CN100359348C - The protection method of substrate surface in ion exchange process - Google Patents
The protection method of substrate surface in ion exchange process Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- substrate
- ion exchange
- ion
- glass
- exchange process
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000005342 ion exchange Methods 0.000 title claims abstract description 48
- 239000000758 substrate Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000011521 glass Substances 0.000 claims abstract description 32
- 150000003839 salts Chemical class 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 12
- 150000002500 ions Chemical class 0.000 claims abstract description 11
- 230000000694 effects Effects 0.000 claims abstract description 8
- 238000005260 corrosion Methods 0.000 claims abstract 4
- 239000005365 phosphate glass Substances 0.000 claims description 13
- 230000001681 protective effect Effects 0.000 claims description 13
- 239000010408 film Substances 0.000 claims description 12
- 238000004544 sputter deposition Methods 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 230000003628 erosive effect Effects 0.000 claims description 4
- 239000005368 silicate glass Substances 0.000 claims description 4
- 239000010409 thin film Substances 0.000 claims description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract 2
- 230000003287 optical effect Effects 0.000 description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000002178 crystalline material Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000011253 protective coating Substances 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 229920002120 photoresistant polymer Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001039 wet etching Methods 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000087 laser glass Substances 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Images
Landscapes
- Surface Treatment Of Glass (AREA)
Abstract
A method for protecting the surface of substrate in ion exchange technology features that a glass material containing exchangeable ions same as the substrate and having the ability to resist the corrosion of molten salt is used to deposit on the surface of substrate by filming method, so preventing the corrosion of molten salt in ion exchange process. The method for protecting the surface of the substrate in the ion exchange process has the advantages of low material cost, simple and 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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610023418XA CN100359348C (en) | 2006-01-18 | 2006-01-18 | The protection method of substrate surface in ion exchange process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610023418XA CN100359348C (en) | 2006-01-18 | 2006-01-18 | The protection method of substrate surface in ion exchange process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1800893A CN1800893A (en) | 2006-07-12 |
| CN100359348C true CN100359348C (en) | 2008-01-02 |
Family
ID=36811006
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200610023418XA Expired - Fee Related CN100359348C (en) | 2006-01-18 | 2006-01-18 | The protection method of substrate surface in ion exchange process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100359348C (en) |
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 | Erbium-doped phosphate two-step ion-exchange optical waveguide fabrication method |
| 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 | Erbium-doped phosphate two-step ion-exchange optical waveguide fabrication method |
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 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1800893A (en) | 2006-07-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI696592B (en) | Glass-based articles, method of manufacturing the same, and products comprising the same | |
| CN100412583C (en) | Method for preparing buried glass optical waveguide by single-sided molten salt electric field assisted ion exchange | |
| CN102645701B (en) | Method for producing optical waveguide on surface of glass substrate by utilizing ion exchange method | |
| TW202010720A (en) | Glass-ceramic articles with improved stress profiles | |
| US4913717A (en) | Method for fabricating buried waveguides | |
| JP2011032140A (en) | Method for producing ion exchange treatment glass, method for producing chemically strengthened glass and ion exchange treatment apparatus | |
| US5114453A (en) | Lightwave guide produced by ion exchange of cs+ ions | |
| CN100359348C (en) | The protection method of substrate surface in ion exchange process | |
| CN104556685B (en) | Alumina silicate glass and tempered glass | |
| CN100570419C (en) | A kind of optical waveguide containing Cu ions | |
| CN100392446C (en) | Method for making glass optical waveguide with ion mask | |
| JPS6252136A (en) | Manufacture of glass product | |
| CN112110645B (en) | Glass, glass product and manufacturing method thereof | |
| CN113388892A (en) | Method for preparing lead magnesium niobate titanate optical waveguide by titanium diffusion | |
| CN102193146A (en) | Method for manufacturing glass substrate all buried strip-type optical waveguide stack | |
| CN107643560A (en) | A kind of method that magneto-optic glass base ion exchange prepares magneto-optic slab guide | |
| WO2017221805A1 (en) | Reinforced glass production method and reinforced glass production apparatus | |
| CN112110644B (en) | Glass composition and chemically strengthened glass | |
| JPS60200842A (en) | Glass for transmitting ultraviolet rays | |
| CN102633434B (en) | Glass substrate material for integrated optics and preparation method of glass substrate material | |
| CN1553236A (en) | Erbium-doped phosphate two-step ion-exchange optical waveguide fabrication method | |
| Sakida et al. | Optical properties of Er3+-doped tungsten tellurite glass waveguides by Ag+–Na+ ion-exchange | |
| CN114341076A (en) | Ion exchange process for ultrathin glass | |
| Rehouma et al. | Glasses for ion-exchange technology | |
| CN111158084A (en) | Manufacturing method of ion-exchange glass-based surface waveguide spot size converter |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080102 Termination date: 20130118 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |