CN100412583C - Method for preparing glass waveguide by single-side molten salt electric field assistant ion exchange - Google Patents
Method for preparing glass waveguide by single-side molten salt electric field assistant ion exchange Download PDFInfo
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- CN100412583C CN100412583C CNB2006100506184A CN200610050618A CN100412583C CN 100412583 C CN100412583 C CN 100412583C CN B2006100506184 A CNB2006100506184 A CN B2006100506184A CN 200610050618 A CN200610050618 A CN 200610050618A CN 100412583 C CN100412583 C CN 100412583C
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- glass
- electric field
- glass substrate
- molten salt
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Abstract
The present invention discloses a method for preparing buried type glass optical waveguide by a single-side molten salt electric field assisting ion exchange. Firstly, a glass basic piece with a mask carries out ion exchange in molten salt with high polarized rate to attain an ion exchange area on the surface of the glass. Then, a baffle layer is prepared in a region on the surface of the glass basic piece, wherein the region is far away from the core part of optical waveguide, for preventing large numbers of ions from passing through the glass basic piece to damage a metal film electrode when a cathode is reduced in the latter ion exchange processes. Finally, an anode takes the molten salt without high polarized ions; the cathode takes a metal film and takes the single-side molten salt electric field to assist ion exchange for preparing the buried type optical waveguide. The method of the present invention can effectively restrain the hurt of the cathode metal film in the process that the electric field assists ion exchange, and can improve the performance of glass optical waveguide devices prepared by the single-side molten salt electric field assisting ion exchange.
Description
Technical field
The present invention relates to optical device, integrated optics field, relate in particular to the method that a kind of single-side molten salt electric field assisting ion exchange prepares glass waveguide.
Background technology
1969, S.E.Miller proposed the notion of integrated optics, and its basic thought is on the surface of same substrate, with the slightly high material optical waveguide of refractive index, and made various devices such as light source, grating based on this again.By this integrated, can realize the purpose of miniaturization, lightweight, stabilization and the high performance of optical system.
As the important integrated optical device of a class, the optical device that adopts ion exchange process to make on glass substrate is subjected to business circles and researchers' attention always.From the beginning seventies in last century, various countries research institution drops into a large amount of manpower and financial resources and carries out the exploitation of glass-based integrated optical device.Reason is that this device has some excellent character, and comprising: loss is low, is easy to the rare earth ion of doped with high concentration, and with the optical characteristics of optical fiber coupling, coupling loss is little, and environmental stability is good, is easy to integrated, with low cost or the like.At present, the integrated optical device on some glass substrates has been realized scale and seriation, and is successfully used to optical communication and light sensing network.
Normally used ion-exchange process (as shown in Figure 1) is to make the mask 2 that stops ions diffusion on glass substrate 1 surface (normally thickness is metal materials such as Al, the Ag of the micron or the sub-micron order of magnitude, Ti, Ni, Cr-Au, perhaps SiO
2Deng dielectric substance), and on mask, form the diffusion window, the glass substrate 1 that then will have a mask 2 is put into and is contained high polarization ion (K normally
+, Ag
+, Li
+, Rb
+, Cs
+, Cu
+, Tl
+Deng) fused salt 3 in carry out ion-exchange, diffusion window that the high polarization ion in the fused salt forms by mask 2 and the hypopolarization rate ion in the glass substrate 1 (Na normally
+) exchange, the high polarization ion enters the ion diffusion region 4 that glass substrate 1 forms glass surface, as the sandwich layer of surface light waveguide.In general, owing to the sideways diffusion at optical waveguide manufacturing process intermediate ion, the ion diffusion region 4 of glass surface is flat, thereby makes its mould field distribution asymmetric, and the coupling loss of optical waveguide and single-mode fiber is very big; On the other hand, the ion diffusion region 4 of glass surface is positioned at the surface of glass substrate, and optical guided wave will be introduced very high loss in the scattering of glass surface.
