CN1553236A - Manufacture of erbium dosed phosphate two step ion exchange optical waveguide - Google Patents
Manufacture of erbium dosed phosphate two step ion exchange optical waveguide Download PDFInfo
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- CN1553236A CN1553236A CNA2003101227368A CN200310122736A CN1553236A CN 1553236 A CN1553236 A CN 1553236A CN A2003101227368 A CNA2003101227368 A CN A2003101227368A CN 200310122736 A CN200310122736 A CN 200310122736A CN 1553236 A CN1553236 A CN 1553236A
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Abstract
A preparing method includes the following steps: 1) ion exchange fused salt is prepared, 2) mask drawing of backing sample is prepared, 3) twice of ion exchanging is carried out, 4) annealing, 5) mask layer is removed and 6) end face is polished. The fused salt is compound material of sodium nitrate, potassium nitrate and silver nitrate as number one salt bath for the first exchange is contained by wt. with silver nitrate of 5-10% and potassium nitrate of 90-95% as well as number two for the second exchange is contained by wt. with potassium nitrate of 0-10% and sodium nitrate of 90-100%.
Description
Technical field
What the present invention relates to is a kind of ion exchange optical waveguide method for making, and particularly a kind of is two step of er-doped phosphate ion exchange optical waveguide method for making.Belong to optical communication field.
Background technology
Image intensifer is an important devices in optical communication and the optical information processing system.The er doped silica glasses orthoron has that volume is little, stable and reliable for performance, efficient is high, low in energy consumption, advantage such as easy to use.But the loss of ion exchange optical waveguide is big, Polarization Dependent Loss (PDL) is big, it is one of key factor of restriction fiber waveguide device tremendous development always, now common ion-exchange is made the method for glass optical waveguide and is mostly only done once exchange, wherein the bar waveguide loss of making of high quality optical BK7 glass is 0.21dB/cm, prepared light guide surface optical quality instability, maximum shortcoming is that the waveguide region xsect is half elliptic, its Polarization Dependent Loss is bigger, influenced the transport property of optical waveguide greatly, to such an extent as to glass light waveguide device press down for a long time foot not before.There are a few peoples to use the auxiliary ion of the electric field technology that distributes again, find Jitka by literature search
With Josef Schrofel at " optical communication ", 1998 the 156th volumes, " electric field is assisted K+-Na+ ionic exchange glass light waveguide structure " (the Optics Communications that delivers on the 384-391 page or leaf, " Integrated waveguide structures prepared in very pure glass byelectric field assisted K+-Na+ ion exchange " Vol.156 1998 384-391) mentioned in the literary composition electric field auxiliary down ion-exchange process, but its experimental provision complexity, be difficult to realize, be difficult to guarantee the stability of technology.In this field, so far not about the loss of erbium doped phosphate glass secondary ion exchange low transmission, the play-by-play and the relevant patent of low Polarization Dependent Loss optical waveguide.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of erbium doped phosphate glass ion exchange optical waveguide method for making is provided, utilize two step ion-exchange process to make optical waveguide, make it realize the low transmission loss of optical waveguide, the characteristic of low Polarization Dependent Loss by specific exchange and annealing process.
The present invention is achieved by the following technical solutions, and method may further comprise the steps: the 1) preparation of ion-exchange fused salt; 2) preparation of substrate sample mask pattern; 3) twice ion-exchange; 4) annealing; 5) remove mask layer; 6) end face polishing.
Below the inventive method is further described, particular content is as follows:
1) preparation of ion-exchange fused salt
The component of fused salt has very big influence to the ion-exchange result, and the used ion-exchange fused salt of the inventive method is the potpourri of silver nitrate, sodium nitrate, potassium nitrate, and its percentage by weight compositing range is:
A salt bath: once silver nitrate 5～10%, potassium nitrate 90～95% are used in exchange;
No. two salt baths: potassium nitrate 0～10%, sodium nitrate 90～100% are used in the secondary exchange;
Will fully stir after salt mixes makes it even.
2) preparation of substrate sample mask pattern
The inventive method aluminium is as the mask of ion-exchange, forming thickness with the method for the ion sputtering of routine on surface of erbium doped phosphate glass sheet sample is 1000～2000 dust aluminium masks, open one group of marking shape window with conventional lithography corrosion technology on mask again, width is respectively 5.0,5.5,6.0,6.5,7.0 microns.
