TW593455B - Polysilsesquioxane-metal alkoxide hybrid film material, its preparation and use - Google Patents

Abstract

The present invention relates to a polysilsesquioxane-metal alkoxide hybrid film material, which possesses an excellent thermal stability and platness, low transmission loss and a controlled refractive index and thus is an excellent optical wave-guide material. The present invention also relates to a method for producing the polysilsesquioxane-metal alkoxide hybrid film material, which possesses the steps of (1) subjecting trialkoxysilane to hydrolyzing-condensation to form a polysilsesquioxane, (2) reacting the resultant poly-silsesquioxane with metal alkoxide to form a solution of polysilsesquioxane/metal alkoxide hybrid material; and (3) applying the solution of polysilsesquioxane/metal alkoxide hybrid material on a substrate and subjecting heat treatment to form a film. The present invention further relates to a use of the poly-silsesquioxane-metal alkoxide hybrid film material.

Description

593455 V. Description of the invention (1) One:-[Technical field to which the invention belongs] The present invention relates to a 4¾ SX ϊΙ > ^ m ^ species of t-half stone oxyfiring-metal burning gas porphyry, and shishi 2 into a thin film material With good thermal stability and 20% thin propagation of the compound ^ Controlling the refractive index is an excellent optical waveguide material :. The present invention is related to a method for preparing the polysemioxygen eyebrow mixed film material and the polysynthetic mixed film material as the light material material. H belongs to fired oxidation. [Previous Technology] Since the Corning fiber, the purpose is light. Only fiber is sufficient for speed. Constructed in the optical network video, video phone, video, image transmission, and the popularization of the Internet exhibition. These reliance requirements are also increasing due to bandwidth and more economical

Glass developed the first low-loss, all-optical network for transmitting information in 1970. It attracted the attention of the audience. The broadband and road services required to provide communication and various additional services also include Internet browsing, on-demand video Meetings, telemedicine consultations, documents, image database retrieval and calculation, etc. As technology advances and spreads, new applications and services continue to deliver volume information and instant response services. Bandwidth needs this. Multi-wavelength optical networks with larger capacity, easier management and distribution are needed to meet these needs. Claim. There are two important developments in multi-wavelength optical networks: (丨) broadband Erbium Doped Fiber Amplifiers (EDFAs), and (2) southbound, degree-division multiplexers (Dense Wave-Division)

Multiplexing, DWDM). Erbium-doped fiber amplifiers and high-density multiplexers have been widely used in backbone networks for long-distance communications, expanding bandwidth with minimal installation costs. However, due to the demand for bandwidth at the access end, 5935455 tends to be used. 5. Description of the invention (2) The service provider has extended the construction of erbium-doped fiber amplifiers and high-density multiplexers to the Metropolitan Area Netw. rk, MAW to solve the situation of network access end congestion. At the same time, it also promotes the ideal of all-fiber networks and fiber to the home (FTTH).

The important role played here is a novel communication component that can replace traditional expensive and time-consuming components. These components must meet high performance, mass production, high integration and accumulation, and most importantly, low unit price. , Low multi-wavelength fiber network construction cost. In the construction of a multi-wavelength optical network system centered on a high-density multiplexer, most of the planar optical waveguide elements (Planar Lightwave Ciruit (PLC), such as array waveguide grating Umyed Waveguide Grating, AWG) are used in semiconductors. Optical waveguides have been fabricated on substrates in industry with very mature technologies, so they have the most potential for capacity expansion, mass manufacturing, and low cost.

Optical waveguides are the basic components of planar optical waveguide components such as array waveguide gratings, light couplers, optical switches, gratings, optical amplifiers, optical modulators, and optical modulators. Because the transmission of light in an optical waveguide depends on the refractive index difference between the core layer and the coating layer, a channel optical waveguide of 10 μm × 10 μm is used as an example. The refractive index difference between the core layer and the coating layer is usually below 丨%, so A material that can precisely control the refractive index is required to make a high-quality optical waveguide. The way to make an optical waveguide is usually to first make a thin film of the light-guiding core layer on the substrate or the coating layer, and then use the cut or cast film to make the designed element pattern. Thin film manufacturing methods include Chemical Vapor

Deposition (CVD), Thermal Evaporation (Therfflai Evaporation),

Page 7 V. Description of the invention (3) ^ Sputtering, Flame Hydrolysis FHD, Spin coating, etc. Among the film-forming methods, the spin coating method is widely used because of its simplicity and low cost, and the wide variety of materials used. In the material of the optical waveguide prepared by the spin coating method, the organic material includes polymethyl acrylate (PMMA), polyimide, polycarbonate, and the like. Dehydrogenated poly (methyl propyl lysamide) I is often used to reduce the loss due to the formation of carbon-chlorine bonds in the near-infrared light band (1310nm and 1550nm) used in optical communications. Good water absorption: Due to its good thermal stability and low m, the chemically-immobilized polyimide is higher than the oxygen-dominated fiber. When the optical waveguide is connected, Fresnn fiber will be generated due to the large refractive index difference. Light loss. "Prepared by spin-coating method; because it can combine organic and two = 6: / two Italian, patent number: emissivity of optical waveguide materials. Other hybrid materials = ㈡ 可 ㈣ titanium oxide, poly (extended aryl radical) Titanium oxide, titanium oxide)-titanium oxide, polyimide-titanium oxide and: earth ether ketone)-silicon oxide · titanium oxide, etc. The station a ^ M vinylpyrrolidine 5934455 5. Description of the invention (4) Quality. In the application as an optical waveguide, the scattering loss caused by low roughness, 22 meets the surface flatness to reduce heat resistance. In general mixed materials, 1 controlled refractive index and good heat resistance are poor, at higher temperatures Shifen: ^: Organic polymer components usually degenerate early, which makes the material easily ^ The inorganic phase components contained in the material are more stable when used over time. H group 'reduces the material in view of the above disadvantages. The present invention, Therefore, the present invention has been completed. More extensive research on the first wave material [Content of the Invention] According to this, 'an object of the present invention is to provide an alkoxide mixed film material, which is a coincidence = a wide variety of silsesquioxane-metallic and Flatness, low propagation loss ^ film material Prepare a good thermally stable waveguide material. It is known that the light is lost and the refractive index can be controlled, so it is an excellent light. The second object of the present invention is a alkoxide mixed film material: method suit: dimeric sesquisiloxane-Jinyuan Hydrolytic condensation reaction to synthesize polysilses "= = The reaction of polysilsesquioxane obtained from cornerstone and metal burnt oxide; the reaction of sintering / metal halide oxide mixed with thallium oxide ♦ Silverstone oxidized on the substrate into a version Heat treatment to obtain the present, alkane-metal alkoxide mixed film material. & ". + Silicon Oxide The first purpose of this month is to provide the polyfold film material as an optical waveguide. The polysilsesquiox sintered-metal burnt oxide mixed thin film material of the present invention

5. Description of the invention on page 9 (5) It is a trihydroxanthine stone fired to firstly hydrolyze the green alkoxides in reverse storage. $, Θ # # "D becomes polysilsesquioxane and then forms with the metal. After forming the material solution, it is coated on the substrate and treated by the following method: = formed by the film material. Because the polysilsesquioxane itself has baking; J: ί: After mixing with the metal alkoxide to make a film ， It 1 η 歹 S 〇Η group 'after baking also has good surface flatness and low propagation loss at a wavelength of aeration, so it is excellent; The method of firing-metal firing oxide bismuth film material includes (1) hydrolyzing and condensing a trioxane oxide represented by formula R1Si (〇R2) 3 to synthesize polysilsesquioxane, and then 1) The obtained polysilsesquiox sintered and the metal burnt oxide of formula M (0R3) 4 are inverse f to obtain a solution of strictly polysilsesquioxane / metal alkoxide mixed material; and (3) ~ The mixed material solution is coated on a substrate to form a film and heat-treated, and the polysilsesquiox sintered _ metal dazzling oxide mixed film material of the present invention is made in two copies. Among the trisoxyoxylithoxanes shown by ^ 1Si (GR2) 3 used in the method, U_cyanoundecyl, m-methylphenethyl, p-ethylphenethyl, n- Octadecyl, ethoxymethyl, ethoxypropyl, N- (3-propenyloxy-2-hydroxypropyl) _3-aminopropyl, (3-propoxyloxypropyl) , 3- (N-allylamino) propyl, allyl, 4-aminobutane, (aminoethylaminomethyl) phenethyl 1_ (2_aminoethyl) _3_ Aminopropyl, N- (6-aminohexyl) aminopropyl, 3- (m-aminophenoxy) propoxy, m-aminophenyl, p-aminophenyl, 3_ ( 3-aminopropyloxy) -3,3-dimethylpropane, 3-aminopropyl, 6-azido