The optical waveguide of making buried type can be improved the symmetry of optical waveguide sandwich layer index distribution, and and then improve the symmetry of light wave guided mode field distribution, reduce fiber waveguide device and with the coupling loss of optical fiber.Simultaneously, the core of optical waveguide is imbedded below the glass surface, made optical guided wave not produce scattering, reduce the loss of device at glass surface.The mode of the auxiliary secondary ion exchange of electric field is adopted in the making of buried type optical waveguide usually.As shown in Figure 2, to the glass substrate after the primary ions exchange
Carry out the ion-exchange second time, do not contain in the fused salt 5 of high polarization ion in the glass substrate both sides, insert contact conductor 6 respectively, apply Dc bias between positive electrode and the negative electrode, under the effect of this Dc bias, the ion diffusion region 4 of the glass surface that ion-exchange for the first time forms is pushed into glass substrate, forms the ion-exchange area 7 of buried type.But the auxiliary secondary ion exchange of this electric field needs more complicated experimental facilities, and is also harsher to the requirement of the process conditions of ion-exchange, not only increased the element manufacturing cost, and reduced the production efficiency of device.
The method of another kind of electric field Assisted Preparation buried type optical waveguide is the side fused salt 5 that does not contain the high polarization ion at glass substrate, and the opposite side employing is produced on the metal film 8 of glass surface as electrode, as shown in Figure 3, this method needs simple equipment just can make the buried type optical waveguide.But in actual mechanical process, there is certain problem in this technology, along with the carrying out of ion exchange process, a large amount of monoacidic base metal (Na is arranged
+Deng) on negative electrode metal film 8, be reduced into the very active alkaline metal of chemical property, and generate basic anhydride with airborne oxygen reaction immediately, metal film 8 is caused corrosion, and metal film 8 is come off from glass substrate 1 surface, ion-exchange can't normally be carried out.
Summary of the invention
The object of the present invention is to provide a kind of single-side molten salt electric field assisting ion exchange to prepare the method for glass waveguide, improve single-side molten salt electric field assisting ion exchange process, make glass optical waveguide.
The technical solution adopted for the present invention to solve the technical problems is:
Adopt a step ion-exchange to make the surface light waveguide, adopt the microfabrication means to make mask at the upper surface of glass substrate, and making ions diffusion window, the glass substrate that then will have a mask is put into the fused salt that contains the high polarization ion and is carried out ion-exchange, the window that high polarization ion in the fused salt forms by mask through the thermal diffusion effect forms the ion diffusion region of glass surface at the upper surface of glass substrate, forms the core of surface light waveguide; It is characterized in that:
The mask of the upper surface of glass substrate is removed with corrosive liquid, and adopted the microfabrication means to make the restraining barrier at the upper surface of glass substrate, the window width that the restraining barrier forms is greater than the width of the ion diffusion region of glass surface;
Lower surface at glass substrate is made metal film, electrode as the exchange of electric field assisting ion, use single-side molten salt ion-exchange then, make electrode at the glass substrate upper surface with the fused salt that does not contain the high polarization ion, upper and lower surface at glass substrate applies Dc bias, carries out the exchange of electric field assisting ion, under the effect of Dc bias, the ion diffusion region of the glass surface that ion-exchange forms is pushed into glass substrate, forms the ion diffusion region of buried type.
Described glass substrate is the silicate glass of the doping with rare-earth ions or the rare earth ion that undopes, phosphate glass or borate glass.
Described mask material is Al, Ag, Ti, Ni, Cr-Au or SiO
2
The contained high polarization ion of fused salt that contains the high polarization ion is: Tl
+, Ag
+, Li
+, Cs
+, Rb
+Or Cu
+
The contained negative ion of fused salt that contains the high polarization ion is: NO
3 -, CO
3 2-, SO
4 2-Or Cl
-
The restraining barrier that the buried type optical waveguides is made in the exchange of electric field assisting ion is Al, Ag, Ti, Ni, Cr-Au or SiO
2
The electrode metal film that single-side molten salt electric field assisting ion clearing house is used is Al, Ag, Ti, Ni or Cr-Au.
The present invention compares with common single-side molten salt electric field assisting ion exchange process, the beneficial effect that has is: in carrying out electric field assisting ion exchange making buried type optical waveguide process, the surface of glass substrate has made one deck restraining barrier, be used to stop a large amount of ions to pass through glass substrate, prevent that a large amount of metallic ions are reduced at negative electrode and destroy metal film as electrode, thereby reduced damage significantly to metal film, guaranteed ion-exchange continue carry out.
Description of drawings
Fig. 1 is the synoptic diagram that ion exchange process prepares surperficial strip optical waveguide.
Fig. 2 is that the synoptic diagram of buried type optical waveguide is made in the exchange of bilateral molten salt electric field assisting ion.
Fig. 3 is that the synoptic diagram of buried type optical waveguide is made in the exchange of single-side molten salt electric field assisting ion.
Fig. 4 is the barrier layer structure synoptic diagram, and wherein A is a sectional view, and B is a vertical view.
Fig. 5 is the synoptic diagram of single-side molten salt electric field assisting ion exchange preparation glass waveguide of the present invention.
Among the figure: 1. glass substrate, 2. mask 3. contains the fused salt of high polarization ion, and the 4. ion diffusion region of glass surface does not 5. contain the fused salt of high polarization ion, 6. contact conductor, the 7. ion-exchange area of buried type, 8. metal film, 9. restraining barrier.
Embodiment
The implementation step of improving one's methods that single-side molten salt electric field assisting ion exchange process involved in the present invention prepares optical waveguide is as follows:
(1) adopt first step ion-exchange to make the surface light waveguide.With reference to shown in Figure 1, (normally thickness is metal materials such as Al, the Ag of the micron or the sub-micron order of magnitude, Ti, Ni, Cr-Au, perhaps SiO to adopt conventional microfabrication means (comprising depositing operations such as evaporation or sputter, photoetching and corrosion) to make mask 2 on the surface of glass substrate 1
2Deng dielectric substance), and the window of making ion-exchange on mask 2; The glass substrate 1 that then will have a mask 2 is put into the fused salt 3 that contains the high polarization ion and is carried out ion-exchange, ion-exchange temperature is decided according to selected fused salt composition and glass substrate, generally between 280~450 ℃, ion-exchange time is determined according to designing requirement, between 5 minutes to 24 hours; High index of refraction ion in the fused salt acts on the ion diffusion region 4 that forms glass surface in the glass substrate 1 through thermal diffusion, forms the core of surface light waveguide.
(2) mask 2 on glass substrate 1 surface is removed, and (thickness is metal materials such as Al, the Ag of the micron or the sub-micron order of magnitude, Ti, Ni, Cr-Au, perhaps SiO to adopt microfabrication means (comprising depositing operations such as evaporation or sputter, photoetching and corrosion) to make restraining barrier 9 on the surface of glass substrate 1
2Deng dielectric substance), and on the restraining barrier, form the diffusion window, window width is greater than the width of the ion diffusion region 4 of glass surface.Shown in Figure 4 is the structural representation on restraining barrier 9, and wherein A is a sectional view, and B is a vertical view.
(3) adopt the auxiliary technology of burying of electric field to prepare the buried type optical waveguide.Employing is made metal film 8 on another surface of glass substrate, as the electrode of electric field assisting ion exchange.Then with technology like the common single-side molten salt ion exchange phase, with reference to shown in Figure 5, make electrode with the fused salt 6 that does not contain the high polarization ion in the one side that is manufactured with the surface light waveguide; With the fused salt heat fused, between 280~400 ℃, both sides at glass substrate 1 apply Dc bias, carry out the exchange of electric field assisting ion, under the effect of Dc bias, the ion diffusion region 4 of the glass surface that ion-exchange for the first time forms is pushed into glass substrate, forms the ion-exchange area 7 of buried type, determines according to required burying depth diffusion time.
Embodiment 1: adopt low temperature diffusion technology to make the buried type waveguide.
(1) is being mixed with rare earth ion Er
3+And Yb
3+Upper surface evaporation (perhaps sputter) layer thickness of phosphate glass substrate be the Al of 80~200nm, on flooding, produce the bar shaped diffusion window that width is 4~12 μ m by photoetching and wet corrosion technique;
(2) glass substrate that then will have mask is put into an AgNO
3With NaNO
3And KNO
3Fused salt mixt in carry out ion-exchange, 280 ℃ of ion-exchange temperatures, ion-exchange time is 30 minutes, the Ag in the fused salt
+Act on the ion diffusion region 4 that forms glass surface in the glass substrate 1 through thermal diffusion, form the core of surface light waveguide;
(3) the Al film with glass substrate surface adopts H
3PO
4Corrosive liquid is removed;
(4) surface evaporation (perhaps sputter) layer thickness at glass substrate is the Al of 80~200nm, produces the bar shaped diffusion window that width is 20~50 μ m by photoetching and wet corrosion technique on flooding;
(5) adopt evaporation (perhaps sputter) technology to make metal A g film, as the electrode of electric field assisting ion exchange at the lower surface of glass substrate.Glass sheet upper surface NaNO
3And KNO
3Fused salt mixt make electrode; With the fused salt heat fused, and be warming up to 280 ℃ of maintenances, apply Dc bias, keep current density 0.2~4mA/cm by glass substrate in the both sides of glass substrate 1
2, carry out the exchange of electric field assisting ion, under the effect of Dc bias, the ion diffusion region of the glass surface that ion-exchange for the first time forms is pushed into glass substrate, forms the ion-exchange area of buried type, 1.5 hours diffusion times.