3) twice ion-exchange
Salt and step 2 with step 1) preparation) sample of preparation all puts into constant temperature oven, be preheated to once exchange temperature required after, sample is immersed in salt bath, take out behind the exchange certain hour; It is temperature required furnace temperature to be adjusted to the secondary exchange rapidly again, sample is immersed in No. two salt baths then and carries out the secondary ion exchange, takes out behind the exchange certain hour.Sample is in the furnace chamber all the time in all above operating process, avoids the sample suddenly cold and hot.Once exchange 330～340 degrees centigrade of temperature, 90～120 minutes reaction time; 310～330 degrees centigrade of secondary exchange temperature, 20～30 minutes reaction time.
4) annealing
After step 3) was finished, sample took out from fused salt and does not leave furnace chamber, then furnace temperature is risen to 340～350 degrees centigrade, with 345 degrees centigrade is good, kept 10～20 minutes, the shut-off circuit power supply takes out sample after making its natural cooling under the situation that fire door is closed then.
5) remove mask layer
To immerse clear a moment in the hot phosphoric acid through the sample of step 4), and see after the aluminium film comes off and take out, clean with deionized water.
6) end face polishing
Method with common mechanical lapping is polished the sample both ends of the surface, obtains optical waveguide.
The inventive method is compared with the method for general ion-exchange making glass optical waveguide following beneficial effect: through two specific step ion-exchange and annealing processs, make being distributed symmetrically property of fiber waveguide refractive index better, Polarization Dependent Loss is lower than 0.2～0.3dB, and transmission loss of optical waveguide is lower than 0.7～1.2dB/cm; Two step ion-exchanges and annealing are carried out continuously, and process cycle is short, good stability; The inventive method not only is applicable to erbium doped phosphate glass, and other similar glass materials are suitable for too.
Description of drawings
Fig. 1 is the inventive method process flow diagram
Embodiment
As shown in Figure 1, the present invention includes following steps: the 1) preparation of ion-exchange fused salt; 2) preparation of substrate sample mask pattern; 3) twice ion-exchange; 4) annealing; 5) remove mask layer; 6) end face polishing.
Provide embodiment below in conjunction with method of the present invention, technical solution of the present invention is done further to understand.
Embodiment 1
Salt bath: 10% silver nitrate, 90% potassium nitrate; No. two salt baths: 10% potassium nitrate, 90% sodium nitrate, mask thicknesses 1200 dusts.Salt and sample inserted to be preheated in the constant temperature oven once exchange 330 degrees centigrade of temperature, sample is immersed a salt bath reaction to be taken out in 120 minutes, furnace temperature is stable at 310 degrees centigrade of secondary exchange temperature after about 5 minutes, sample is immersed No. two salt bath reactions to be taken out in 30 minutes, furnace temperature is adjusted to 340 degrees centigrade then, kept 20 minutes, powered-down takes out sample after making its natural cooling.Sample is cleaned polishing at last dissolve away the aluminium film on surface with hot phosphoric acid after.The gained result, 6.5 microns width waveguide: loss 1.2dB/cm, PDL＜0.3dB; 6 microns width waveguide, loss 0.70dB/cm, PDL＜0.3dB.The waveguide of all the other width is owing to damage and can't measure in the technological process.
Embodiment 2
Salt bath: 8% silver nitrate, 92% potassium nitrate; No. two salt baths: 100% sodium nitrate.Once exchange 335 degrees centigrade of temperature, the reaction time is 100 minutes; 320 degrees centigrade of secondary exchange temperature, 25 minutes reaction time, 345 degrees centigrade of annealing temperatures, other are with embodiment 1, gained result: 7.0 microns width waveguide: loss 0.57dB/cm, PDL＜0.2dB; 6 microns width waveguide, loss 0.72dB/cm, PDL＜0.2dB.
Embodiment 3
No. two salt baths: 5% potassium nitrate, 95% sodium nitrate, mask thicknesses 1500 dusts once exchange 340 degrees centigrade of temperature, and the reaction time is 90 minutes; 325 degrees centigrade of secondary exchange temperature, in 20 minutes reaction time, all the other are with embodiment 1, gained result: 7.0 microns width waveguide: loss 1.1dB/cm, PDL＜0.2dB; 6 microns width waveguide, loss 0.83dB/cm, PDL＜0.2dB.
