CN101403809B - Production method for amorphous Sn1As20S79 bar-shaped optical waveguide - Google Patents

Production method for amorphous Sn1As20S79 bar-shaped optical waveguide Download PDF

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CN101403809B
CN101403809B CN2008102025296A CN200810202529A CN101403809B CN 101403809 B CN101403809 B CN 101403809B CN 2008102025296 A CN2008102025296 A CN 2008102025296A CN 200810202529 A CN200810202529 A CN 200810202529A CN 101403809 B CN101403809 B CN 101403809B
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annealing
irradiation
amorphous
substrate
optical waveguide
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CN101403809A (en
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陈抱雪
孙蓓
隋国荣
王关德
浜中广见
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a manufacturing method of an Sn1As20S79 amorphous stripe light waveguide and a technology for preparing the Sn1As20S79 amorphous stripe light waveguide by adopting the processes of annealing for two times and irradiation. The invention solves the problems of preparation technique that the Sn1As20S79 amorphous stripe light waveguide can not be realized by adopting conventional techniques such as a reaction ion etching technique and an etching technique of a wet method and provides operational possibility for preparing wave guiding loop devices which are formed by the Sn1As20S79 amorphous stripe light waveguide.

Description

Amorphous Sn 1As 20S 79The strip optical waveguide manufacture method
Technical field
The present invention relates to a kind of optical waveguide technique, particularly a kind of amorphous Sn 1As 20S 79The strip optical waveguide manufacture method.
Background technology
Amorphous state sulfur family multi-element compounds semiconductor is used to prepare Infrared Lens, infrared biochemical sensor, CO as a kind of long wavelength's nonlinear optical medium 2(Bureau B etc.: J.Non-Cryst.Solids., Vol.345﹠amp such as existing report such as the work of laser transmission fiber, high-speed optical switch, load limiter, optical kerr effect chopper and optical nonlinearity ring mirror etc.; 346, p.276,2004; Hocde S etc.: J.Non-Cryst.Solids., Vol.274, p.17,2000; Nishii J etc.: J.Non-Cryst.Solids., Vol.140, p.199,1992; Asobe M etc.: J.Appl.Phys., Vol.77, p.5518,1995; TrolesJ etc.: Opt.Mater., Vol.25, p.231,2004; Asobe M etc.: Opt.Lett., Vol.18, p.1056,1993; Asobe M etc.: Electron.Lett., Vol.32, p.1396,1996).With the As that knows 2S 3Difference, As 2S 8Average coordination number lower, the chemical bond defect concentration that unusual electron configuration constitutes is higher, has several times energy level (Adler D:J.Non-Cryst.Solids., Vol.35﹠amp in the energy gap; 36, p.819,1980).We have reported and have had only at As 2S 8The disconnected test of the photoresistance of the light-luminous effect that can see in the waveguide (L.Zou, B.Chen etc.: Appl.Phy.Lett., Vol.88, p.153510-1,2006), light blocking effect has the cut-out response of ms magnitude and since the self-trapping potential well of polaron to excited electron repeat capture, recovering response is a slower s magnitude process.Recover response for improving, we have tested at As 2S 8The experiment that middle low concentration is mixed Sn utilizes Sn 1As 20S 79The shallow energy level de excitation passage that the anti-key attitude of exclusive coordination link energy level provides not only makes the disconnected recovery response of photoresistance rise to the ms magnitude, also has the effect (Du Liping, old armful of snow etc.: Acta Physica Sinica, 57 volumes, 3593 pages, 2008) that reduces residual loss.Utilize this effect to prepare the waveguide device of new function, prepare Sn 1As 20S 79Stripe waveguide is necessary, and test shows that conventional reactive ion etching process or wet etching process can not be suitable for, and the former can not make the reaction of As generating gasification, causes the residual a large amount of arsenic oxide arsenoxide particles of bar waveguide sidewalls after the etching; The latter is because Sn 1As 20S 79Not alkaline-resisting, do not cross the pass of multiple working procedure neutral and alkali solution.
Summary of the invention
The present invention be directed to existing preparation Sn 1As 20S 79The problem of stripe waveguide difficulty has proposed a kind of amorphous Sn 1As 20S 79The strip optical waveguide manufacture method adopts twice shoe to prepare Sn through the method for annealing-irradiation process 1As 20S 79The technology of amorphous state stripe waveguide makes and by the refractive index of the strip region of light wave irradiation irreversible increasing is taken place, and reaches to form Sn 1As 20S 79The purpose of amorphous state stripe waveguide.
