CN101364702A - Organic-inorganic composite erbium doping flat optical waveguide amplifier and preparing method thereof - Google Patents
Organic-inorganic composite erbium doping flat optical waveguide amplifier and preparing method thereof Download PDFInfo
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- CN101364702A CN101364702A CNA2008100510761A CN200810051076A CN101364702A CN 101364702 A CN101364702 A CN 101364702A CN A2008100510761 A CNA2008100510761 A CN A2008100510761A CN 200810051076 A CN200810051076 A CN 200810051076A CN 101364702 A CN101364702 A CN 101364702A
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Abstract
The invention relates to a strip-shaped optical waveguide amplifier by adopting a novel organic polymer material as an optical waveguide envelope, and adopting an organic-inorganic hybrid material doped with LaF3: Er, Yb nano-particles which are modified by an oleic acid surface as a sandwich layer, as well as the preparation method thereof. The optical waveguide amplifier is composed of a silicon substrate, a lower envelope, the sandwich layer and an upper envelope, wherein the lower envelope and the upper envelope adopt the novel organic polymer material; the sandwich layer adopts the organic-inorganic hybrid material doped with the LaF3:Er, Yb nano-particles which are modified by the oleic acid surface; the refractive index of the sandwich layer is larger than the refractive index of the lower envelope and the upper envelope; a plurality of strip-shaped waveguide grooves are formed on the lower envelope; the strip-shaped waveguide grooves are filled with the organic-inorganic composite materials of the sandwich layer, so as to form a buried structure. The method for making the optical waveguide amplifier is simple; the refractive index difference between the polymer sandwich layer and the envelope material is easy to control; and the thickness of each layer of material is easy to control. The optical waveguide amplifier has the advantages of low cost, good gain performance and high yield, and is suitable for mass production.
Description
Technical field
The present invention relates to organic-inorganic compoiste optical waveguides amplifier and preparation method thereof, being specifically related to adopt novel organic polymer material is the fiber waveguide covering, adopts the LaF of oleic acid finishing
3: Er, the nano-particle doped organic-inorganic hybridized material of Yb are compound embedding erbium doping flat strip optical waveguide amplifier of sandwich layer and preparation method thereof.
Background technology
Erbium doping flat optical waveguide amplifier (EDWA) is a kind of important photonic propulsion element, it is the important component part of optical communication dense wave division multipurpose (DWDM) transmission system, can integrate with any lossy devices such as modulator, optical switch, array waveguide grating, isolators, all kinds of losses of compensation in the optical transmission process, this solution of key technology will make the light interconnection of chip chamber and light is integrated makes a breakthrough.
Erbium-doped fiber amplifier (EDFA) is one of most important invention on the optical fiber communication history, and its length is generally several meters to tens meters, this in long haul communication without a doubt; But in the short-distance transmission that Fiber to the home in future (FTTH), the application of EDFA just has certain difficulty.Simultaneously, in optical communication system, in order to guarantee the transmission of light signal, inevitably to use some optics such as multiplexing demultiplexing device, beam splitter and optical switch etc., these devices all exist certain loss, as not compensated, will reduce the transmitting range of signal greatly, therefore also to be amplified enhancing to signal.Also need a kind of amplifier that can provide the certain gain amount on the specific node of metropolitan area network and Access Network as required in the optical communication network, this amplifier must be cheap, and maintenance cost is low, and can make full use of existing fiber bandwidth resource, and can dilatation.In view of in the planar light subclass becomes, using EDFA, therefore press for development flat optical waveguide amplifier (EDWA) and satisfy the demand simultaneously.EDWA be a kind of compactness, reliable, be easy to integrated, image intensifer cheaply, it is rear-earth-doped (as Er
3+) concentration ratio EDFA (is 10 for high about 100 times
26m
-3), several centimetres to tens centimetres length just can realize the gain (but too high doping content can make pumping efficiency descend) more than the 10dB.Relative EDFA, EDWA has the advantage that size is little, cost is low; Relative semiconductor optical amplifier (SOA)), EDWA has the advantage of low, polarization correlated low, the no channels crosstalk of noise figure.The EDWA product can be single wavelength amplify also and can amplify by multi-wavelength, can unidirectional pumping also can two directional pump; Can be on same substrate integrated a plurality of EDWA, form the EDWA array, be implemented in the dynamic adjustments of multi-wavelength gain in the dwdm system.At present, according to the doped substrate difference of erbium ion, the EDWA device can be divided into following three types:
1, at SiO
2, Al
2O
3, Y
2O
3, ZrO
2Deng oxide ceramics, phosphate, silicate and LiNbO
3Er mixes in the inorganic matrix materials such as crystal
3+, prepare inorganic EDWA.Preparation technology generally adopts ion-exchange, ion injection, molecular beam epitaxy, physical vapor deposition, flame hydrolysis deposit and plasma chemical vapor deposition etc.Comparatively ripe to the research of inorganic EDWA at present, gain can reach 4dB/cm.But its preparation technology is complicated, the preparation cost height, and waveguide core district and cladding region refractive index change amount are little, and device is not very compatible with silica-base material, have any problem in the application of planar light subclass one-tenth.