Page 10 593455 V. Description of the invention (6) Hexyl, phenylfluorenyloxypropyl, benzyl, 5- (dicycloheptenyl), bis (2-hydroxyethyl) -3-aminopropyl Group, bis (glutarate) titanium-bis (oxyethyl) aminopropyl group, o-bromophenyl group, m-bromophenyl group, p-bromophenyl group, 3-> styropropyl group, 11- Molybdenyl, butylamyl, n-butyl, methenyl, 2-chloroethyl, p-methyl, m- (p-methyl) phenethyl, p-'(chloromethyl) phenethyl, (Chloromethyl) phenyl, chlorophenyl, 3-chloropropyl, 2- (4-chlorosulfonamidophenyl) ethyl, 2-cyanoethyl, 3-cyanopropyl, 2- ( 2-cyclohexenyl) ethyl, cyclohexyl, 2- (cyclohexyl) ethyl, 3-cyclopentadienylpropyl, cyclopentyl, n-decyl, di-third butoxyaluminum oxide N, N-diethyl-3 -aminopropyl, diethylphosphonoethyl, N, N-dimethylaminopropyl, 3- (2, 4-dinitrophenyl Amino) propyl, 2- (diphenylphosphonium) ethyl, 21-difluorenyl alkenyl (docoseny 1), dodecyl, 2- (3, 4-epoxycyclohexyl), 5, 6-epoxyhexyl, Methyl, 3-glycidyloxypropyl, heptafluorodecyl, hexadecyl, hexyl, N- (hydroxyethyl) -N-fluorenylaminopropyl, trimethyl, 3-ethylidene , Isobutyl, 3-isocyanatopropyl, isooctyl, 3-hydrothiopropyl, N- (3-methylpropyloxy-2-hydroxypropyl) -3 aminoaminopropyl Methyl, methacryloxymethyl, I-based allyloxypropyl, 2-methoxy (polyethyloxy) propyl, 3-monomethoxypropyl, N-fluorenylaminopropyl , Methyl, nonyl, n-octadecyl, 1,7-octadienyl, 7-octylfluorenyl, n-octyl, pentafluorophenylpropyl, pentyl, phenethyl, N- Phenylaminopropyl, phenyl, n-propyl, isopropyl, styrylethyl, 3- (N-styrylmethyl-2-aminoethylamino) propyl, 3-thio Cyanatopropyl, p-tolyl, tridecyloctyl, 3, 3, 3-trifluoropropyl, ureidopropyl, vinyl, ethoxyethyl

Page 11 593455 V. Description of the invention (7) group, allyloxyundecyl, N-3 -amino (polypropoxy) aminopropyl, N-2 -aminoethyl-11 -Amino group "I-alkyl, n-butylaminopropyl, diethylaminomethyl, N-ethylamino isobutyl, pentafluorophenyl, perfluorodecyl and perfluorotetradecane base. In the trialkoxysilane represented by the formula FSi (OR2) 3, the R2 group may be the same or different and are other representative of a Cu group, a C2_6 group, a C2_6 group, a phenyl group, and a di-C group. base.

In the trialkoxysilane shown by the formula RiSi (OR2) 3, the (6-6 alkyl group represented by the R2 group includes a linear or branched alkyl group, such as methyl, ethyl, n-propyl, isopropyl, and n-butyl. Group, second butyl group, third butyl group, n-pentyl group, octyl group, n-hexyl group and the like. Examples of the alkanoyl group represented by the R2 group in the trialkoxysilane represented by the formula WSUOR2: ^ are, for example, Acetyl, propionyl, butylfluorenyl, pentamyl, hexamethylene and the like. Trialkoxysilanes represented by the formula WSiCOR2) 3. Examples of the alkenyl group represented by the R2 group are, for example, vinyl, alkenyl Propyl, propionyl, butenyl, pentenyl, hexenyl and the like.