Technical scheme of the present invention is: a kind of amorphous Sn 1As 20S 79The strip optical waveguide manufacture method, manufacture method comprises the steps:
(1), substrate adopts optical plate glass or the optical flat crystal of upper surface through the optical grade plane lapping, two side direction end faces of described substrate polish through optical grade, adopt technique for vacuum coating to prepare 0.5 μ m～thick Sn of 2 μ m on the upper surface of described substrate 1As 20S 79Noncrystalline membrane;
(2), with described Sn 1As 20S 79Noncrystalline membrane and substrate thereof place 125 ℃～135 ℃ air atmosphere insulations 1 hour, finish 1 annealing;
(3), adopting wavelength coverage is that 300～436nm, luminous power surface density are 58mW/cm 2The Sn of ultraviolet light irradiation after step (2) 1 times annealing 1As 20S 79Noncrystalline membrane, the irradiation duration was finished irradiation 1 time between 60 minutes～100 minutes;
(4), with the described Sn that finishes 1 irradiation 1As 20S 79Noncrystalline membrane and substrate thereof place 125 ℃～135 ℃ air atmosphere insulations 1 hour, finish 2 annealing;
(5), the mask that will have a bar shaped transparent window places described Sn after 2 annealing 1As 20S 79The noncrystalline membrane upper surface, the width of described marking shape window is between 3 μ m～6 μ m;
(6), adopting wavelength coverage is that 300～436nm, luminous power surface density are 58mW/cm 2Ultraviolet light by the described Sn of described marking shape window irradiation 1As 20S 79Noncrystalline membrane, the irradiation duration was finished the selectivity uv-exposure between 80 minutes～120 minutes, described Sn 1As 20S 79Refractive index through the bar-shaped zone of described uv-exposure in the noncrystalline membrane increases, and forms strip optical waveguide.
In the process of described technique for vacuum coating preparation, the temperature of described substrate is controlled at below 60 ℃.
Beneficial effect of the present invention is: amorphous Sn of the present invention 1As 20S 79The strip optical waveguide manufacture method has solved the irrealizable Sn of routine techniques such as reactive ion etching technique and wet etch technique 1As 20S 79Preparation technology's problem of amorphous state stripe waveguide is for preparing by Sn 1As 20S 79The guided wave loop device that the amorphous state stripe waveguide constitutes provides operational feasibility.
Description of drawings
Fig. 1 is an amorphous Sn of the present invention 1As 20S 79Sn in the strip optical waveguide manufacture method 1As 20S 79The visible light synoptic diagram;
Fig. 2 is an amorphous Sn of the present invention 1As 20S 79Deposition attitude Sn in the strip optical waveguide manufacture method 1As 20S 79The refractive index of film and Thickness Variation and ultraviolet are according to spoke time relation synoptic diagram;
Fig. 3 is an amorphous Sn of the present invention 1As 20S 79Sn in the strip optical waveguide manufacture method 1As 20S 79The X-ray diffraction spectrum synoptic diagram of film sample before and after ultraviolet light irradiation;
Fig. 4 is an amorphous Sn of the present invention 1As 20S 79Sn in the strip optical waveguide manufacture method 1As 20S 79The refractive index of film and Thickness Variation and annealing temperature concern synoptic diagram;
Fig. 5 is an amorphous Sn of the present invention 1As 20S 79In the strip optical waveguide manufacture method: 130 ℃ of annealed state Sn 1As 20S 79The synoptic diagram that concerns of the photorefractive effect of film and the resume of annealing;
Fig. 6 is an amorphous Sn of the present invention 1As 20 S 79118 ℃ of annealed state Sn in the strip optical waveguide manufacture method 1As 20S 79The synoptic diagram that concerns of the photorefractive effect of film and the resume of annealing;
Fig. 7 is an amorphous Sn of the present invention 1As 20S 79Annealed state Sn in the strip optical waveguide manufacture method 1As 20S 79The X-ray diffraction spectrum synoptic diagram of film sample behind ultraviolet light irradiation;
Fig. 8 is an amorphous Sn of the present invention 1As 20S 79Light saturated mode Sn in the strip optical waveguide manufacture method 1As 20S 79Film refractive index increment and annealing temperature concern synoptic diagram;
Fig. 9 is an amorphous Sn of the present invention 1As 20S 79Sn in the strip optical waveguide manufacture method 1As 20S 79The output near field photograph of 632.8nm wavelength guide mode in the bar waveguide.