2, with Er
3+Ion and organic ligand form complex, are dissolved in the organic EDWA of preparation in the organic polymer material.Compare with traditional inorganic optical waveguide material, the processing technology of organic polymer optical waveguide is simpler, cheap than inorganic fiber waveguide, need only just can prepare the integrated optoelectronic device of function complexity by technologies such as room temperature spin coating and photoetching, and refringence is easy to adjust, the device of preparation is light and handy, good mechanical property, thereby be applicable to preparation high density integrated device, for these reasons, polymeric material makes that the application of photoelectron technology is more extensive.But because Er
3+Salt solubility in polymer is low, makes Er
3+The difficult requirement that reaches the device amplification performance of doping content, and, be easy to Er owing to have a large amount of C-H, O-H high energy vibration group in the polymer
3+Vibration coupling takes place, thereby reduces Er
3+Life-span on excited level.Because these more formidable shortcomings, the research that utilizes polymeric material to prepare EDWA both at home and abroad at present mostly is in the material preparation stage, and the report of related device is few.
3, when carrying out the research of erbium complex material, the scientific research personnel is also making great efforts to prepare the organic-inorganic compoiste material that is used for orthoron.This class material combines the two advantage of inorganic and organic material, improves greatly than general polymerization thing matrix as the luminescent lifetime of material, can reach a millisecond magnitude, and the more inorganic EDWA of device preparing process is simple and preparation cost is cheap, receives people's very big concern.Yet the domestic and international at present report about er-doped organic-inorganic compoiste EDWA still belongs to blank, and most research concentrates on the material preparation stage.
The present invention adopts LaF
3: Er, the organic-inorganic compoiste optical waveguides amplifier of the hybrid inorganic-organic materials preparation that Yb is nano-particle doped, it is a kind of novel optical waveguides amplifier that the deficiency at organic EDWA and inorganic EDWA puts forward, can effectively remedy the shortcoming of above-mentioned two kinds of EDWA, be expected in the planar light subclass becomes, to obtain commercial application.
Summary of the invention
The objective of the invention is to overcome disadvantages of background technology, the preparation method of a kind of organic-inorganic composite erbium doping flat (EDWA) optical waveguides amplifier and this optical waveguides amplifier is provided.
The described method of this patent does not re-use expensive thick film growth and corresponding ion implantation device, avoids the difficulty of high growth temperature material simultaneously, is beneficial to the optimal design of device; Be easy to control the core layer thickness and the refractive index of waveguide, the technical process that (room temperature to 150 ℃) realizes easily in lower temperature range prepares the EDWA device.
The LaF of the present invention's preparation
3: Er, the organic-inorganic composite erbium doping flat optical waveguide amplifier that Yb is nano-particle doped when importing the flashlight of 1550nm wavelength, can obtain the gain of light of 6.8dB on the long device of 2cm.The performance parameter of device is close with inorganic EDWA device performance, but the price of organic-inorganic composite erbium doping flat optical waveguide amplifier is well below inorganic EDWA device.
The LaF that the present invention relates to
3: Er, the nano-particle doped organic-inorganic composite erbium doping flat optical waveguide amplifier of Yb is made up of silicon substrate, under-clad layer, sandwich layer and top covering successively, it is characterized in that:
Under-clad layer and top covering are organic polymer materials;
Sandwich layer is the LaF of oleic acid finishing
3: Er, the organic-inorganic compoiste material that Yb is nano-particle doped;
The refractive index of sandwich layer is greater than the refractive index of under-clad layer and top covering.
A plurality of slab waveguide grooves are arranged on under-clad layer, be filled with sandwich layer in the slab waveguide groove, form and bury the type structure.