(6) 270 ℃ are incubated 10 hours down glass substrate are annealed.
Embodiment 2: warm diffusion technique is made the buried type waveguide in the employing.
(1) upper surface evaporation (perhaps sputter) layer thickness at the borate glass substrate is the Gr-Au of 80~200nm, produces the bar shaped diffusion window that width is 4~12 μ m by photoetching and wet corrosion technique on flooding;
(2) glass substrate that then will have mask is put into an AgNO
3With NaNO
3And KNO
3Fused salt mixt in carry out ion-exchange, 340 ℃ of ion-exchange temperatures, ion-exchange time is 10 minutes, the Ag in the fused salt
+Act on the ion diffusion region that forms glass surface in the glass substrate through thermal diffusion, form the core of surface light waveguide;
(3) the Gr-Au film with glass substrate surface adopts the standard Gr-Au corrosive liquid of microelectronic technique special use to remove;
(4) surface evaporation (perhaps sputter) layer thickness at glass substrate is the Al of 80~200nm, produces the bar shaped diffusion window that width is 20~50 μ m by photoetching and wet corrosion technique on flooding;
(5) adopt evaporation (perhaps sputter) technology to make metal A g film, as the electrode of electric field assisting ion exchange at the lower surface of glass substrate.Glass sheet upper surface NaNO
3And KNO
3Fused salt mixt make electrode; With the fused salt heat fused, and be warming up to 320 ℃ of maintenances, apply Dc bias, keep current density 0.2~4mA/cm by glass substrate in the both sides of glass substrate 1
2, carry out the exchange of electric field assisting ion, under the effect of Dc bias, the ion diffusion region of the glass surface that ion-exchange for the first time forms is pushed into glass substrate, forms the ion-exchange area of buried type, 1 hour diffusion time.
Embodiment 3: adopt High temperature diffusion technology to make the buried type waveguide.
(1) upper surface evaporation (perhaps sputter) layer thickness at the silicate glass substrate is the Ag of 80~200nm, produces the bar shaped diffusion window that width is 4~12 μ m by photoetching and wet corrosion technique on flooding;
(2) glass substrate that then will have mask is put into an AgNO
3With NaNO
3And KNO
3Fused salt mixt in carry out ion-exchange, 450 ℃ of ion-exchange temperatures, ion-exchange time is 3 minutes, the Ag in the fused salt
+Act on the ion diffusion region that forms glass surface in the glass substrate through thermal diffusion, form the core of surface light waveguide;
(3) the Ag film with glass substrate surface adopts the standard A g corrosive liquid of microelectronic technique special use to remove;
(4) surface evaporation (perhaps sputter) layer thickness at glass substrate is the Al of 80~200nm, produces the bar shaped diffusion window that width is 20~50 μ m by photoetching and wet corrosion technique on flooding;
(5) adopt evaporation (perhaps sputter) technology to make metal A g film, as the electrode of electric field assisting ion exchange at the lower surface of glass substrate.Glass sheet upper surface NaNO
3And KNO
3Fused salt mixt make electrode; With the fused salt heat fused, and be warming up to 400 ℃ of maintenances, apply Dc bias, keep current density 0.2~4mA/cm by glass substrate in the both sides of glass substrate 1
2, carry out the exchange of electric field assisting ion, under the effect of Dc bias, the ion diffusion region of the glass surface that ion-exchange for the first time forms is pushed into glass substrate, forms the ion-exchange area of buried type, 0.5 hour diffusion time.
