CN100359348C - Substrate surface protection method for ion exchange process - Google Patents
Substrate surface protection method for ion exchange process Download PDFInfo
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- CN100359348C CN100359348C CNB200610023418XA CN200610023418A CN100359348C CN 100359348 C CN100359348 C CN 100359348C CN B200610023418X A CNB200610023418X A CN B200610023418XA CN 200610023418 A CN200610023418 A CN 200610023418A CN 100359348 C CN100359348 C CN 100359348C
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Abstract
The present invention relates to a substrate surface protection method in an ion exchange process. The method has the essence that glass material which has the same exchangeable ions with a substrate and has the resistance to the erosion of molten salt is utilized, and the glass material is deposited on the surface of the substrate in filming method to achieve the function that the erosion of the molten salt is prevented in the ion exchange process. The present invention has the advantages of low material cost, easy process and good effect.
Description
Technical field
The present invention relates to ion-exchange process, particularly utilize ion exchange process to prepare integrated optical wave guide device and substrate surfaces such as glass or crystalline material are carried out the guard method of substrate surface in the ion-exchange process that modification handles.
Background technology
In recent years, along with developing rapidly of integrated optics technique, people are more and more deep to the research that fiber waveguide device designs and produces.The making of optical waveguide mainly is at Si, InP, GaAs, LiNbO at present
3, finish on the backing material such as glass, main preparation technology has flame hydrolysis, chemical gaseous phase deposition method, sputtering method, sol-gal process, ion exchange process etc.Wherein utilize ion exchange process to prepare glass light waveguide device to have that simple, with low cost, the prepared glass waveguide device of manufacture craft has that loss is low, refractive index and mould field distribution and optical fiber coupling are good, be convenient to advantages such as integrated, in optical communication, optical sensor and other fields that need handle and control light signal wide application prospect are arranged.
The ultimate principle of utilizing ion exchange process to prepare glass waveguide is: glass substrate is immersed in the fused salt with uniform temperature (as AgNO
3, KNO
3Deng), because the thermal diffusion effect, metal cation is (as Na in the glass
+) with fused salt in metal cation (as Ag
+Or K
+) exchange, the kation in the fused salt enters into glass, and the kation in the glass is displaced, thereby causes the change of exchange place refractive index.By the concentration of exchange ion and the time and the temperature of ions diffusion in the control fused salt, can control the change amount and the index distribution of refractive index, thereby prepare satisfactory glass waveguide device.
Along with the development of material science, the backing material that is used to prepare optical waveguide is more and more.Especially special glass, as rear-earth-doped phosphate glass, Ge-doped photosensitivity glass etc., multiple optical crystal material etc. have various advantage and characteristic.But some special glasss and crystal are in ion exchange process, because the effect of high-temperature molten salt, the surface can suffer erosion, and influences the performance of fiber waveguide device and optical element greatly.Simultaneously, many special glasss and crystalline material also need to utilize ion-exchange process to carry out surface ion modification in application, to strengthen machinery and chemical property.Therefore the protection of substrate surface is the important techniques problem that needs solve in the ion-exchange process.
Summary of the invention
Purpose of the present invention just provides the guard method of substrate surface in a kind of ion-exchange process, to solve the problem that substrate surface is corroded by fused salt.
Experiment basis of the present invention: in the ion-exchange process of routine, often adopt silver nitrate as the exchangeable ion source in the fused salt.Practice shows that it does not have erosion action for silicate glass as K8 glass, K9 glass.Can utilize K9 glass production ion exchange optical waveguide device.For rear-earth-doped phosphate glass, its primary raw material composition is P
2O
5, Al
2O
3, BaO, Na
2O etc. and rare earth element.P
2O
5Has very strong hygroscopic effect.Even after melting becomes glass material, still be subjected to the influence of moisture easily.During ion-exchange, fused salt generally is made of silver nitrate and sodium nitrate mixing, though the silver nitrate components in proportions is not high, the amount of a few percent only, but because silver nitrate is the strong acid weak base material, in fused salt, have stronger acidity, can produce erosion action the surface of phosphate glass.And directly after the K9 ion-exchange process of doing same fused salt on glass, surface topography does not have any variation.
Technical solution of the present invention is as follows:
The guard method of substrate surface in a kind of ion-exchange process; this method is that the substrate that easily corroded by fused salt is before carrying out ion-exchange; utilize a kind of protective material that contains the exchangeable ion identical and have anti-fused salt erosional competency with substrate; adopt the method for plated film to be deposited on the substrate surface, form a thinfilm protective coating.