Further, have 3～10 slab waveguide grooves that width is different with spacing, further, have 5 slab waveguide grooves that width is different with spacing, width is followed successively by 3.5～5 μ m, 5.5～7 μ m, 7.5～9 μ m, 9.5～11 μ m and 11.5～13 μ m, and spacing is 100～150 μ m.
The upper and lower covering of orthoron of the present invention is the organic polymer material that has added the refractive index conditioning agent, and sandwich layer is the LaF of oleic acid finishing
3: Er, the hybrid inorganic-organic materials that Yb is nano-particle doped is solution state before all material spin coating of upper and lower covering and sandwich layer, need filter through the filter below 0.4 micron and 0.4 micron; Covering, core material possess heat cross-linking or photo-crosslinking characteristic simultaneously, 100～130 ℃ down or ultraviolet light (＜365nm) cross-linking reaction can take place down in irradiation, makes the stability raising of material.
As the organic polymer material of upper and lower covering is that (this material can make from methyl methacrylate and the copolyreaction of two kinds of materials employings of GMA conventional method methyl methacrylate with GMA copolymer p MMA-GMA, belong to known product, apply for a patent, the patent No. is: 03127171.5), its molecular structural formula is shown in general formula (I).
General formula (II) is the refractive index conditioning agent, in upper and lower clad material (I), need to add the refractive index conditioning agent (II) of 17wt%～40wt%, and then the refractive index of adjusting upper and lower clad material is between 1.48～1.51, thereby makes light field keep single mode transport in core material.
Sandwich layer used in the present invention is active dopant material, is the LaF through the oleic acid finishing
3: Er, Yb nano particle.In order to improve Er
3+The absorption efficiency of ion pair 980nm pump light, Yb
3+Ion is added into as sensitizer, Yb
3+Ion
2F
5/2Energy level and Er
3+Ion
4I
11/2Energy level is complementary, and the pump energy of the 980nm of its absorption effectively can be passed to Er
3+Ion effectively remedies Er
3+Ion improves the absorption and the utilization ratio of pump light for the little shortcoming of 980nm pump light absorption cross-section.
The LaF of oleic acid finishing
3: Er, the basic building-up process of Yb nano particle is: 0.504g NaF is dissolved in the deionized water of 90ml, adds 60ml ethanol and 20ml oleic acid again.Under nitrogen environment, mixture is heated to 75 ℃, and powerful the stirring, when mixture becomes clear solution, add 1.4804gLaCl
37H
2O, 0.1020g ErCl
36H
2O and 0.4124g YbCl
36H
2O, the water that dropwise adds 10ml fully dissolves it.Keep 75 ℃ temperature, the powerful stirring 5 hours, treat that it fully reacts after, be cooled to room temperature.The inorganic salts of remnants and oleic acid are filtered, take turns ultrasonic cleaning reaction precipitation thing to residue with absolute ethyl alcohol and deionized water and remove fully, can get the LaF of oleic acid finishing afterwards with 8000 rev/mins rotating speed centrifugation in 10 minutes
3: Er, Yb mix nano particle altogether.The mol ratio of each element is LaF in the nano particle
3: Er:Yb=0.75:0.05:0.20, can adopt XRD and TEM means of testing proof synthetic material to form the nano particle with hexagonal crystallographic texture.
Hybrid inorganic-organic materials is to adopt Metacrylopro-pyltrimethoxysilane (MPTS) and the Zr (OBu) that does not purify
4As raw material.At first, in the isopropyl alcohol that MPTS is dissolved in, volume ratio is 1:1, adds hydrochloric acid and makes their that part hydrolysis take place, the volume ratio of hydrochloric acid and isopropyl alcohol is 1:2, dropwise adds Zr (OBu) after 1 hour in the MPTS solution that partial hydrolysis reacts has taken place
4, the powerful stirring 2 hours dropwise adds entry under the room temperature, and the volume ratio of water and hydrochloric acid is 1:1, after 12 hours, Zr (OBu)
4Can with the siloxanes generation hydrolysis among the MPTS, the mol ratio of element Zr and Si is 0.5:1, and reactant is dissolved with toluene, adopts the method for liquid extraction to purify then, obtains the toluene solution of hybrid inorganic-organic materials.With behind the wherein remaining moisture of anhydrous magnesium sulfate absorption anhydrous magnesium sulfate being leached, solution can get gluey, yellow-white transparent resin 50 ℃ of following vacuumizes 2 hours, i.e. the described hybrid inorganic-organic materials of this patent.
Core material of the present invention is the LaF with the oleic acid finishing
3: Er, Yb is nano-particle doped in above-mentioned hybrid inorganic-organic materials.The LaF of weighing 0.576g oleic acid finishing at first
3: Er, the Yb nano particle, it is dissolved in the toluene solution that 2ml crosses through anhydrous magnesium sulfate drying, add (mesityl) meth-anone (IHT-PI-TPO) of above-mentioned hybrid inorganic-organic materials of 1.152g and 0.0346g light trigger (diphenylphosphoryl) then, at room temperature powerful the stirring fully dissolved it in 12 hours, filter, can get LaF
3: Er, the hybrid inorganic-organic materials solution that Yb is nano-particle doped, refractive index is 1.512.
The LaF that the present invention relates to
3: Er, its preparation method of the organic-inorganic composite erbium doping flat optical waveguide amplifier that Yb is nano-particle doped referring to accompanying drawing 3, specifically is stated as:
A, be substrate with the monocrystalline silicon piece, spin coating has been added organic polymers condensation material (I) of 17wt%～40wt% refractive index conditioning agent (II) as under-clad layer on monocrystalline silicon piece, dry then, isothermal curing is 3～5 hours under 120～125 ℃ of temperature conditions, and the thickness of gained under-clad layer is 5～10 μ m;
B, on under-clad layer evaporation of aluminum 30～100nm, coating thickness is the photoresist of 3～5 μ m on the aluminium film, carry out photoetching with optical waveguides amplifier mask plate with a plurality of strip structures, the aqueous solution with NaOH develops, thereby with the waveguide figure transfer on the mask plate to photoresist, carrying out the oxygen reactive ion etching then, is a plurality of stripe shape waveguide groove of 3.0～5.0 μ m deeply on polymer under-clad layer material after the etching;
C, with the LaF of oleic acid finishing
3: Er, the nano-particle doped hybrid inorganic-organic materials of Yb is as sandwich layer, be spin-coated on the under-clad layer that contains the slab waveguide groove with 2000～3000 rev/mins rotating speeds, thickness is 2～5 μ m, in nitrogen atmosphere under 100～110 ℃ of temperature conditions before the baking 5～10 minutes, uv-exposure 3～5 minutes under 150～200W power makes sandwich layer generation photopolymerization reaction again, solidifies 4～6 hours down in 120～125 ℃ of temperature conditions then;
D, on sandwich layer spin coating thick be 3～6 μ m interpolation the organic polymer material (I) of 17wt%～40wt% refractive index conditioning agent (II) as top covering, put into baking oven isothermal curing 3～5 hours under 120～125 ℃ of temperature conditions, promptly prepare the organic-inorganic composite erbium doping flat optical waveguide amplifier thereafter.
As a kind of concrete execution mode, optical waveguides amplifier mask plate with a plurality of strip structures is to have 3～10 bar shaped arrays that width is different with spacing, more preferably have 5 bar shaped arrays that width is different with spacing, be followed successively by 3.5～5 μ m, 5.5～7 μ m, 7.5～9 μ m, 9.5～11 μ m and 11.5～13 μ m as width, spacing is the strip structure mask plate of 100～150 μ m.
Preparation of devices method of the present invention is not only controlled the refringence of core polymer layer and covering easily, and controls the thickness of each layer material easily; Device cost is low, the rate of finished products height, and gain performance is good, is fit to produce in enormous quantities.
In sum, LaF
3: Er, advantage such as it is simple that the nano-particle doped organic-inorganic compoiste EDWA device of Yb has preparation technology, and cost is low, and refractive index is easy to control can adopt traditional photoetching technique and reactive ion (RIE) dry etching technology to realize technology.Organic-inorganic compoiste EDWA device can adopt the photoresist of antioxygen, and (UV15 SU-8) makes mask, carries out reactive ion etching then in oxygen; Also can adopt aluminium film to carry out the oxygen reactive ion etching as mask, have good controllability in conjunction with photoresist.The present invention has remedied Er
3+Ion doping content in polymer substrate is low and by the shortcomings such as vibration quencher that C-H, O-H key bring, overcome to prepare the required high cost of inorganic EDWA, and complicated drawbacks such as technology, device performance and inorganic EDWA are approaching.But method of the present invention is suitable for producing in enormous quantities the EDWA device of practical application.
Description of drawings
Fig. 1: LaF under the room temperature
3: Er, the absorption spectrogram of the hybrid inorganic-organic materials film that Yb is nano-particle doped;
Fig. 2: the 980nm pump light excites down LaF
3: Er, the emission spectrogram of the hybrid inorganic-organic materials film that Yb is nano-particle doped;
Fig. 3: the process chart of preparation organic-inorganic compoiste EDWA device of the present invention;
Fig. 4: the picture of the slab waveguide groove of the EDWA figure that in the under-clad layer material, etches of the present invention;
Fig. 5: LaF
3: Er, the organic-inorganic compoiste EDWA device gain The performance test results that Yb is nano-particle doped;
Fig. 5 (a): before and after the 980nm pump light input organic-inorganic compoiste EDWA, spectrometer registration change curve;
Fig. 5 (b): the relation curve that organic-inorganic compoiste EDWA gain changes with pump power;
Fig. 5 (c): the registration change curve of spectrometer before and after the input of 980nm pump light;
Fig. 5 (d): input signal light power not simultaneously, relative gain is with the change curve of pump power.
As shown in Figure 1, the LaF of the oleic acid finishing of the present invention's preparation3: Er, the thick about 140 μ m of hybrid inorganic-organic materials film that Yb is nano-particle doped have obvious absorption at 525nm, 650nm, 975nm and 1530nm wavelength place, respectively corresponding Er3+Ion is by ground state4I
15/2Energy level is to excitation state2H
11/2、
4F
9/2、
4I
11/2、
4I
13/2The typical transition of energy level absorbs. Because Yb3+The adding of ion, film sample is at the 980nm ripple The absorption cross-section of strong point is bigger, shows that material has higher absorption and utilization ratio for pump light.
As shown in Figure 2, the LaF of the oleic acid finishing of the present invention's preparation3: Er, the thick about 140 μ m of hybrid inorganic-organic materials film that Yb is nano-particle doped, under the 980nm pumping, maximum emission peak is positioned at the 1535nm place, corresponding Er3+Ion is by excitation state4I
13/2Energy level is to ground state4I
15/2The radiation transistion of energy level, the fluorescence halfwidth (FWHM) be 83nm.
As shown in Figure 3, the spin coating under-clad layer refers to tool certain molecular weight and concentration (methyl methacrylate With the number-average molecular weight of GMA copolymer material be 100,000, concentration is 15～30%) energy Free-pouring polymeric material drops in the list of processing (cleaning and ultrasonic cleaning with toluene, acetone, ethanol) On the crystal silicon substrate 1, monocrystalline substrate 1 is placed on the rotary coating machine, under 2000～3000 rev/mins rotating speed The rotation substrate is filmed, and the time of spin coating is 20～40 seconds, makes to have added 17wt%～40wt% refractive index The polymer under-clad layer 2 of conditioning agent is evenly coated on the substrate 1, and the thickness of under-clad layer 2 is 5～10 μ m.
Said evaporation of aluminum is the aluminium film at method evaporation one deck 30～100nm of the evaporation of under-clad layer 2 usefulness or sputter 4, the spin coating thick layer is the positive photoresist 5 of 3～5 μ m on aluminium film 4 then.
Said mask, photoetching are that the mask plate 6 that will have the strip optical waveguide amplifier figure of different in width and different spacing is placed on photoresist 5 (Beijing chemical reagent factory, the BP212 type) on, again this sample is placed on the litho machine, shine with 365nm, 150～200W ultraviolet light 7, transparent area by mask plate 6 exposes photoresist, time for exposure is 30～50 seconds, by exposure the EDWA figure on the mask plate 6 is transferred on the photoresist 5, sample after the exposure is developed NaOH and H with the aqueous solution of NaOH2The proportioning of O Be 0.1g:250ml, developing time is 50～90 seconds, by developing the figure 10 of EDWA is also turned to simultaneously Move on on the aluminium film 4, shown in the step 13,14 of Fig. 3.
Said oxygen reactive ion etching step 15 with process step 13, after 14 with the EDWA figure Sample carries out reactive ion etching 8 under Oxygen Condition, photoresist 5 at first is etched away, and exposes aluminium film 4, by When the aluminium film carried out reactive ion etching in oxygen atmosphere, aluminium meeting and oxygen reaction formed one deck oxygen on the surface Change aluminium, thereby stop oxygen and 2 polymer reactions of the under-clad layer below it. There is not the part of aluminium film to continue quilt Oxygen reacts and etches away, and forms slab waveguide grooves 11 at under-clad layer 2, so 4 pairs of under-clad layer polymerizations of aluminium film Thing 2 plays good mask effect, can guarantee the bar shaped with the EDWA figure for preparing in clad material The end surface shape of waveguide groove 11 is shown in Fig. 3 step 15. The incident microwave power of oxygen reactive ion etching 20～100 watts, reflection power＜1 watt, etching 5～20 minutes, use then with said method in same concentration The aluminium film 4 of NaOH solution removal oxidation.
Said spin coating core material is the doping LaF with the oleic acid finishing3: Er, Yb nano particle organic-inorganic hybrid material (doping content of nano particle be 30～60wt%) drop in the slab waveguide groove 11 and On the under-clad layer 2, monocrystalline substrate 1 is placed on the rotary coating machine, under 2000～3000 rev/mins rotating speed The rotation substrate is filmed, and the time of spin coating is 20～40 seconds, and it is recessed to make core material 3 be evenly coated in slab waveguide In the groove 11, groove is filled formation bury type waveguiding structure 12, and evenly overlay on the under-clad layer 2, sandwich layer 3 is thick Degree is 2～5 μ m.
Said spin coating top covering 9 is that the concentration of will add 17wt%～40wt% adjustable refractive index agent is 15%～30% polymer material is evenly coated on the sandwich layer 3 with the method for spin-coating, and thickness is 3～6 μ m, and then obtain the EDWA device, this process is shown in Fig. 3 step 16.
Be depicted as under different microscope multiplication factors such as Fig. 4 (a), (b), etch in the under-clad layer material The ESEM picture of slab waveguide groove. The prepared strip groove degree of depth is 3.0～5.0 μ m, the width branch Be not 4 μ m, 6 μ m, 8 μ m, 10 μ m and 12 μ m, the distance between groove is 127 μ m.
Being depicted as in length such as Fig. 5 (a) is 22mm, and slab waveguide groove sectional dimension is 8 μ m * 3.5 μ m, On the fiber waveguide of the thick about 3 μ m of sandwich layer planar waveguide, when signal light wavelength is 1535nm, power is 0.12mW The time, input wavelength is that 980nm, power are that the registration of spectrometer changes before and after the pump light of 128mW, Changing value is 4.51dB, the gain of light that has namely produced 2.1dB/cm.
Being depicted as in length such as Fig. 5 (b) is 22mm, and slab waveguide groove sectional dimension is 8 μ m * 3.5 μ m, On the fiber waveguide of the thick about 3 μ m of sandwich layer planar waveguide, when input signal power is respectively 0.05mW, 0.2mW During with 0.5mW, the relation curve that the organic-inorganic compoiste EDWA of preparation gain changes with pump power. Test result shows: for fixing signal light power, gain increases with the increase of pump power; For solid Fixed pump power, the power of input signal light is more little, and the yield value of acquisition is more big; Work as input signal light power Be 0.05mW, when pump power was 120mW, gain reached maximum 4.7dB.
Being depicted as in length such as Fig. 5 (c) is 20mm, and slab waveguide groove sectional dimension is 10 μ m * 4 μ m, On the fiber waveguide of the thick about 4 μ m of sandwich layer planar waveguide, the input signal light wavelength is that 1536nm, power are 0.03 MW, input wavelength are that 980nm, power are that the registration of spectrometer changes before and after the pump light of 100mW. During input pumping light, spectrometer shows that output optical signal is-64.64dBm, adopts spectrum high accuracy scan function The variation that the pump power of record is fallen the moment spectrometer shows that output optical signal is reduced to-71.44dBm, reduces 6.8dB, the gain of light that has namely produced 3.4dB/cm, this is in the waveguide of 8 μ m * 6 μ m than sectional dimension The gain of the 2.1dB/cm that produces has improved many.
We the development organic-inorganic compoiste EDWA device finally will with silica-based electric light/hot optical modulator, coupling Close the opto-electronic devices such as device, wavelength division multiplexer and integrate, in order to satisfying all kinds of losses in the optical communication network, Its effect is equivalent to the triode of integrated circuit the inside, therefore requires the device can be to the low-loss window of optic communication The light of mouth 1550nm wavelength amplifies.
Be depicted as in 1550nm signal light-wave strong point such as Fig. 5 (d), when input signal light power by 0.05mW When being increased to 0.5mW gradually, the situation that the spectrometer power output changes with pump power is in the groove sectional dimension Be 12 μ m * 4 μ m, on the fiber waveguide of the thick about 4 μ m of sandwich layer planar waveguide, when pump light is increased to by 0mW During 120mW, output signal power increases with the increase of pump light, for different input signal light powers, Power output variation tendency, amplitude are more consistent. When the flashlight of input 0.05mW, pump power is 120mW The time, gain reaches maximum 6.83dB, and relative gain is 3.4dB/cm. The organic and inorganic that shows preparation is compound Type EDWA has obvious amplification for the flashlight of 1550nm wavelength.
Embodiment
Embodiment 1: the preparation of clad material
In the single neck bottle of 500ml, add the 200ml methyl methacrylate, add 2% hydroquinones, under 80 ℃ of water bath condition, after the decompression distillation, collect methyl methacrylate, stand-by.
Blender, reflux condensing tube, thermometer and N are installed on the 500ml four-hole bottle
2Protective device; add methyl methacrylate 50g (0.5mol), GMA 7g (0.05mol), the fine 0.1g of azo two isobutyls; butyl acetate 150ml; heat in water-bath, reaction obtained copolymer solution in 4 hours under 70～75 ℃ of conditions, and filter the dilution back; the distillation fraction solvent; add imidazoles at last as curing agent, can obtain solid content and be the copolymer solution of 19% PMMA-GMA, its molecular structural formula is shown in general formula (I).
Add the refractive index conditioning agent GMA of 30wt% then therein, after tested, the refractive index of this material at 1.54 μ m places is 1.491.In clad material, add certain amount of solvent and dilute, mix and stir,, regulate its concentration and be 15～30% and make it and can slowly flow with 0.4 micron filter filtration, standby.
Embodiment 2:LaF
3: Er, the preparation of the organic-inorganic hybrid material that Yb is nano-particle doped
Weighing 1.519g hybrid inorganic-organic materials is placed in the little flask, the LaF of weighing 0.7595g oleic acid modified
3: Er, the Yb nano particle puts it in the little flask that fills hybrid material.Weighing is through MgSO
4Dry toluene solution 1.13925g is poured in the little flask that fills hybrid material and nano particle, adds a cover to prevent volatilization.Magnetic agitation 5 hours, ultrasonic agitation is 20 minutes again, dissolves in hybrid inorganic-organic materials evenly up to nano particle, and refractive index is 1.512.The LaF of oleic acid modified
3: Er, the doping content of Yb nano particle in hybrid inorganic-organic materials is 50wt%.
Embodiment 3: a kind of mode of spin coating
The clad material of embodiment 1 preparation is applied on the monocrystalline substrate of handling 1, and with 3000 rev/mins rotating speed rotation, rotational time is 30 seconds, dries then, and the thickness that obtains under-clad layer 2 is 7 microns; The aluminium film 4 of oven dry back evaporation one deck 50nm, spin coating photoresist BP212 then, photoetching, development are carried out with EDWA mask plate 6 in the baking back before the photoresist 5, with the EDWA figure transfer on the mask plate 6 to photoresist 5, by developing further the EDWA figure transfer to aluminium film 4, mask plate is the mask plate of strip structure, and the height of waveguide bar is 5.0 μ m, width is respectively 4 μ m, 6 μ m, 8 μ m, 10 μ m and 12 μ m, and the distance between the waveguide bar is 127 μ m.
Embodiment 4: reactive ion etching
The sample of embodiment 3 preparations is positioned in the reactive ion etching machine, under the oxygen condition, carry out reactive ion etching 8, photoresist 5 at first is etched away, expose aluminium film 4, because during the reactive ion etching of aluminium film in oxygen atmosphere, aluminium meeting and oxygen reaction, form one deck aluminium oxide on the surface, stop 2 reactions of oxygen and the covering polymer below it, play good mask effect, can guarantee the end surface shape of the polymer waveguide for preparing.200 watts of the incident microwave powers of reactive ion etching, reflection power＜1 watt-hour, etching 15 minutes; Use NaOH solution removal aluminium film 4 then.Spin coating core material 3 on the sample after the etching, the thickness of control material are 3 microns, spin coating top covering material 9 on core material at last, and thickness is 3 microns, so just prepares the EDWA device that adheres to specification.