Embodiment
Sn 1As 20S 79The manufacturing test procedure of amorphous state bar waveguide is as follows:
(1) length be 10mm, upper surface polishes through two ends through the optical quartz substrate of optical grade plane lapping, adopts technique for vacuum coating to prepare the thick Sn of 1 μ m on it 1As 20S 79Noncrystalline membrane, in the vacuum coating process, the temperature of substrate is controlled at below 60 ℃.
(2) with Sn 1As 20S 79Noncrystalline membrane places 130 ℃ of air atmosphere insulations 1 hour together with substrate, finishes 1 annealing.
(3) adopting wavelength coverage is that 300～436nm, luminous power surface density are 58mW/cm 2Ultraviolet light irradiation through 1 time annealing after Sn 1As 20S 79Noncrystalline membrane, the irradiation duration is 80 minutes, finishes irradiation 1 time.(4) will finish the Sn of 1 irradiation 1As 20S 79Noncrystalline membrane places 130 ℃ of air atmosphere insulations 1 hour together with substrate, finishes 2 annealing.
(5) mask that will have a bar shaped transparent window places the Sn after 2 annealing 1As 20S 79Noncrystalline membrane upper surface, the width of marking shape window are 5 μ m.
(6) adopting wavelength coverage is that 300～436nm, luminous power surface density are 58mW/cm 2Ultraviolet light by marking shape window irradiation Sn 1As 20S 79Noncrystalline membrane, the irradiation duration is 100 minutes, finishes the selectivity uv-exposure.Sn 1As 20S 79Refractive index through the bar-shaped zone of uv-exposure in the noncrystalline membrane increases, and forms strip optical waveguide.
The Sn that preparation is finished 1As 20S 79The waveguide of amorphous state bar adopts the end face coupling technique to carry out the guided mode excitation of optical waveguide, and input end docks with single-mode fiber, aims at the automatic core-adjusting method that adopted of regulating.At the waveguide output terminal, adopt the CCD shooting to observe the mould field distribution of guided mode.Fig. 9 is the output near field photograph of 632.8nm wavelength guide mode, has shown very good guiding property.
To Sn 1As 20S 79The manufacture method of amorphous state bar waveguide is described below:
One, Sn 1As 20S 79The noncrystalline membrane preparation:
Sn 1As 20S 79Film adopts the vacuum coating technology preparation, and component material Sn, As and S are counted trim by the More, and vacuum is heated to 900 ℃ of fusions, stirs insulation 10 hours, clays into power as evaporation source behind the natural cooling.Underlay substrate can be an optical glass, also can be lithium columbate crystal.In order to prevent the composition proportion change of film in the coating process, substrate temperature is controlled at below 60 ℃.Weighing method is adopted in film thickness monitoring, by regulating the quality control thickness of evaporation source.
Two, deposition attitude Sn 1As 20S 79The photorefractive effect of film:
Sn as shown in Figure 1 1As 20S 79The visible light of film, shortwave absorption edge are near 450nm, and the energy gap width is about 2.81eV.The radiation source that experiment is adopted is a ultraviolet mercury lamp, and wavelength coverage is 300～436nm.Sn before and after the photoirradiation 1As 20S 79The refractive index of film and thickness adopt the test of prismatic film coupling technique, and the test wavelength is 632.8nm.
Deposition attitude Sn without annealing in process 1As 20S 79The index increment of film and the relation of ultraviolet irradiation between the time as shown in Figure 2, ultraviolet mercury lamp intensity is 58mW/cm 2, the film refractive index n of predose 0=2.2988.Index increment and exposure time are linear in 15 minutes, begin to occur saturated phenomenon after 70 minutes, and the saturation value of index increment is near 0.045.Fig. 2 gives the measured curve of corresponding Thickness Variation, and thickness is attenuation with the increase of radiated time, and radiation is after 70 minutes, and Thickness Variation reduces, and is tending towards a stationary value, and maximum variable quantity is about-0.018 μ m.
