CN105093406A - Lithium niobate optical waveguide and method for preparing near-stoichiometric lithium niobate optical waveguide by means of titanium diffusion and vapor transport equilibration (VTE) - Google Patents
Lithium niobate optical waveguide and method for preparing near-stoichiometric lithium niobate optical waveguide by means of titanium diffusion and vapor transport equilibration (VTE) Download PDFInfo
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Abstract
The invention relates to the technical field of optical devices and especially relates to a lithium niobate optical waveguide and a method for preparing the near-stoichiometric lithium niobate optical waveguide by means of titanium diffusion and VTE. The lithium niobate optical waveguide comprises a substrate and a waveguide layer arranged on the substrate. The substrate is made of a lithium niobate crystal. The waveguide layer is arranged on a +z surface of the lithium niobate crystal, the direction of a stripe waveguide is the y direction of the lithium niobate crystal. A photo-etching process is adopted for preparing the waveguide layer on the substrate. The prepared optical waveguide is good in performance, is low in loss and has a good effect on various kinds of optical researches; in addition, the lithium niobate crystal after the titanium diffusion process is subjected to a lithium-rich vapor transport equilibration process, and a near stoichiometric ratio (NS, [Li]/[Nb]>99%) is achieved. The near-stoichiometric lithium niobate crystal has more excellent advantages that the crystal defects are less, the optical uniformity is good, and higher electro-optic and non-linear effects are realized. The titanium diffusion optical waveguide has the advantages that the waveguide performance is good, the loss is relatively low, etc.
Description
Technical field
The present invention relates to photoelectric device technical field, particularly relate to a kind of lithium niobate fiber waveguide and prepare the method for near-stoichiometric ratio lithium niobate optical waveguide by titanium diffusion and VTE.
Background technology
Waveguide, is used to the electromagnetic structure of directional guide.Common waveguiding structure mainly contains parallel double conducting wire, coaxial cable, parallel flat waveguide, rectangular waveguide, circular waveguide, microstrip line, slab dielectric optical waveguide and optical fiber.From the angle of guide electromagnetic waves, they all can be divided into interior zone and perimeter, and electromagnetic wave is limited in interior zone and propagates (requiring in waveguide cross-section, meet transverse resonance principle).
Usually, waveguide specially refers to hollow metal waveguide and the surface wave guide of various shape, and the electromagnetic wave be transmitted is limited in metal tube by completely, also known as closed waveguide; The electromagnetic wave of guiding constrains in around waveguiding structure, also known as open waveguide by the latter.When radio wave frequency brings up to centimeter wave wave band and the millimeter wave band of 3000 megahertz to 300 gigahertz (GHZ)s, the use of coaxial cable is restricted and adopts metallic waveguide or other guide wave devices.The advantage of waveguide is that conductor losses and dielectric loss are little; Power capacity is large; There is no radiation loss; Structure is simple, is easy to manufacture.Electromagnetic field in waveguide can by the Boundary Condition for Solving of maxwell equation group in conjunction with waveguide, different from normal transmission line, can not transmit TEM mould in waveguide, there is serious dispersion phenomenon in electromagnetic wave in the air, and dispersion phenomenon illustrates that electromagnetic wave propagation speed is relevant with frequency.The feature of surface wave guide is outside border, have electromagnetic field to exist.Its communication mode is surface wave.At millimeter wave and submillimeter wave wave band, the size because of metallic waveguide is too little and loss is strengthened and manufactures difficulty.At this moment use surface wave guide, except having good transmission, major advantage is that structure is simple, makes easily, can have the planar structure that integrated circuit needs.
Lithium columbate crystal is the good multifunctional light electric material of a kind of thermal stability, chemical stability, has outstanding piezoelectricity, acousto-optic, electric light, ferroelectric, pyroelectricity, the performance such as non-linear.At present, with lithium columbate crystal be base photovalve optical communication modulator, laser modulator, optoisolator, laser frequency multiplier, etc. in obtain and apply widely.
Compared with same composition lithium columbate crystal, lithium niobate crysal with near stoichiometric ratio has numerous excellent properties: the anti-light of (1) crystal causes lesion capability more by force, approximately improves an order of magnitude.(2) matter crystal internal defect is few, and therefore crystal response speed can be faster, and its response time can foreshorten to tens to hundreds of millisecond.Method now for lithium niobate crysal with near stoichiometric ratio growth preparation mainly contains following several: mix flux growth metrhod, double crucible method and vapor transportation balancing method.