Examples of the R2 group in the trialkoxysilane represented by the formula PSUOR2: ^ —q 6 alkyl radicals are examples of dimethyl sulfanyl, diethyl sulfanyl, dipropylsilyl , Dibutylsilyl, dipentylsilyl, dihexylsilyl and the like. Μ in the metal oxide of the formula M (0 R3 \ represents metal such as Chin (τ i), W (Ge), Sn (Sn), and bait (Er), and the R3 group represents (^ 6 alkyl, ( ^ Alkino, C24 fluorenyl, phenyl, and di-Chalkylsilyl, each of which is shown by R3

Page 12 593455 V. Description of the invention (8) "Based on the definition shown in the aforementioned R2. The method for preparing a polysilsesquioxane-metal alkoxide mixed film material t according to the present invention is to perform a reaction in a solvent having good solubility for both polysilsesquioxane and metal alkoxide, and a solvent can be used. It includes, for example, tetrahydrofuran, aeroform, hexane, pyridine, methyl isopropyl ketone 'or a mixed solvent thereof. The polysilsesquioxane-metal alkoxide mixed film material of the present invention. Change the ratio of the added metal alkoxide to polysilsesquine :: Control: The refractive index of the mixed film material is obtained. According to this, the ratio of 4 = t siloxane to metal alkoxide in the present invention is not particularly limited, and can be selected according to the refractive index required for the thin film material. Material preparation: Polysemisparite oxy-firing-Metal Oxide mixed film, the mixed material solution is coated on the substrate by a spin coating method, a spin coating method, and a roll coating method. ), Flow coating method (〇w⑽㈣), dip coating method, Harbin coating you, and soil, ^^ McurtaingC0 ^ # ^ S ^ — the substrate suitable for the method of the present invention includes a silicon-based ceramic circuit Substrates, multi-layer membranes, and ceramic materials are used as substrate materials. Substrate film substrate, copper / polyimide group Step ^ q + 埶 treatment in the method of the present invention. At least Xiao #) ”, thermal processing to different temperatures for multiple steps to V include solvent removal steps, ten steps of pre-shrinking car and car, and removal of residual _ A and 譃 & Refining the reaction step. Residual radicals and steps to ensure the complete cross-linking condensation reaction This solvent removal step can be carried out at a temperature of, for example, 50, t. · Pre-η plane, page 13, 593455 V. Invention Note (9) The condensation step can be performed at, for example, 1 30- 1 65. (: between temperatures; the condensation reaction step can be performed at, for example, 220-270 ° C; The step of completing the crosslinking condensation reaction can be performed at a temperature of, for example, 350-450 ° C. The present invention will be further illustrated by the following examples, but these examples are only used to illustrate the present invention and not to limit the present invention. Range: Example 1 Preparation and testing of a (nolly (methvlsilsesauioxane)) film (4.08 g (0.03 mol) methyltrimethoxysilane and 9 · 24 grams of methyl is obutyl ketone (ΜΙΒΚ) In a three-necked flask cooled in an ice bath, 0.88 g of hydrochloric acid / deionized water (0094 wt%) was dissolved in 5.13 g of tetrahydrofuran (THF), and the resulting hydrochloric acid / deionized water in THF was dissolved. The solution was slowly dropped into the three-necked flask over a period of 30 minutes. The pH of the reactants in the three-necked flask was maintained at about 3, while the molar ratio of water to methyltrimethoxystone was maintained at about 1 · 625. After the completion of the dropwise addition of the THF solution of hydrochloric acid / deionized water, the three-necked flask was taken out of the ice bath, and the temperature was raised to room temperature in about 5 minutes. The solution was placed in a silicone oil at a constant temperature of 60 t for hydrolysis. The condensation reaction was carried out for 3 hours, during which nitrogen was passed and refluxed through a condenser. The product after completion of the reaction was called solution (A). Solution (A) was spin-coated on a silicon wafer at a rotation speed of 3000 rpm for 40 seconds. After curing at 80 ° C, 150 ° C and 250 ° C, and passing nitrogen gas into the furnace tube, it is cured at 4Q °. The poly (methylsilsesquioxane) (PMSq) obtained after curing ) The film was measured with an n & k analyzer-its thickness was 0 · 12 microns, and its surface was measured with an atomic force microscope (AFM)

