CN112723754A - Lead zirconate titanate film facing next-generation high-speed communication and preparation method and application thereof - Google Patents
Lead zirconate titanate film facing next-generation high-speed communication and preparation method and application thereof Download PDFInfo
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- CN112723754A CN112723754A CN202110008078.8A CN202110008078A CN112723754A CN 112723754 A CN112723754 A CN 112723754A CN 202110008078 A CN202110008078 A CN 202110008078A CN 112723754 A CN112723754 A CN 112723754A
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- 229910052451 lead zirconate titanate Inorganic materials 0.000 title claims abstract description 106
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000004891 communication Methods 0.000 title claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 89
- 239000010408 film Substances 0.000 claims abstract description 70
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000010409 thin film Substances 0.000 claims abstract description 33
- 239000000758 substrate Substances 0.000 claims description 69
- 229940046892 lead acetate Drugs 0.000 claims description 57
- 239000010936 titanium Substances 0.000 claims description 56
- 238000004528 spin coating Methods 0.000 claims description 43
- 239000002243 precursor Substances 0.000 claims description 41
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 26
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 25
- 239000010703 silicon Substances 0.000 claims description 25
- 238000000137 annealing Methods 0.000 claims description 24
- 238000004140 cleaning Methods 0.000 claims description 20
- 239000002738 chelating agent Substances 0.000 claims description 19
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 229910052710 silicon Inorganic materials 0.000 claims description 17
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 14
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 claims description 13
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- 238000005253 cladding Methods 0.000 claims description 8
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 6
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 6
- XQBXQQNSKADUDV-UHFFFAOYSA-N lanthanum;nitric acid Chemical compound [La].O[N+]([O-])=O XQBXQQNSKADUDV-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 6
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 6
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims description 5
- QUVMSYUGOKEMPX-UHFFFAOYSA-N 2-methylpropan-1-olate;titanium(4+) Chemical compound [Ti+4].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] QUVMSYUGOKEMPX-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 239000007772 electrode material Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 6
- 230000003287 optical effect Effects 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000009022 nonlinear effect Effects 0.000 abstract 1
- 230000005676 thermoelectric effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 170
- 238000010438 heat treatment Methods 0.000 description 51
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 38
- 238000001816 cooling Methods 0.000 description 32
- KQNKJJBFUFKYFX-UHFFFAOYSA-N acetic acid;trihydrate Chemical compound O.O.O.CC(O)=O KQNKJJBFUFKYFX-UHFFFAOYSA-N 0.000 description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000009987 spinning Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 238000007789 sealing Methods 0.000 description 11
- 229910052594 sapphire Inorganic materials 0.000 description 10
- 239000010980 sapphire Substances 0.000 description 10
- 229910052814 silicon oxide Inorganic materials 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 description 8
- 238000001259 photo etching Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 6
- 238000005530 etching Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 4
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- ZJJWXAUNWSORPB-UHFFFAOYSA-N propan-2-ol;zirconium Chemical compound [Zr].CC(C)O ZJJWXAUNWSORPB-UHFFFAOYSA-N 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- VQVDTKCSDUNYBO-UHFFFAOYSA-N neodymium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VQVDTKCSDUNYBO-UHFFFAOYSA-N 0.000 description 2
- 238000000206 photolithography Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 description 2
- HDCOFJGRHQAIPE-UHFFFAOYSA-N samarium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HDCOFJGRHQAIPE-UHFFFAOYSA-N 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical compound CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
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- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C03C17/27—Oxides by oxidation of a coating previously applied
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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Abstract
The invention discloses a lead zirconate titanate thin film facing next-generation high-speed communication, a preparation method and application thereof. The method has the advantages of simple operation, low energy consumption and low cost, and the grown film is a pure perovskite type single-phase crystal film, has high transparency and high temperature resistance, is easy to adjust the thickness and the size of the film, and can meet the requirements of various electro-optical modulation devices. The thin film lead zirconate titanate prepared by the invention has nonlinear effect, electro-optic effect, piezoelectric effect, thermoelectric effect and the like, and can be used for preparing optical waveguides, optical switches, beam splitters/combiners, piezoelectric modulators, thermoelectric modulators, electro-optic modulators and other devices in integrated photonic circuits.
Description
Technical Field
The invention relates to the field of integrated photonic communication, in particular to a lead zirconate titanate film oriented to next-generation high-speed communication, and a preparation method and application thereof.
