thereon.Potsherd with a punching (diameter is 10mm) is bonded in interior pottery bottom with high-temp glue then, and guarantees that its sealing is fine.Why selecting diameter is 5mm, is to consider that the potsherd size only is 20 * 20mm 2, if the hole too conference cause that K9 glass is easier to break.Secondly, pottery bottom in passing with power cathode (nickel sheet and lead) allows the nickel sheet of negative electrode be full of the circular hole space of whole potsherd, makes it and exchanges the K9 glass sheet and contact closely.To exchange the K9 glass sheet again and be bonded on the potsherd with high-temp glue, and by extruding, allow exchange K9 glass sheet closely contact with the nickel sheet, and make the exchange area of exchange K9 glass sheet downward, plated nickel film 9 upwards.At last positive source is drawn from the fused salt of outer pottery, forming upper surface on exchange K9 glass sheet is negative pole, and lower surface is anodal electric field, and the exchange K9 glass sheet of this moment has played the effect of similar electric capacity in circuit.This device is put into high temperature furnace, is that thermograde rises one by one with 40 ℃, determines that at last about 500 ℃ are the exchange temperature.In this design,, just can not cause the short circuit of circuit, so we are set in minimum scope to the circular hole size as long as fused salt does not flow into the circular hole of potsherd.Used power supply is the adjustable direct supply of 0-80v, and adjustable resistance case by connecting wide range respectively and the reometer of 300 μ A can play a protective role to circuit, also can in time observe whether short circuit of circuit simultaneously.
Embodiment 2
As different from Example 1, preferred, described two through holes 10 and 11 are provided with one heart.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.

Claims (6)

1. an additional electric field-assisted ion exchange device is characterized in that, comprises interior pottery, outer pottery, ceramic rod, potsherd and exchange K9 glass sheet; Described outer pottery is used to hold the employed fused salt of exchange; Pottery, described potsherd, described exchange K9 glass sheet fixedly are superimposed together successively in described; Pottery is fixedlyed connected with described ceramic rod in described, by described ceramic rod pottery in described is hung in the outer pottery; Pottery bottom and described potsherd all are provided with a through hole in described, are used for fixing negative electrode, and described negative electrode closely contacts with the one side of described exchange K9 glass plated nickel film by the through hole of described potsherd.
2. ion interchange unit according to claim 1 is characterized in that, described two through holes are provided with one heart.
3. ion interchange unit according to claim 1 is characterized in that, adopts high-temperature resistant structural adhesive that pottery, described potsherd, described exchange K9 glass sheet in described are bonded together successively.
4. ion interchange unit according to claim 1 is characterized in that, the potsherd size only is 20 * 20mm 2
5. ion interchange unit according to claim 1 is characterized in that, outer ceramic length and width height is of a size of 75mm-75mm-50mm, and interior ceramic length and width height is of a size of 50mm-40mm-25mm.
6. ion interchange unit according to claim 1 is characterized in that, the through-hole diameter of described interior pottery bottom is 5mm, and the through-hole aperture of described potsherd is 10mm.
CN 201010240159 2010-07-30 2010-07-30 Additional electric field-assisted ion exchange device Expired - Fee Related CN101907739B (en)

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CN111025471B (en) * 2019-12-30 2021-04-13 浙江大学绍兴微电子研究中心 Voltage-segmented glass-based buried optical waveguide continuous production method
CN111239894B (en) * 2020-02-07 2022-11-25 芜湖佳豪电子有限公司 Method for continuously manufacturing buried optical waveguide by using voltage-segmented electric field-assisted ion migration

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CN1128113C (en) * 1999-11-18 2003-11-19 华东理工大学 Non-linear optical wave guide of thiohelogen glass and its preparing process by ion exchange
JP2003149481A (en) * 2001-11-13 2003-05-21 Nec Corp Optical amplifier-integrated waveguide
US7315683B2 (en) * 2004-09-09 2008-01-01 Corning Incorporated Optical waveguides formed in glass-ceramic materials and method for making same
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Inventor after: Zhou Zigang

Inventor after: Li Jing

Inventor after: Luo Xiaoying

Inventor after: Sun Guangchun

Inventor after: Chen Wenqiang

Inventor after: Deng Zongquan

Inventor after: Zhou Hangcheng

Inventor after: Hu Chang

Inventor before: Zhou Zigang

Inventor before: Li Jing

Inventor before: Luo Xiaoying

Inventor before: Sun Guangchun

Inventor before: Chen Wenqiang

Inventor before: Deng Zongquan

Inventor before: Zhou Hangcheng

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Free format text: CORRECT: INVENTOR; FROM: ZHOU ZIGANG LI JING LUO XIAOYING SUN GUANGCHUN CHEN WENQIANG DENG ZONGQUANZHOU HANGCHENG TO: ZHOU ZIGANG LI JING LUO XIAOYING SUN GUANGCHUN CHEN WENQIANG DENG ZONGQUAN ZHOU HANGCHENG HU CHANG

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Granted publication date: 20111012

Termination date: 20120730