At present, the lithium columbate crystal adopting Czochralski grown is mostly the congruent crystal departing from its stoichiometric compositions, show as the disappearance of Li atom, by the Li/Nb ratio (Li/Nb) adding kali or change in lithium niobate melt in congruent melt, or by gas phase transportation balance (VTE) technology, crystal is processed etc., can change the Li/Nb ratio in lithium columbate crystal, thus the LN crystal of near stoichiometric proportion is prepared in growth.
The good lithium niobate crysal with near stoichiometric ratio of optical quality can be grown by mixing kali flux.But because kali can not enter in crystal substantially, the component of melt constantly can be grown up with crystal and changed, and causes the upper and lower component of crystal uneven.The lithium niobate crysal with near stoichiometric ratio component of double crucible method growth is relatively more even, and can grow large-sized crystal.But adopt the stoichiometric proportion raw material that need continue to insert equivalent in this way in the growth course of crystal, require to use automated packing system, technical equipment more complicated, common laboratory is difficult to realize.To obtain near stoichiometric proportion LN crystal different from first two method direct growth, and rich lithium VTE is with same composition lithium columbate crystal for starting material, obtain near stoichiometric proportion LN crystal by changing its component.Adopt the component of Lithia in the wafer of VTE fabrication techniques can reach mole fraction 50.0%, and component is relatively uniform.Compared with first two method, rich lithium VTE technical costs is minimum, has important researching value.Along with the research of the device of all-optical switch, periodically poled lithium niobate wavelength shifter is applied, VTE fabrication techniques lithium niobate crystal chip with near stoichiometric ratio is adopted to be subject to attracting attention of people.
Lithium niobate fiber waveguide can be divided into preparation method: titanium diffusion lithium niobate fiber waveguide, ion-exchange lithium niobate fiber waveguide and proton exchange lithium niobate fiber waveguide etc.Ion-exchange, proton-exchanged optical waveguide are because of optics unstable properties during high temperature, and application is restricted.Use titanium diffusion technique at the bottom of lithium niobate base on to make optical waveguide be unusual proven technique.People have done detailed theoretical research to titanium diffusion technique, find that titanium atom diffuses in crystal with the form substituted.Under the high temperature conditions, titanium atom can be diffused into lithium columbate crystal inside, and elasto-optical effect and electrooptical effect make the refractive index of titanium diffusion zone increase, thus forms the optical waveguide of gradually changed refractive index.
The fast development of integrated optics and optical communication technique requires more and more higher to wavelength shifter.The class device in the past made using other body materials such as lithium niobates as core parts can not meet current to optical device miniaturization, integrated requirement.Compared with congruent lithium columbate crystal, titanium diffusion near stoichiometric proportion optical waveguide has important research and using value.Use titanium to be diffused at the bottom of lithium niobate base and make the technology that optical waveguide has been comparative maturity, simple titanium diffused optical waveguide there will be local periodical poling on ducting layer surface, cause the uneven of waveguide depth and width, thus the structure of waveguide also can be uneven, cause the loss of waveguide too high, weak to the restriction ability of light.
Summary of the invention
The object of the invention is to the deficiency overcoming above-mentioned technology, and a kind of lithium niobate fiber waveguide is provided and prepares the method for near-stoichiometric ratio lithium niobate optical waveguide by titanium diffusion and VTE, optical waveguide function admirable, loss is little, can play good effect in various optical research.
The present invention for achieving the above object, by the following technical solutions:
A kind of lithium niobate fiber waveguide, is characterized in that: comprise substrate and be positioned at described suprabasil ducting layer, described substrate adopts lithium columbate crystal, and described ducting layer is positioned at the+z face of described lithium columbate crystal, and the direction of Luciola substriata is the y direction of lithium columbate crystal.
Preferably, what prepare ducting layer employing on the substrate is photoetching process.