Page 14 593455 V. Description of the invention (ίο) The average roughness Ra is 0.4 nm. The root-mean-square roughness Rq was 0.51 nm. The refractive index of this PMSQ thin film at 632.8 nm was measured using a rubidium coupler to be 1.395. The obtained PMDQ has a cage structure and was measured with an X-ray single crystal diffractometer. The bond length was 1.617 Angstroms and the bond angle was 186.86-149.38 degrees. Fourier transform infrared spectroscopy (FTIR) was used to identify the structure of PMSQ, showing that PMSq has a cage-like and network-like mixed structure. The Si-O-Si absorption peak of the cage structure is located at 1120 cm-1, and the Si-O-Si absorption peak of the network structure is located at 〇30 cm-1. 19Si nuclear magnetic resonance (NMR) verification of the PMSQ has the following structural formula:

In the above structure of the PMSQ obtained in Example 1, R represents a methyl group, and R represents a chlorine or a methyl group. In addition, the thermal gravimetric analyzer (TGA) and thermal differential scanning card meter (DSC) analysis results show that the film has a uniform stability at a temperature of 400 ° C or above. Example 2 Blends of trimethyloloxyxane) with titanium vaporized hind limbs. 222 g of the solution (A) prepared in the above Example 1 was fed into a three-necked flask. In addition 3.06 grams of tetra-n-butoxide was dissolved in 12.80 grams of thf. The obtained THF solution of tetra-n-butoxide was slowly added dropwise to the 593455 containing the solution (A). 5. Description of the invention (11) The three-necked flask was reacted at 60 ° C for 1 hour at a constant temperature. Then 18.0 g of THF was added. In order to increase the degree of condensation of tetra-n-butyrate titanium oxide, another 0. 0 8 1 g of deionized water was added. After completion, the resulting solution was cooled to room temperature, and then the solution was concentrated to a higher solid content in a usual manner to obtain a product solution (B). The solution (B) was applied on a single polished wafer, a double polished wafer, and a quartz wafer by spin coating method to perform quality measurement. The condition of spin coating was 1 500 rpm, which lasted for 40 seconds. After coating, the plates were heated and baked for 30 minutes at 80 ° C, 150 C, and 250 C, and then the test pieces were placed in a high-temperature nitrogen furnace and baked at 400 ° C for 1 hour. . The molar ratio of tetra-n-butoxide and PMSQ is 0.3. The thickness of the film obtained after baking is 丨 · 6 microns, the average roughness (Ra) is 0.31 nm, and the root-mean-square roughness (^ ㈧ is ^ 43 nm, which has good flatness. It is used as a 稜鏡 coupler Wavelength ^ "Nano-laser measurement film refractive index is 丨 · 455. Based on TGA and measurement results, it can be found that the thermal cracking / m degree of the polymethylsilsesquioxane / titanium oxide mixed material of the present invention is between Above 50 ° C and above 0 ° C, and the material still remains above 95% when heated to 900 ° C. DSC measurement results found that no significant glass transition temperature exists. Titanium oxide blended ^ Y * FE-SEM photograph (Figure i) with excellent thermal stability properties Found sheet = polymethyl polysesquisene oxide sintered by the voxel, mixed with a thin film material: titanium The UXRD pattern of the chain size below 10 nanometers (Figure 2) shows that there is no crystalline phase anatase or rutile in the burned titanium oxide in the mixed film material of this invention. In addition, the UV / visible light Figure (Figure 3) can be seen in the present invention ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ Continuing continuation Ke + + 3 water methyl times + silicon alkane / titanium alkoxide., The band edge of 蚪 is 291 nm.