Background
Lead zirconate titanate (PZT) is a multifunctional material with large piezoelectric and electrooptical coefficients, high dielectric constant and significant remanent polarization, showing its excellent properties in piezoelectric, electrooptical and pyroelectric fields. Therefore, the lead zirconate titanate has wide application in a plurality of fields such as sensors, micro-electro-mechanical systems, electro-optical modulators, ferroelectric memories and the like. However, the preparation of a compact, uniform, crack-free, highly transparent, highly electro-optic effect PZT crystal film has been a great challenge, and especially the preparation of a thin film that can be used for an electro-optic modulator has been a difficulty. The performance of the PZT thin crystal film is closely related to the composition, texture, phase structure and the like of the film. Therefore, the preparation of high-quality PZT thin films with large electro-optic effect has important significance for the electro-optic field.
The preparation method of the PZT film at present mainly comprises a solid phase method: including magnetron sputtering, pulsed laser deposition, molecular beam epitaxy, etc.; liquid phase method: hydrothermal method, sol-gel method, etc. The solid phase method generally uses expensive equipment, the atomic ratio is difficult to control, the quality of the film depends on the target material seriously, and the size of the film is limited; the hydrothermal method has complex preparation process and harsh conditions. Has certain limitation in practical application. At present, most PZT thin film seed crystal layers adopt platinum and titanium, and the application of the PZT thin film seed crystal layers in the field of electro-optic is severely limited due to the absorption of the platinum and the titanium to light, and the lead titanate (PT) is used as the seed crystal layer, so that the single-phase crystal thin film with advantageous orientation is difficult to prepare, and the electro-optic effect is difficult to obtain.
Disclosure of Invention
Aiming at the defects of the prior art, the invention discloses a lead zirconate titanate film and an electro-optic modulator for next-generation ultrahigh-speed communication (in the field of integrated photonics). And then, designing and optimizing a device structure, and preparing a series of electro-optic modulation devices through micro-nano processing technologies such as photoetching, etching and the like.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a lead zirconate titanate film facing next-generation high-speed communication comprises the following steps:
(1) substrate cleaning
Cleaning the substrate, removing organic and inorganic impurities on the substrate, and drying; the substrate is an inorganic substrate or a composite substrate formed by growing an inorganic film on the inorganic substrate;
(2) disposing a seed layer solution
Dissolving lanthanide nitrate in n-propanol or ether alcohol solvent to obtain lanthanide nitrate solution as seed crystal layer solution;
(3) preparation of lead zirconate titanate PbxZryTi1-yO3Precursor solution
Firstly, preparing a lead acetate solution, wherein the solute is lead acetate, and the solvent is an ether alcohol solvent; then dissolving any one of tetraethyl titanate, isopropyl titanate or tetraisobutyl titanate in a lead acetate solution according to the atomic ratio in the chemical formula, dripping a zirconium n-propoxide or zirconium isopropoxide solution according to the atomic ratio in the chemical formula, and uniformly stirring; finally, dropwise adding acetylacetone as a chelating agent, fully stirring to obtain a chelated lead zirconate titanate precursor solution, and sealing and standing;
(4) preparing a seed layer
Dripping the seed crystal layer solution prepared in the step (2) on the substrate cleaned in the step (1), and then sequentially carrying out spin coating and pyrolysis treatment to prepare a seed crystal layer; the thickness of the film is adjusted by adjusting the spin-coating speed and the spin-coating times in the preparation process;
(5) preparation of lead zirconate titanate film
Dripping the lead zirconate titanate precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), and sequentially performing spin coating and annealing treatment to prepare a lead zirconate titanate crystal film; the thickness of the film is adjusted by adjusting the spin-coating speed and the spin-coating times in the preparation process.
Further, in the step (2), the concentration of the prepared lanthanide nitrate solution is 0.01-0.4 mol/L;
in the step (3), the concentration of the prepared PZT precursor solution is 0.02-1.0 mol/L.
Further, in the step (4), the pyrolysis temperature is 200-450 ℃;
in the step (5), the annealing temperature is 500-850 ℃.
Further, in the step (3), lead zirconate titanate PbxZryTi1-yO3In the precursor solution, x is 1.0-1.5, and y is 0.2-0.8.
Further, in the step (3), the amount of the added chelating agent acetylacetone is 0.5-8% of the total volume.