Embodiment 4
Salt bath: 5% silver nitrate, 95% potassium nitrate; No. two salt baths: 100% sodium nitrate, film thickness 2000 dusts once exchange 333 degrees centigrade of temperature, and the reaction time is 100 minutes; 318 degrees centigrade of secondary exchange temperature, in 25 minutes reaction time, all the other are with embodiment 1, gained result: 7.0 microns width waveguide: loss 0.54dB/cm, PDL＜0.2dB; 6.5 the micron width waveguide, loss 0.65dB/cm, PDL＜0.2dB; 6 microns width waveguide, loss 0.71dB/cm, PDL＜0.3dB.
Claims (4)
1, a kind of two step of er-doped phosphate ion exchange optical waveguide method for making is characterized in that, comprises the steps:
1) preparation of ion-exchange fused salt, the 2) preparation of substrate sample mask pattern, 3) twice ion-exchange, 4) annealing, 5) remove mask layer, 6) the end face polishing, wherein
Described ion-exchange fused salt is the potpourri of silver nitrate, sodium nitrate, potassium nitrate, and its percentage by weight compositing range is: a salt bath: once silver nitrate 5～10%, potassium nitrate 90～95% are used in exchange; No. two salt baths: potassium nitrate 0～10%, sodium nitrate 90～100% are used in the secondary exchange.
2, two step of er-doped phosphate ion exchange optical waveguide method for making as claimed in claim 1 is characterized in that, twice ion-exchange of described step 3) is specific as follows:
Salt and step 2 with step 1) preparation) sample of preparation all puts into constant temperature oven, be preheated to once exchange temperature required after, in salt bath of sample immersion, take out the exchange back, it is temperature required furnace temperature to be adjusted to the secondary exchange rapidly again, sample is immersed in No. two salt baths then and carries out the secondary ion exchange, and take out the exchange back, sample is in the furnace chamber all the time in all above operating process, avoids the sample suddenly cold and hot.
4, two step of er-doped phosphate ion exchange optical waveguide method for making as claimed in claim 3, it is characterized in that once exchanging temperature is 330～340 degrees centigrade, the reaction time is 90～120 minutes, secondary exchange temperature is 310～330 degrees centigrade, reacts to be 20～30 minutes time.
5, two step of er-doped phosphate ion exchange optical waveguide method for making as claimed in claim 1 is characterized in that, described step 4) annealing is specific as follows:
Annealing process is right after after step 3) carries out, and sample takes out from fused salt, and furnace temperature rises to 340～350 degrees centigrade then, is good with 345 degrees centigrade, keeps 10～20 minutes, and the shut-off circuit power supply is taking out sample behind the natural cooling under the situation that fire door is closed then.
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| CN 200310122736 CN1252500C (en) | 2003-12-19 | 2003-12-19 | Manufacture of erbium dosed phosphate two step ion exchange optical waveguide |
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| CN 200310122736 CN1252500C (en) | 2003-12-19 | 2003-12-19 | Manufacture of erbium dosed phosphate two step ion exchange optical waveguide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100356216C (en) * | 2005-12-29 | 2007-12-19 | 天津大学 | Method of preparing long period bar wave guide optical grating on optical glass surface |
| CN100359348C (en) * | 2006-01-18 | 2008-01-02 | 中国科学院上海光学精密机械研究所 | Method for protecting substrate surface in ion exchange process |
| CN102645701A (en) * | 2012-05-04 | 2012-08-22 | 上海光芯集成光学股份有限公司 | Method for producing optical waveguide on surface of glass substrate by utilizing ion exchange method |
| CN105683118A (en) * | 2013-08-26 | 2016-06-15 | 康宁股份有限公司 | Methods for localized annealing of chemically strengthened glass |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10197732B2 (en) | 2016-08-26 | 2019-02-05 | Corning Optical Communications LLC | Methods for forming ion-exchanged waveguides in glass substrates |
-
2003
- 2003-12-19 CN CN 200310122736 patent/CN1252500C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100356216C (en) * | 2005-12-29 | 2007-12-19 | 天津大学 | Method of preparing long period bar wave guide optical grating on optical glass surface |
| CN100359348C (en) * | 2006-01-18 | 2008-01-02 | 中国科学院上海光学精密机械研究所 | Method for protecting substrate surface in ion exchange process |
| CN102645701A (en) * | 2012-05-04 | 2012-08-22 | 上海光芯集成光学股份有限公司 | Method for producing optical waveguide on surface of glass substrate by utilizing ion exchange method |
| CN105683118A (en) * | 2013-08-26 | 2016-06-15 | 康宁股份有限公司 | Methods for localized annealing of chemically strengthened glass |
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| CN1252500C (en) | 2006-04-19 |
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