Page 16, 455, 455 5. Description of the invention (12) Absorption. From the osmium, xrdauv / visible light spectrum (1st to 3rd j ... the results show that the mixed film material prepared by the present invention has good moonlight 'suitable as an optical waveguide material. The polymethyl sesquihalide prepared according to Example 1 Siloxane solution (A) Fish four _ positive _ like ϊϊ ϊϊ 方式 mixed in the manner described in Example 2 to obtain a mixed solution, and according to titanium-like family I I into a variety of different composition ratio of the film, of which 4-n-butoxide 0 6 Λ The weight percentage of basal sesquioxane (PMSQ) is controlled to 0.1 to the appropriate test example 1 ifei Gan 'Γ " Γ > + shot two = various films obtained using a prism handle coupling at 1319 too + titanium oxide Percentage weight rb Y ^ 4 graph / jin. The X-axis substitution of the film refractive index η in Figure 4. The relationship between the V-reduction rate and the sexual relationship. With the reset percentage of the weight of titanium oxide, a line is formed. Titanium alkoxide in the cured film? 6 5. (Note: Calculated due to heating (hydrolysis of oxidized titanium oxide reduces to emulsified 1 and therefore weight 100 ΐ)) / (hydrolysis and condensation of titanium alkoxide Takashiri (and titanium oxide) Weight (weight) χ 10 0%). 篁 4 ^ PMSQ after hydrolysis and condensation complete emissivity η and titanium oxide in Fig. 4 ,,, percent amount of regression of the experimental points, can be folded η = 0 · 0 0 527χ + 1 · 32792 regression; ^ relationship represented by the following formula:. U unloading crane R is the number of square-96050.

$ 17 页 593455 V. Description of the invention (13) t Examination example 2. Alkane / fired oxidation ^^ formed into a thin film sealing oblique ..., the polyfluorenyl silsesquioxane / titanium alkoxide mixture obtained in Example 2 The structure of the thin film material is identified using FTIR. The characteristic absorption peaks of all polyfluorenyl silsesquioxanes are as in the examples! As shown. The FTIR spectrum (figure 5) shows that the absorption peak at 220 ° C is located at 92 ° CD1 1. At the same time, the intensity of this absorption peak increases with the increase of =: 篁, and it can be confirmed that titanium has successfully reacted to bond to the polyformate. Base silsesquioxane. Its structural formula is as follows: / Si-O-Si: sMsS? R > f 〇. \ 0, ； Si-0--Si

• R-Si4n0H

-Si ~ R HO Experimental Example 3 Determination of Peach Loss of Peach by Using 4a Titanium Mixed Plate According to the process shown in Fig. 6, the thin composite material is prepared into an optical pattern, and the flow chart of the planar waveguide and the guide: (6) (A) flow chart. Among them, the A (B) thick layer (VB) pattern is used to make the channel waveguide. The material has a low refractive index, so that Guli can be used as the core layer. B allows the first wave to be totally reflected in the core layer. Article 6 (A)

P.18 5935455 5. Description of the invention (14) In the figure, I 2 micron silicon dioxide is deposited on the silicon wafer as the substrate 1 and the coating layer 2 is used to make the various polymethylsilsesquioxane obtained in Example 3 An alkane / cadaverine mixed solution was applied thereon to form a film 3 to obtain a planar waveguide. (B ^ In the figure, firstly, silicon dioxide is deposited on a silicon wafer serving as a substrate, and as a coating layer 2, an optical waveguide layer 3 is coated on the coating layer 2, and then a hard mask layer is covered. 4. Next, lithographic etching is used to etch the mask layer other than the desired pattern, leaving a hard mask layer corresponding to the pattern. 4, and then etching the optical waveguide layer other than the desired pattern to leave 3 corresponding to the pattern. Then, the hard mask layer 4 is removed, and then a coating layer 22 is deposited thereon, and the channel waveguide of the present invention is used. The etching used in the manufacture of the waveguide may include, for example, reactive ion etching, laser, etc. User ablation, electron beam direct writing method (seven writing), embossing, and wet etching (^ 七 etching), etc. The details of these etching processes are well known The technical knowledge is not repeated here. The obtained waveguide uses the cut_b = k method to measure the optical transmission loss (opticai 10SS) of the waveguide at a wavelength of 319 nm. The obtained optical transmission loss data is relative to The percentage of oxygenated titanium oxide is plotted in the 'cardiogram'. It can be seen that the weight percentage of chemical titanium increases and decreases, for example, the weight percentage of oxidized titanium: 25 · 45 Wt% to Hi wt% 'The optical transmission loss is reduced from Q.3idB / to 0.18 dB / Cm. From these results It is shown that the polymethylsilsesquioxane // fired titanium oxide mixed film material of the present invention has low optical transmission loss and is sufficient as an optical waveguide. 593455 V. Description of the Invention (15) The invention has been described by the above-mentioned specific example, but This is a preferred embodiment of the present invention, and does not mean that the present invention is limited to the π can be used for a long time. You can do all kinds of decoration, modification and iron / bull without departing from the spirit and scope of the present invention. , Xiwangjiu the scope of the present invention. &Amp; changes

Page 20593455 Brief description of the diagram 1L Brief description of diagram • The first diagram is an FE-SEM photograph of the polysilsesquioxane-metal alkoxide mixed film material obtained in Example 2 of the present invention; the second diagram is The XRD pattern of the polysilsesquioxane-metal sintered oxide mixed film material obtained in Inventive Example 2; 'Figure 3 is the polysilsesquioxane-metal alkoxide mixed film obtained in Example 2 of the present invention UV / visible light spectrum of the material;

FIG. 4 is a relationship diagram between the content of titanium alkoxide in the polysilsesquioxane-metal alkoxide mixed film material obtained in Example 3 of the present invention and the refractive index of the film material at 3 j 9 nm; Fig. 5 is an FT IR spectrum of the polysilsesquioxane-metal alkoxide mixed film material obtained in Example 2 of the present invention; and Fig. 6 is a diagram of the polysilsesquioxane-metal alkoxide using the present invention Flowchart for making optical waveguides by mixing thin film materials, of which the flowchart of Fig. 6 (A) is used to make planar optical waveguides and the flowchart of Fig. 6 (B) is used to make channel optical waveguides; and Fig. 7 This is a graph showing the relationship between the titanium oxide content in the courtyard of the polysilsesquioxane-metal alkoxide mixed film material and the light transmission loss of the film material at 1319 nm.

Description 1 Shi Xi wafer substrate 2, 2 2 Cover layer 3 Core layer 4 Hard mask layer

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Claims (1)