In the step (1), the substrate is selected from silicon, aluminum oxide, magnesium oxide, glass, or a composite substrate formed by growing any one of silicon nitride, silicon dioxide, titanium dioxide, and aluminum nitride on an inorganic substrate.
Further, the ether alcohol solvent in the step (2) and the step (3) is selected from any one or more of ethylene glycol methyl ether, diethylene glycol methyl ether, ethylene glycol ethyl ether and the like.
A lead zirconate titanate thin film prepared by any one of the above preparation methods.
An electro-optical modulator made of a lead zirconate titanate film is characterized in that a cladding film or a strip waveguide or a Mach-Zehnder structure is prepared on the lead zirconate titanate film through a micro-nano processing technology, and a corresponding electrode structure is prepared to obtain the corresponding electro-optical modulator.
Furthermore, the material of the cladding film is SiO2、TiO2Or Si3N4The strip waveguide and Mach-Zehnder structure are made of lead zirconate titanate (PZT) and SiO2、TiO2、Si3N4The electrode material adopts gold, silver, copper, titanium, aluminum and nickel.
The invention has the following beneficial effects:
(1) the preparation method of the lead zirconate titanate film is simple to operate, low in energy consumption and low in cost;
(2) the film grown by the method is a pure perovskite type single-phase crystal film, has high transparency and high temperature resistance, is easy to adjust the thickness and the size, and can meet the requirements of various electro-optical modulation devices.
(3) The prepared PZT film is applied to an electro-optical modulator, has good compatibility, an electro-optical coefficient of 68-280pm/V and a modulation bandwidth of 10-100GHz, and has huge application prospect in the field of future integrated photonic communication
Drawings
FIG. 1 is the XRD profile of the thin film of the seed layer prepared by multiple spin coating in example 3;
FIG. 2 is an XRD plot of a lead zirconate titanate thin film prepared by multiple spin-coating processes in example 3;
FIG. 3 is an XRD plot of a lead zirconate titanate thin film prepared in example 5;
FIG. 4 is a schematic diagram of a waveguide structure designed for the electro-optic coefficient test of embodiment 10;
FIG. 5 is an electron micrograph of a slab waveguide prepared in example 10;
FIG. 6 is a graph showing the light extraction test of the slab waveguide prepared in example 10, using a 1550nm semiconductor laser as the light source.
FIG. 7 is a SiO thin film based on lead zirconate titanate prepared in example 112The structure of the ridge waveguide is shown schematically.
FIG. 8 is a SiO thin film based on lead zirconate titanate prepared in example 122The structure of the ridge waveguide is shown schematically.
FIG. 9 is SiO for lead zirconate titanate-based film prepared in example 112And (3) selecting a 1550nm semiconductor laser as a light source for a light-emitting test pattern of the ridge waveguide.
FIG. 10 is a schematic view of a waveguide of the structure of upper and lower electrodes based on a lead zirconate titanate thin film prepared in example 13.
FIG. 11 is a schematic view of a waveguide of the structure of upper and lower electrodes based on a lead zirconate titanate thin film prepared in example 14.
FIG. 12 is a schematic structural view of a lead zirconate titanate thin film-based ridge waveguide prepared in example 15.
FIG. 13 is a schematic view of the Mach-Zehnder structure based on lead zirconate titanate thin film prepared in example 16
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and preferred embodiments, and the objects and effects of the present invention will become more apparent, it being understood that the specific embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
(1) Washing the glass substrate with deionized water, then sequentially ultrasonically cleaning the glass substrate with acetone, deionized water and isopropanol for 10 minutes, and then drying the glass substrate in a drying oven at 85 ℃ for later use;
(2) dissolving lanthanum nitrate in n-propanol solution to prepare seed crystal layer solution with the concentration of 0.02mol/L, and sealing for later use;
(3) according to Pb1.0Zr0.2Ti0.8O3Dissolving lead acetate trihydrate into diethylene glycol monomethyl ether to prepare a lead acetate solution; then tetraethyl titanate is reacted with Pb1.0Zr0.2Ti0.8O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.0Zr0.2Ti0.8O3The isopropanol zirconium solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, 0.5 percent of acetylacetone as a chelating agent is dripped into the solution and fully stirred to obtain a precursor solution after chelating; the concentration is 0.04mol/L, and the mixture is sealed and kept stand for later use;
(4) dripping the lanthanum nitrate crystal seed layer solution on the cleaned glass substrate, sequentially spinning at 500rpm and 3500rpm, pyrolyzing at 200 ℃ for 30min, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, and the thickness is about 2 nm;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), pyrolyzing at 200 ℃ for 30min and annealing at 500 ℃ for 20min sequentially at 500rpm and 3000rpm, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, and the perovskite crystal film is prepared, the thickness is about 5nm, and the target thickness can be prepared by repeated spin coating.