Claims (7)
1. a single-side molten salt electric field assisting ion exchanges the method for preparing glass waveguide, adopt a step ion-exchange to make the surface light waveguide, adopt the microfabrication means to make mask (2) at the upper surface of glass substrate (1), and making ions diffusion window, the glass substrate (1) that then will have mask (2) is put into the fused salt (3) that contains the high polarization ion and is carried out ion-exchange, high polarization ion in the fused salt passes through the ion diffusion region (4) of the window of mask (2) formation at the upper surface formation glass surface of glass substrate (1) through the thermal diffusion effect, form the core of surface light waveguide; It is characterized in that:
The mask (2) of the upper surface of glass substrate (1) is removed with corrosive liquid, and adopted the microfabrication means to make restraining barrier (9) at the upper surface of glass substrate (1), the window width that the restraining barrier forms is greater than the width of the ion diffusion region (4) of glass surface;
Lower surface at glass substrate (1) is made metal film (8), electrode as the exchange of electric field assisting ion, use single-side molten salt ion-exchange then, make electrode at glass substrate (1) upper surface with the fused salt (5) that does not contain the high polarization ion, upper and lower surface at glass substrate (1) applies Dc bias, carry out the exchange of electric field assisting ion, under the effect of Dc bias, the ion diffusion region (4) of the glass surface that ion-exchange forms is pushed into glass substrate, forms the ion diffusion region (7) of buried type.
2. a kind of single-side molten salt electric field assisting ion exchange according to claim 1 prepares the method for glass waveguide, it is characterized in that: described glass substrate (1) is the silicate glass of the doping with rare-earth ions or the rare earth ion that undopes, phosphate glass or borate glass.
3. a kind of single-side molten salt electric field assisting ion exchange according to claim 1 prepares the method for glass waveguide, and it is characterized in that: described mask (2) material is Al, Ag, Ti, Ni, Cr-Au or SiO
2
4. a kind of single-side molten salt electric field assisting ion exchange according to claim 1 prepares the method for glass waveguide, and it is characterized in that: the contained high polarization ion of fused salt (3) that contains the high polarization ion is: Tl
+, Ag
+, Li
+, Cs
+, Rb
+Or Cu
+
5. a kind of single-side molten salt electric field assisting ion exchange according to claim 1 prepares the method for glass waveguide, and it is characterized in that: the contained negative ion of fused salt (3) that contains the high polarization ion is: NO
3 -, CO
3 2-, SO
4 2-Or Cl
-
6. a kind of single-side molten salt electric field assisting ion exchange according to claim 1 prepares the method for glass waveguide, it is characterized in that: the restraining barrier (9) that the buried type optical waveguides is made in the exchange of electric field assisting ion is Al, Ag, Ti, Ni, Cr-Au or SiO
2
7. a kind of single-side molten salt electric field assisting ion exchange according to claim 1 prepares the method for glass waveguide, and it is characterized in that: the electrode metal film (8) that single-side molten salt electric field assisting ion clearing house is used is Al, Ag, Ti, Ni or Cr-Au.
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Families Citing this family (12)
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CN101907739B (en) * | 2010-07-30 | 2011-10-12 | 西南科技大学 | Additional electric field-assisted ion exchange device |
CN102732930A (en) * | 2011-04-14 | 2012-10-17 | 上海光芯集成光学股份有限公司 | Method for making glass base ion exchange waveguides |
CN102662211B (en) * | 2012-05-24 | 2015-01-07 | 上海光芯集成光学股份有限公司 | Method and device for monitoring field assisted optical waveguide burying process |
CN103496848B (en) * | 2013-09-16 | 2016-01-06 | 大连工业大学 | A kind of praseodymium doped phosphate glass and prepare the method for waveguide |
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CN111699424A (en) * | 2018-01-18 | 2020-09-22 | 康宁公司 | Low loss waveguide formed in high transmission glass using Ag-Na ion exchange |
CN108828718A (en) * | 2018-06-15 | 2018-11-16 | 深圳市慧康精密仪器有限公司 | A method of improving glass based optical waveguide chip uniformity |
CN111208607A (en) * | 2020-02-09 | 2020-05-29 | 浙江大学深圳研究院 | Method for manufacturing glass-based spot-size converter by grooved hot plate temperature gradient ion diffusion |
CN111239898A (en) * | 2020-02-09 | 2020-06-05 | 浙江大学深圳研究院 | Method for manufacturing glass-based buried type spot-size converter by grooved hot plate temperature gradient ion diffusion |
CN113391397B (en) * | 2021-06-08 | 2023-05-30 | 浙江大学绍兴微电子研究中心 | Method for improving core symmetry of glass-based optical waveguide by adopting external barrier layer |
CN113391396B (en) * | 2021-06-08 | 2023-09-19 | 浙江大学绍兴微电子研究中心 | Method for improving core symmetry of glass-based optical waveguide by adopting inner barrier layer |
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