Prepared a method for near-stoichiometric ratio lithium niobate optical waveguide by titanium diffusion and VTE, it is characterized in that: comprise the following steps:
Step one, preparation of samples, selecting is that to cut the thick same composition lithium columbate crystal of 0.5mm be original material to optical grade Z, uses precision gas cutting machine that lithium columbate crystal is cut into sample;
Step 2, photoetching, the first step, the sample cleaned up is put and toasts 10min on hot plate, temperature is 85 DEG C, then, carry out the coating of photoresist, use sol evenning machine on sample, apply one deck SPR6112B type photoresist and carry out even glue, the rotating speed of setting sol evenning machine is 3000r/min, time is 1min, below, at 85 DEG C, the sample of complete for spin coating photoresist baking 10min, second step, exposure, sample and mask plate are put on the operator's console of litho machine, adjust position, exposure 40s, wherein selected mask plate is be manufactured with the slab waveguide pattern of 7 μm, 3rd step, development, service property (quality) number percent is the sodium hydroxide solution of 0.5%, development time is 16s, after exposed portion photoresist dissolves, the pure washed with de-ionized water of rapid use is clean, then high-purity elevated pressure nitrogen air gun is used to be dried up by sample, 4th step, the wafer of development work will have been carried out, put and toast 10min on hot plate, temperature is 85 DEG C,
Step 3, titanizing, puts into sample the sputtering that d.c. sputtering machine carries out platinum/titanium metal thin film, is filled with argon gas during sputtering, make pressure maintain about 4Pa, form one deck titanium film at sample surfaces;
Step 4, peel off, acetone is used to peel off the sample having plated platinum/titanium metal thin film, utilize supersonic wave cleaning machine to wash plating titanium on a photoresist off, after having peeled off, use alcohol and high-purity deionized water to wafer cleaning, after having cleaned, use high-purity elevated pressure nitrogen air gun to be dried up by sample, after having peeled off, use step instrument to record the thickness of titanium metal film for 90nm.
Step 5, titanium metal film prediffusion, puts into high temperature furnace by sample, carries out the prediffusion of platinum/titanium metal thin film, and time and temperature are respectively 2h, 1060 DEG C, can ensure that titanium ion enters lithium columbate crystal inside like this.
Step 6, rich lithium VTE process, uses rich lithium VTE technical finesse to complete the sample of platinum/titanium metal thin film prediffusion, puts into by mole fraction sample than the Li being 68mol%:32mol%
2cO
3and Nb
2o
5in the rich lithium crucible that mixed-powder sinters into, add one deck platinum pad below sample, by crucible with after rich lithium powder sealing, put into box high-temperature energy-conservation stove, the operational process of box-type high-temperature furnace, by procedure auto-control, to sample at 1100 DEG C, processes 30h.
Step 7, the polishing of optical waveguide end face, successively carries out polishing with the burnishing powder of 20,7,1.5 μm and polishing fluid to the end face of optical waveguide.
Preferably, in described box-type high-temperature furnace, temperature controls to be divided into four-stage: a low temperature rapid heating condition, in 50min, by 25
oc rises to 400
oc; Two high temperature temperature-rise periods, 400
oc is heated to 1100
oc, used time 140min; Three is holding stages, 1100
o30h is maintained under C; Four temperature-fall periods, by 1100
oc is down to room temperature.
The invention has the beneficial effects as follows: compared with prior art, prepare the method that optical waveguide adopts titanium diffusion, prepared optical waveguide function admirable, loss is little, good effect can be played in various optical research, rich lithium vapor transportation Balance Treatment is adopted to the lithium columbate crystal after titanium diffusion, reaches near stoichiometric proportion (NS, [Li]/[Nb] >99%).Lithium niobate crysal with near stoichiometric ratio has a lot of more excellent performance: crystal defect is few, and optical homogeneity is good, has stronger electric light and nonlinear effect.Titanium diffused optical waveguide has waveguide function admirable, and the advantage such as loss is less, can be widely used in for radio art such as radio communication, radar, navigation.
Accompanying drawing explanation
Fig. 1 is workflow diagram of the present invention;
Fig. 2 rich lithium vapor transportation balanced structure schematic diagram;
Fig. 3 is structural representation of the present invention.
Embodiment
The specific embodiment of the present invention is described in detail below in conjunction with accompanying drawing and preferred embodiment.As shown in the figure, a kind of lithium niobate fiber waveguide, comprises substrate 2 and is positioned at described suprabasil ducting layer 1, and described substrate adopts lithium columbate crystal, and described ducting layer is positioned at the+z face of described lithium columbate crystal, bar ripple to direction be the y direction of lithium columbate crystal.According to Crystal Growth of Lithium Niobate technique, lithium columbate crystal is divided into three directions by coordinate system, the different in kind of crystal in different directions, this is the method that certain experiment adopts, object is conveniently described embodiment of the present invention, and the direction making Luciola substriata during Luciola substriata experimentally requires to decide.What prepare ducting layer employing on the substrate is photoetching process.