Fig. 3 is before the ultraviolet light irradiation and the deposition attitude Sn of irradiation after 80 minutes 1As 20S 79(diffractogram of λ=0.1542nm) shows very wide diffraction halation to the Cu-K α-X ray of film, shows that sample all is a glassy state before and after ultraviolet radiation.Main peak value angle of diffraction 2 θ before the ultraviolet light irradiation are 8.20 °, corresponding mean molecule diameter is 1.0784nm, behind the ultraviolet light irradiation, main peak value angle of diffraction increases to 8.50 °, corresponding mean molecule diameter is 1.0404nm, rate of change (1.0404-1.0784)/1.0784=-3.52% shows deposition attitude Sn 1As 20S 79Film is volume-diminished behind ultraviolet light irradiation, and this phenomenon with the thickness attenuation that experiment obtains is consistent.Can also observe a little secondary peak near 2 θ=16.4 °, this is As 2S 3Typical diffraction peak, show Sn 1As 20S 79Contain a small amount of As in the film sample 2S 3Composition, behind the ultraviolet light irradiation, the diffracted intensity of main peak relatively increases and the relative reduction of secondary peak means As 2S 3Ratio further reduce.Sn 1As 20S 79Average coordination number be 2.19, deposition attitude film contains excessive S element, the energy of ultraviolet light irradiation lower part photon is converted into the chemical activity energy of molecule by the energy level transition that excites outer-shell electron, the new balance reconstruct of subsiding with stress relief has taken place to comprise in the intermolecular mechanics structure of film, structure is more stable, and density improves.According to the Lorenz-Lorentz relation, refractive index is directly proportional with density of material, Sn 1As 20S 79The increase of film refractive index mainly comes from the raising of ultraviolet light irradiation rear film density.
Three, annealed state Sn 1As 20S 79The photorefractive effect of film:
Annealing helps to improve the stability of adhesion, film compactness and the thin film physics characteristic of film and substrate, is an important process link of the high-quality optical waveguide of preparation.Sn 1As 20S 79Glass temperature T gAbout 130 ℃, annealing temperature is lower than T gCan obviously not influence the component of film.Carry out in the air atmosphere of annealing experiment between 110 ℃～130 ℃, constant temperature time is 1 hour, at room temperature cooling.Fig. 4 has provided between annealing temperature and the index increment and has concerned, in low temperature range, index increment and annealing temperature are roughly linear, and maximal value △ n is arranged near 124 ℃ Max≈ 0.04, and annealing temperature is near T gThe time, downtrending appears in index increment.Fig. 4 is Sn 1As 20S 79The graph of a relation of the refractive index of film and Thickness Variation and annealing temperature, thickness successively decreases with the increase of annealing temperature before 124 ℃, near T gThe time, thickness begins bounce-back.Because T gFollowing annealing temperature does not influence film quality, and the experimental data of Thickness Variation and index increment still reflects the Lorenz-Lorentz relation.
Annealed state Sn 1As 20S 79The photorefractive effect of film is shown in Fig. 5,6, and Fig. 5,6 annealing temperature are respectively 130 ℃ and 118 ℃, and annealing time is 1 hour, and radiation source is above-mentioned 58mW/cm 2Ultraviolet mercury lamp.Can find annealed state Sn 1As 20S 79Though the refractive index of film also increases progressively with the increase of irradiation dose, but photorefractive effect is relevant with the annealing resume, the experimental result of Fig. 5 shows two important feature, one is the process of carrying out through " 130 ℃/1h annealing-80min irradiation " more than twice, the relation curve of index increment and exposure time tends towards stability, index increment saturation value and deposition attitude Sn 1As 20S 79The light of film is sold off saturation value and is reached unanimity; Another important feature is, the photon-induced refractive index increment of 130 ℃/1h annealed state sample can be wiped by annealing, and the effect of annealing and ultraviolet irradiation provides intimate reversible process completely.These characteristics have not only been pointed out reliable refractive index control method for the waveguide of preparation bar, also indicate Sn 1As 20S 79Film is as a kind of possibility of the recording medium that can hot wipe.It is worthy of note, this completely reversibility process only in annealing temperature near T gShi Caineng sees, for being starkly lower than T gThe annealed state sample, carry out after annealing-irradiation process twice or more, it is not obvious that photorefractive effect becomes, Fig. 6 has provided the example of 118 ℃ of annealed state samples, the photorefractive effect of annealing is repeatedly afterwards obviously degenerated.