Described substrate is to be made by rear-earth-doped phosphate glass or rear-earth-doped crystal.
The basic demand of described protective material is: (1) can see through the ion that is exchanged; (2) fused salt had the anti-erosion effect; (3) same substrate has good adhesiveness; (4) has close thermal expansivity.
Described protective material is K9 glass, K8 glass or silicate glass.
Described film plating process is high-frequency sputtering, magnetron sputtering or thermal evaporation.
The guard method of substrate surface in the described ion-exchange process is characterized in that this method comprises following concrete steps:
(1) phosphate glass or crystalline material are made needed workpiece through cutting, processing, polishing;
(2) selected film plating process and corresponding apparatus;
(3) selected protective material is made corresponding target;
(4) the workpiece protective film coating to needing protection;
(5) the preparation fused salt places fused salt with described workpiece, carries out ion-exchange treatment under certain process conditions;
(6) take out workpiece after the ion-exchange, clean its surperficial fused salt, obtain the sample after the ion-exchange treatment.
Advantage of the present invention is: technologies such as the plated film of the technology maturation of lower cost for material, employing and photoetching, and simple for process, respond well.
Description of drawings
Fig. 1 is a substrate surface protective seam synoptic diagram
The 1-substrate, the 2-thinfilm protective coating
Fig. 2 is for to carry out the technological process of ion-exchange treatment to substrate
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing.
The essence of the inventive method is to utilize a kind of glass material that contains the exchangeable ion identical with substrate and have opposing fused salt erosional competency, adopt film plating process to be deposited on the surface of substrate, and then substrate carried out ion-exchange treatment, reach the effect that prevents that in ion exchange process fused salt from corroding.Structural representation as shown in Figure 1.1 for carrying out the substrate of ion-exchange treatment among the figure, and as the phosphate glass substrate, perhaps other are subject to special glass and crystalline material that fused salt corrodes; 2 is thinfilm protective coating, and thickness can be K9 glass, K8 glass or silicate glass etc. in sub-micrometer scale.Because the sodion in phosphate glass and the K9 glass at high temperature has animal migration; Silver ion at high temperature also has certain animal migration simultaneously, and therefore diffusion and exchange will take place.Though the coefficient of diffusion of two kinds of materials has certain difference, ion exchange process can see through the K9 glassivation fully, enters the phosphate laser glass material, and Fig. 1 the right is the concentration of silver ions distribution curve.
Fig. 2 is for to carry out the technological process of ion-exchange treatment to substrate.At first needs are carried out the shaping and the polishing of the optical element of ion-exchange and protection.Such as the dull and stereotyped phosphate glass of polishing, need the lens, prism of surface modification etc.The present invention adopts the method for plated film to prepare the protective seam film, and film plating process can be high-frequency sputtering, magnetron sputtering and thermal evaporation etc.For the high-frequency sputtering coating process, select and process target, such as K9 glass plectane as protective material.According to technological experiment, experimental parameters such as control radio-frequency power, vacuum tightness, sputtering time are at the certain thickness diaphragm of optical element surface deposit.Can carry out ion-exchange process with that.Do if desired and select figure ion-exchange, just carry out ion-exchange again after sheltering pattern carrying out.
Protective material of the present invention will have basic performance requirement, and the one, can see through the ion that is exchanged; The 2nd, have the anti-erosion effect for fused salt; The 3rd, same substrate has good adhesiveness, has close thermal expansivity.For phosphate glass, K9 glass can satisfy these several conditions well.
A specific embodiment of the inventive method:
Substrate material is the phosphate glass of er-doped, and protective material adopts K9 glass.Utilize the high-frequency sputtering coating technique, deposition thickness is about the K9 glass film of 100nm on the erbium doped phosphate glass substrate.Sputter thickness is about the titanium masking film of 150nm again.Spin coating photoresist on titanium metal film, photoetching, development utilize wet etching method to obtain titanium then and shelter pattern.Go to carry out ion-exchange after photoresist, the cleaning.Fused salt is AgNO
3: NaNO
3=2: 98 (mol%), ion-exchange temperature are 340 ℃, and the time is 3 hours.After the ion-exchange, wash surperficial fused salt, wet etching and remove titanium and shelter.Glass substrate after the ion-exchange is carried out cutting, the polishing of end face, finally obtain well behaved ion-exchange waveguides device example.