Prepared a method for near-stoichiometric ratio lithium niobate optical waveguide by titanium diffusion and VTE, comprise the following steps:
Step one, preparation of samples, selecting is that to cut the thick same composition lithium columbate crystal of 0.5mm be original material to optical grade Z, uses precision gas cutting machine that lithium columbate crystal 100 is cut into sample;
Step 2, photoetching, the first step, the sample cleaned up is put and toasts 10min on hot plate, temperature is 85 DEG C, then, carry out the coating of photoresist 101, use sol evenning machine on sample, apply one deck SPR6112B type photoresist and carry out even glue 110, the rotating speed of setting sol evenning machine is 3000r/min, time is 1min, below, at 85 DEG C, the sample of complete for spin coating photoresist baking 10min, second step, exposure 111, sample and mask plate 102 are put on the operator's console of litho machine, adjust position, exposure 40s, wherein selected mask plate is be manufactured with the slab waveguide pattern of 7 μm, 3rd step, development 112, service property (quality) number percent is the sodium hydroxide solution of 0.5%, development time is 16s, after exposed portion photoresist dissolves, the pure washed with de-ionized water of rapid use is clean, then high-purity elevated pressure nitrogen air gun is used to be dried up by sample, 4th step, the wafer of development work will have been carried out, put and toast 10min on hot plate, temperature is 85 DEG C,
Step 3, titanizing 113, puts into sample the sputtering that d.c. sputtering machine carries out platinum/titanium metal thin film, is filled with argon gas during sputtering, make pressure maintain about 4Pa, form one deck titanium film 103 at sample surfaces;
Step 4, peel off 114, acetone is used to peel off the sample having plated platinum/titanium metal thin film, utilize supersonic wave cleaning machine to wash plating titanium on a photoresist off, after having peeled off, use alcohol and high-purity deionized water to wafer cleaning, after having cleaned, use high-purity elevated pressure nitrogen air gun to be dried up by sample, after having peeled off, use step instrument to record the thickness of titanium metal film for 90nm.
Step 5, titanium metal film prediffusion 115, puts into high temperature furnace by sample, carries out the prediffusion of platinum/titanium metal thin film, and time and temperature are respectively 2h, 1060 DEG C, can ensure that titanium ion enters lithium columbate crystal inside like this.
Step 6, rich lithium VTE process, uses rich lithium VTE technical finesse to complete the sample of platinum/titanium metal thin film prediffusion, and device, as Fig. 2, comprises rich lithium crucible 201, rich lithium powder 202, titanium diffused optical waveguide sample 203.Sample is put into by mole fraction than the Li being 68mol%:32mol%
2cO
3and Nb
2o
5in the rich lithium crucible that mixed-powder sinters into, below sample, add one deck platinum pad, directly contact with rich lithium crucible 201 to avoid titanium diffused optical waveguide sample 203.By crucible with after rich lithium powder sealing, put into box high-temperature energy-conservation stove, the operational process of box-type high-temperature furnace is by procedure auto-control, to sample at 1100 DEG C, process 30h, in described box-type high-temperature furnace, temperature controls to be divided into four-stage: a low temperature rapid heating condition, in 50min, by 25
oc rises to 400
oc; Two high temperature temperature-rise periods, 400
oc is heated to 1100
oc, used time 140min; Three is holding stages, 1100
o30h is maintained under C; Four temperature-fall periods, by 1100
oc is down to room temperature.
Step 7, optical waveguide 104 end face polishing 116, successively carries out polishing with the burnishing powder of 20,7,1.5 μm and polishing fluid to the end face of optical waveguide.
Compared with prior art, prepare the method that optical waveguide adopts titanium diffusion, prepared optical waveguide function admirable, loss is little, good effect can be played in various optical research, rich lithium vapor transportation Balance Treatment is adopted to the lithium columbate crystal after titanium diffusion, reaches near stoichiometric proportion (NS, [Li]/[Nb] >99%).Lithium niobate crysal with near stoichiometric ratio has a lot of more excellent performance: crystal defect is few, and optical homogeneity is good, has stronger electric light and nonlinear effect.Titanium diffused optical waveguide has waveguide function admirable, and the advantage such as loss is less, can be widely used in for radio art such as radio communication, radar, navigation.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. a lithium niobate fiber waveguide and prepare the method for near-stoichiometric ratio lithium niobate optical waveguide by titanium diffusion and VTE, it is characterized in that: comprise substrate and be positioned at described suprabasil ducting layer, described substrate adopts lithium columbate crystal, described ducting layer is positioned at the+z face of described lithium columbate crystal, bar ripple to direction be the y direction of lithium columbate crystal.