Fig. 7 has provided the Sn that carries out through " 130 (or 118) ℃/1h annealing-80min irradiation " process more than twice 1As 20S 79The X-ray diffraction spectrum of film sample for relatively, gives deposition attitude Sn among the figure 1As 20S 79Film is through the X-ray diffraction spectrum of 80 minutes ultraviolet irradiation samples, and three's main peak value angle of diffraction is close to consistent, and this is consistent with the very approaching phenomenon of the three's of Fig. 5 demonstration index increment.In addition, more smooth through the diffraction halation of heat treated sample, have more the vitrifacation feature.
Four, light saturated mode Sn 1As 20S 79The annealing effect of film:
Above-mentioned experiment shows that ultraviolet light irradiation and thermal annealing can change Sn 1As 20S 79The refractive index of film, different annealing resume can cause also that completely reversible process or part wipe phenomenon.Deposition aspect product reach the light saturated mode Sn of index increment saturation value through ultraviolet irradiation 1As 20S 79The annealing experiment of film is another important visual angle of observing photoirradiation and thermal annealing relation.Fig. 8 has provided light saturated mode Sn 1As 20S 79The index increment of film and the relation of annealing temperature, annealing time is 1 hour, and ordinate Δ n is the refringence of annealing back sample and light saturated mode sample.A very useful conclusion is, near annealing 115 ℃ can obviously not change the refractive index of light saturated mode film, and annealing temperature is got the size that can regulate refractive index about it.
Deposition attitude and annealed state Sn 1As 20S 79Film was being placed respectively 6 months under the dry room temperature condition and after nearly 4 months through the sample behind the ultraviolet irradiation and the light saturated mode sample after annealing, test once again all show refractive index to the radix point the 3rd remain unchanged, show and adopt the combined with heat treatment light technology of selling off to prepare Sn 1As 20S 79The waveguide of amorphous state bar is a kind of technology that can expect.

Claims (2)

1. amorphous Sn 1As 20S 79The strip optical waveguide manufacture method, manufacture method comprises the steps:
(1), substrate adopts optical plate glass or the optical flat crystal of upper surface through the optical grade plane lapping, two side direction end faces of described substrate polish through optical grade, adopt technique for vacuum coating to prepare 0.5 μ m～thick Sn of 2 μ m on the upper surface of described substrate 1As 20S 79Noncrystalline membrane;
(2), with described Sn 1As 20S 79Noncrystalline membrane and substrate thereof place 125 ℃～135 ℃ air atmosphere insulations 1 hour, finish 1 annealing;
(3), adopting wavelength coverage is that 300～436nm, luminous power surface density are 58mW/cm 2The Sn of ultraviolet light irradiation after step (2) 1 times annealing 1As 20S 79Noncrystalline membrane, the irradiation duration was finished irradiation 1 time between 60 minutes～100 minutes;
(4), with the described Sn that finishes 1 irradiation 1As 20S 79Noncrystalline membrane and substrate thereof place 125 ℃～135 ℃ air atmosphere insulations 1 hour, finish 2 annealing;
(5), the mask that will have a bar shaped transparent window places described Sn after 2 annealing 1As 20S 79The noncrystalline membrane upper surface, the width of described marking shape window is between 3 μ m～6 μ m;
(6), adopting wavelength coverage is that 300～436nm, luminous power surface density are 58mW/cm 2Ultraviolet light by the described Sn of described marking shape window irradiation 1As 20S 79Noncrystalline membrane, the irradiation duration was finished the selectivity uv-exposure between 80 minutes～120 minutes, described Sn 1As 20S 79Refractive index through the bar-shaped zone of described uv-exposure in the noncrystalline membrane increases, and forms strip optical waveguide.
2. according to the described amorphous Sn of claim 1 1As 20S 79The strip optical waveguide manufacture method is characterized in that, in the process of described technique for vacuum coating preparation, the temperature of described substrate is controlled at below 60 ℃.
CN2008102025296A 2008-11-11 2008-11-11 Production method for amorphous Sn1As20S79 bar-shaped optical waveguide Expired - Fee Related CN101403809B (en)

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