State 455, patent application scope Method for preparing the polysilsesquioxane-metal alkoxide mixed film material 'including (1) making a trialkoxy stone represented by the formula R1Si (〇R2) 3 = hydrolytic condensation reaction to synthesize polysilsesquioxane Siloxane, (2) reacting the polysilsesquioxane obtained in the step with a metal alkoxide of formula M (〇R3) 4 to 'obtain a solution of a polysilsesquioxane / metal alkoxide mixed material' and (3) The mixed material solution is coated on a substrate to form a film and subjected to heat treatment to obtain a polysilsesquioxane-metal alkoxide mixed film material; in the formula WSi (OR2) 3, R1 represents u-cyano Undecyl, m-methylphenethyl, p-ethylphenethyl, n-octadecyl, ethoxymethyl, acetoxypropyl, N_ (3-propyloxy- 2-Aminopropyl) -3 -aminopropyl, (3-propenyloxypropyl), 3- (N_allylamino) propyl, amidopropyl, 4-aminobutyl, (Aminoethylaminomethyl) phenethyl, N- (2-aminoethyl) -3-aminopropyl, n- (6-aminohexyl) aminopropyl, 3- (m- Aminophenoxy) propoxy, m-aminophenyl, p-aminophenyl, 3- (3 -Aminopropoxy) -3,3-dimethyl-1-propenyl, 3-aminopropyl, 6-nitrosinofluorenylhexyl, benzyloxypropyl, benzyl Group, 5- (biscycloheptyl), bis (2-ethylethyl 3-aminopropyl, bis (glutarate) titanium-〇, 〇, -bis (oxyethyl) aminopropyl , O-bromophenyl, m-bromobenzyl, p-mophenyl, bromopropyl, 11-bromofluorenyl alkyl, butenyl, n-butyl, carboxymethyl, 2-chloroethyl, chlorofluorene Base, m- (chlorofluorenyl) phenethyl, p- (chloromethyl) phenethyl, (p-methyl) phenyl, p-phenyl, 3-p-propyl, ... 2-(4-chlorostone Flavophenyl) ethyl, 2-cyanoethyl, 3-nitropropyl 593455 VI. Patent application scope, 2- (2-cyclohexenyl) ethyl, cyclohexyl, 2- (cyclohexyl) ethyl •, 3-cyclopentadienylpropyl, cyclopentyl, n- Decyl, di-third-butoxymethyloxy, N, N-diethyl-3-aminopropyl, diethyllinylethyl, N, N-dimethylaminopropyl, 3- (2,4-dinitrophenylamino) propyl, 2- (diphenylphosphonium) ethyl, 21-docosenyl, dodecyl, 2- ( 3,4-epoxycyclohexyl), 5,6-epoxyhexyl, ethyl, 3-glycidoxypropyl, heptafluorodecyl, cetyl, hexyl, N- (hydroxyethyl Methylmethylaminopropyl, hydroxymethyl, 3-iodopropyl, isobutyl, 3-isocyanatopropyl, isooctyl, 3-hydrothiopropyl, N_ (3-methacryloxy 2-Hydroxypropyl) -3-aminopropyl, fluorenylpropenylfluorenyl, methacryloxypropyl, 2-fluorenyl (polyethoxy) propyl, 3- Methoxypropyl, N-fluorenylaminopropyl, methyl, nonyl, n-octadecyl, 1,7-octadienyl, 7-octenyl, n-octyl, pentafluoro Phenylpropyl, Amyl, phenethyl, N-phenylaminopropyl, phenyl, n-propyl, isopropyl, styrylethyl, 3- (N-styrylmethyl-2-aminoethylamine Propyl), propyl, 3-thiocyanatopropyl, p-tolyl, tridecylfluorooctyl, 3, 3, 3-trifluoropropyl, ureidopropyl, ethenyl, acetoxyethyl Allyloxy, allyloxy ^ -alkynyl, N-3 -amino (polypropoxy) aminopropyl, N-2 -aminoethyl-1 propylamino undecyl, n- Butylaminopropyl, diethylaminomethyl, N-ethylaminoisobutyl 'pentafluorophenyl, perfluorodecyl and perfluorotetradecyl; R2 can be the same or different and each represents (V6 Alkyl, C2_6 alkylfluorenyl, C2_6 fluorenyl, phenyl and di-Cualkyl radicals; Page 23 593455 VI. Application for Patent Scope: Alkenyl and benzene formed by formula M (OK '(Er)) 2. If the special steps for the application include steps and steps. 3 · If the application should be in solution 4. If the application is for special Phosphorus and chloroform agents. 5. For example, the application of monooxane and gold refractive index. 6. For a polycondensation application, such as the application of a special film, such as the application of a mixed film) 4, M is selected from titanium (Ti), germanium (Ge), The group of tin (Sn) and fluorene, and the R3 group represent (: 6 alkyl, C 2-6 alkyl fluorenyl, c 2, 6 and di-Cy alkyl silyl groups. The method of item 1 in which the steps ( 3) The method of heat treatment solvent removal step, pre-condensation step, condensation reaction step to remove the residual hydroxyl groups in the film and ensure the complete range of the cross-linking condensation reaction, the method of item 1, wherein steps (丨) and (2) are performed in the reverse agent The method of the third item, wherein the solution is selected from the group consisting of tetrahydrofuran, hexane, pyridine, methyl isopropyl ketone, or a mixed solution thereof: the method of the first item, wherein the polysilsesquioxane is controlled by An oxide-mixed film material that is a mixture of alkoxides and can be controlled into a film material is prepared by the method of item Lev yoke around sesquicarbonates poly silicon alloy material of alumoxane _ 6, the optical waveguide-based material by Van emulsion