2. lithium niobate fiber waveguide according to claim 1, what prepare ducting layer employing on the substrate is photoetching process.
3. prepared a method for near-stoichiometric ratio lithium niobate optical waveguide by titanium diffusion and VTE, it is characterized in that: comprise the following steps:
Step one, preparation of samples, selecting is that to cut the thick same composition lithium columbate crystal of 0.5mm be original material to optical grade Z, uses precision gas cutting machine that lithium columbate crystal is cut into sample;
Step 2, photoetching, the first step, the sample cleaned up is put and toasts 10min on hot plate, temperature is 85 DEG C, then, carry out the coating of photoresist, use sol evenning machine on sample, apply one deck SPR6112B type photoresist and carry out even glue, the rotating speed of setting sol evenning machine is 3000r/min, time is 1min, below, at 85 DEG C, the sample of complete for spin coating photoresist baking 10min, second step, exposure, sample and mask plate are put on the operator's console of litho machine, adjust position, exposure 40s, wherein selected mask plate is be manufactured with the slab waveguide pattern of 7 μm, 3rd step, development, service property (quality) number percent is the sodium hydroxide solution of 0.5%, development time is 16s, after exposed portion photoresist dissolves, the pure washed with de-ionized water of rapid use is clean, then high-purity elevated pressure nitrogen air gun is used to be dried up by sample, 4th step, the wafer of development work will have been carried out, put and toast 10min on hot plate, temperature is 85 DEG C,
Step 3, titanizing, puts into sample the sputtering that d.c. sputtering machine carries out platinum/titanium metal thin film, is filled with argon gas during sputtering, make pressure maintain about 4Pa, form one deck titanium film at sample surfaces;
Step 4, peel off, acetone is used to peel off the sample having plated platinum/titanium metal thin film, utilize supersonic wave cleaning machine to wash plating titanium on a photoresist off, after having peeled off, use alcohol and high-purity deionized water to wafer cleaning, after having cleaned, use high-purity elevated pressure nitrogen air gun to be dried up by sample, after having peeled off, use step instrument to record the thickness of titanium metal film for 90nm;
Step 5, titanium metal film prediffusion, puts into high temperature furnace by sample, carries out the prediffusion of platinum/titanium metal thin film, and time and temperature are respectively 2h, 1060 DEG C, can ensure that titanium ion enters lithium columbate crystal inside like this;
Step 6, rich lithium VTE process, uses rich lithium VTE technical finesse to complete the sample of platinum/titanium metal thin film prediffusion, puts into by mole fraction sample than the Li being 68mol%:32mol%
2cO
3and Nb
2o
5in the rich lithium crucible that mixed-powder sinters into, add one deck platinum pad below sample, by crucible with after rich lithium powder sealing, put into box high-temperature energy-conservation stove, the operational process of box-type high-temperature furnace, by procedure auto-control, to sample at 1100 DEG C, processes 30h;
Step 7, the polishing of optical waveguide end face, successively carries out polishing with the burnishing powder of 20,7,1.5 μm and polishing fluid to the end face of optical waveguide.
4. the method being prepared near-stoichiometric ratio lithium niobate optical waveguide by titanium diffusion and VTE according to claim 3, be is characterized in that:, in described box-type high-temperature furnace, temperature controls to be divided into four-stage: a low temperature rapid heating condition, in 50min, by 25
oc rises to 400
oc; Two high temperature temperature-rise periods, 400
oc is heated to 1100
oc, used time 140min; Three is holding stages, 1100
o30h is maintained under C; Four temperature-fall periods, by 1100
oc is down to room temperature.
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| CN108710267A (en) * | 2018-05-21 | 2018-10-26 | 中国科学院上海光学精密机械研究所 | The preparation method of film micro optical structure based on photoetching and chemically mechanical polishing |
| CN110133802A (en) * | 2019-06-13 | 2019-08-16 | 天津领芯科技发展有限公司 | A kind of novel lithium niobate optical waveguide wafer and preparation method thereof |
| CN111722318A (en) * | 2020-06-29 | 2020-09-29 | 中国科学院上海微系统与信息技术研究所 | Preparation method of lithium niobate waveguide based on internal diffusion and ion implantation |
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