Claims (6)
1, the guard method of substrate surface in a kind of ion-exchange process; it is characterized in that this method is that the substrate that easily corroded by fused salt is before carrying out ion-exchange; utilize a kind of protective material that contains the exchangeable ion identical and have anti-fused salt erosional competency with substrate; adopt the method for plated film to be deposited on the described substrate surface, form a thinfilm protective coating.
2, the guard method of substrate surface in the ion-exchange process according to claim 1 is characterized in that described substrate is to be made by rear-earth-doped phosphate glass or rear-earth-doped crystal.
3, the guard method of substrate surface in the ion-exchange process according to claim 1, it is characterized in that the basic demand of described protective material is: (1) can see through the ion that is exchanged; (2) fused salt had the anti-erosion effect; (3) same substrate has good adhesiveness; (4) has close thermal expansivity.
4, the guard method of substrate surface in the ion-exchange process according to claim 1 is characterized in that described protective material is K9 glass, K8 glass or silicate glass.
5, the guard method of substrate surface in the ion-exchange process according to claim 1 is characterized in that described film plating process is high-frequency sputtering, magnetron sputtering or thermal evaporation.
6, the guard method of substrate surface in the ion-exchange process according to claim 1 is characterized in that this method comprises following concrete steps:
1. phosphate glass or crystalline material are made needed workpiece through cutting, processing, polishing;
2. selected film plating process and corresponding apparatus;
3. selected protective material is made corresponding target;
4. the workpiece protective film coating to needing protection;
5. prepare fused salt, described workpiece is placed fused salt, under certain process conditions, carry out ion-exchange treatment;
6. take out the workpiece after the ion-exchange, clean its surperficial fused salt, obtain the sample after the ion-exchange treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610023418XA CN100359348C (en) | 2006-01-18 | 2006-01-18 | Substrate surface protection method for ion exchange process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610023418XA CN100359348C (en) | 2006-01-18 | 2006-01-18 | Substrate surface protection method for ion exchange process |
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| Publication Number | Publication Date |
|---|---|
| CN1800893A CN1800893A (en) | 2006-07-12 |
| CN100359348C true CN100359348C (en) | 2008-01-02 |
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| CNB200610023418XA Expired - Fee Related CN100359348C (en) | 2006-01-18 | 2006-01-18 | Substrate surface protection method for ion exchange process |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101907739B (en) * | 2010-07-30 | 2011-10-12 | 西南科技大学 | Additional electric field-assisted ion exchange device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6381392B1 (en) * | 1999-01-27 | 2002-04-30 | The United States Of America As Represented By The Secretary Of Commerce | Ion exchange technology for fabrication of waveguide source lasers |
| CN1357950A (en) * | 2001-04-03 | 2002-07-10 | 中国科学院长春光学精密机械与物理研究所 | Prepn of fluozirconate glass waveguide for blue-green laser |
| CN1553236A (en) * | 2003-12-19 | 2004-12-08 | 上海交通大学 | Manufacture of erbium dosed phosphate two step ion exchange optical waveguide |
| US20050115491A1 (en) * | 1998-05-11 | 2005-06-02 | California Institute Of Technology, A California Non-Profit Corporation. | Ion exchange waveguides and methods fabrication |
-
2006
- 2006-01-18 CN CNB200610023418XA patent/CN100359348C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050115491A1 (en) * | 1998-05-11 | 2005-06-02 | California Institute Of Technology, A California Non-Profit Corporation. | Ion exchange waveguides and methods fabrication |
| US6381392B1 (en) * | 1999-01-27 | 2002-04-30 | The United States Of America As Represented By The Secretary Of Commerce | Ion exchange technology for fabrication of waveguide source lasers |
| CN1357950A (en) * | 2001-04-03 | 2002-07-10 | 中国科学院长春光学精密机械与物理研究所 | Prepn of fluozirconate glass waveguide for blue-green laser |
| CN1553236A (en) * | 2003-12-19 | 2004-12-08 | 上海交通大学 | Manufacture of erbium dosed phosphate two step ion exchange optical waveguide |
Non-Patent Citations (1)
| Title |
|---|
| Ag＋-Na＋离子交换波导的折射率分布分析. 刘晓山，付国兰，刘三秋，桑明煌.江西师范大学学报（自然科学版），第28卷第4期. 2004 * |
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| CN1800893A (en) | 2006-07-12 |
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