Claims (7)
1, organic-inorganic composite erbium doping flat optical waveguide amplifier, form by silicon substrate (1), under-clad layer (2), sandwich layer (3) and top covering (9) successively, it is characterized in that: under-clad layer (2) and top covering (9) are organic polymer materials, and sandwich layer (3) is the LaF of oleic acid finishing
3: Er, the organic-inorganic compoiste material that Yb is nano-particle doped, the refractive index of sandwich layer (3) is greater than the refractive index of under-clad layer (2) and top covering (9), a plurality of slab waveguide grooves (11) are arranged on the under-clad layer (2), be filled with the organic-inorganic compoiste material of sandwich layer (3) in the slab waveguide groove (11), form and bury type structure (12).
2, organic-inorganic composite erbium doping flat optical waveguide amplifier as claimed in claim 1, it is characterized in that: under-clad layer (2) and top covering (9) are the organic polymer material of structural formula shown in (I), and the refractive index conditioning agent (II) that has added 17wt%～40wt% therein
3, organic-inorganic composite erbium doping flat optical waveguide amplifier as claimed in claim 1 or 2 is characterized in that: have 3～10 slab waveguide grooves (11) that width is different with spacing.
4, the preparation method of organic-inorganic composite erbium doping flat optical waveguide amplifier as claimed in claim 3, be characterised in that altogether: have 5 slab waveguide grooves (11) that width is different with spacing, width is followed successively by 3.5～5 μ m, 5.5～7 μ m, 7.5～9 μ m, 9.5～11 μ m and 11.5～13 μ m, and spacing is 100～150 μ m.
5, the preparation method of the described organic-inorganic composite erbium doping flat optical waveguide amplifier of claim 1, its step is as follows:
A, be substrate (1) with the monocrystalline silicon piece, organic polymers condensation material (I) of 17wt%～40wt% refractive index conditioning agent (II) has been added in spin coating on monocrystalline silicon piece, as under-clad layer (2), dry then, isothermal curing is 3～5 hours under 120～125 ℃ of temperature conditions, and the thickness of gained under-clad layer (2) is 5～10 μ m;
B, go up evaporation of aluminum film (4) 30～100nm at under-clad layer (2) again, going up coating thickness at aluminium film (4) is the photoresist (5) of 3～5 μ m, carry out photoetching with optical waveguides amplifier mask plate (6) with a plurality of strip structures, the aqueous solution with NaOH develops, with the waveguide figure transfer on the mask plate (6) to photoresist, carrying out oxygen reactive ion etching (8) then, is a plurality of stripe shape waveguide groove (11) of 3.0～5.0 μ m deeply on polymer under-clad layer (2) after the etching;
C, with the LaF of oleic acid finishing
3: Er, the nano-particle doped hybrid inorganic-organic materials of Yb is as sandwich layer (3), be spin-coated on the under-clad layer (2) that contains slab waveguide groove (11) with 2000～3000 rev/mins rotating speeds, thickness is 2～5 μ m, in nitrogen atmosphere under 100～110 ℃ of temperature conditions before the baking 5～10 minutes, uv-exposure 3～5 minutes under 150～200W power makes sandwich layer (3) that photopolymerization reaction take place again, solidifies 4～6 hours down in 120～125 ℃ of temperature conditions then;
D, sandwich layer (3) go up spin coating thick be 3～6 μ m interpolation the organic polymer material (I) of 17wt%～40wt% refractive index conditioning agent (II) as top covering (9), put into baking oven isothermal curing 3～5 hours under 120～125 ℃ of temperature conditions, promptly prepare the organic-inorganic composite erbium doping flat optical waveguide amplifier thereafter.
6, the preparation method of organic-inorganic composite erbium doping flat optical waveguide amplifier as claimed in claim 5 is characterised in that altogether: the optical waveguides amplifier mask plate (6) with a plurality of strip structures is to have 3～10 bar shaped arrays that width is different with spacing.
7, the preparation method of organic-inorganic composite erbium doping flat optical waveguide amplifier as claimed in claim 6, be characterised in that altogether: the optical waveguides amplifier mask plate (6) with a plurality of strip structures is to have 5 bar shaped arrays that width is different with spacing, width is followed successively by 3.5～5 μ m, 5.5～7 μ m, 7.5～9 μ m, 9.5～11 μ m and 11.5～13 μ m, and spacing is 100～150 μ m.
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