Example 2
(1) Soaking a sapphire substrate with concentrated sulfuric acid, washing with deionized water, then sequentially ultrasonically cleaning with acetone, deionized water and isopropanol for 10 minutes, and then drying in a drying oven at 85 ℃ for later use;
(2) dissolving neodymium nitrate in ethylene glycol monomethyl ether solution to prepare neodymium nitrate seed crystal layer solution with the concentration of 0.04mol/L for later use;
(3) according to Pb1.1Zr0.65Ti0.35O3Dissolving lead acetate trihydrate into ethylene glycol monomethyl ether, and dissolving lead acetate in the solution; then adding isobutyl titanate to the mixture according to Pb1.1Zr0.65Ti0.35O3Is dripped into the lead acetate solution according to the atomic ratio of the lead acetate and then is added according to the Pb1.1Zr0.65Ti0.35O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, acetylacetone with the volume ratio of 2% is dripped as a chelating agent, the mixture is fully stirred to obtain a chelated PZT precursor solution with the concentration of 0.2mol/L, and the solution is sealed and kept stand for later use;
(4) dripping the neodymium nitrate seed crystal layer solution on the cleaned sapphire substrate, sequentially spinning at 500rpm and 3500rpm, pyrolyzing at 200 ℃ for 30min, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, and the thickness is about 4 nm;
(5) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), pyrolyzing at 200 ℃ for 30min and annealing at 600 ℃ for 20min sequentially at 500rpm and 3000rpm, wherein the heating rate is 10 ℃/min and the cooling rate is 5 ℃/min, preparing a perovskite crystal film with the thickness of about 25nm, and preparing the target thickness by repeated spin coating for multiple times
Example 3
(1) Washing the glass substrate with deionized water, then sequentially ultrasonically cleaning the glass substrate with acetone, deionized water and isopropanol for 10 minutes, and then drying the glass substrate in a drying oven at 85 ℃ for later use;
(2) dissolving praseodymium nitrate in ethylene glycol monomethyl ether solution to prepare seed crystal layer solution with the concentration of 0.1mol/L, and sealing for later use;
(3) according to Pb1.2Zr0.52Ti0.48O3Dissolving lead acetate trihydrate into ethylene glycol monomethyl ether to prepare a lead acetate solution; then the isopropyl titanate is added according to Pb1.2Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.2Zr0.52Ti0.48O3The isopropanol zirconium solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; most preferablyThen, dripping acetylacetone with the total content of 5 percent as a chelating agent, and fully stirring to obtain a precursor solution after chelating; the concentration is 0.4mol/L, and the mixture is sealed and kept stand for later use;
(4) dropping the praseodymium nitrate crystal seed layer solution on the cleaned glass substrate, sequentially performing film spinning at 500rpm and 3500rpm, performing pyrolysis at 200 ℃ for 30min, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, repeating the steps for three times, the thickness of the crystal seed layer is about 24nm, and the XRD (X-ray diffraction) graph of the crystal seed layer is shown in figure 1, so that the crystal seed layer is in a single-phase crystal structure and is used as a nucleation site to be beneficial to crystallization of the lead zirconate titanate film;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), pyrolyzing at 200 ℃ for 30min and annealing at 600 ℃ for 20min sequentially at 500rpm and 3000rpm, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, the thickness of the perovskite type crystal film is about 50nm, repeating the steps for 4 times and the thickness is about 200nm, and the perovskite type crystal film is prepared.
Example 4
(1) Washing the magnesium oxide substrate with ionized water, then ultrasonically cleaning the magnesium oxide substrate with acetone, deionized water and isopropanol for 10 minutes in sequence, and then drying the magnesium oxide substrate in a drying oven at 85 ℃ for later use;
(2) dissolving samarium nitrate hexahydrate in ethylene glycol ethyl ether solution, and stirring until the samarium nitrate is fully dissolved to prepare samarium nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.3Zr0.35Ti0.65O3Dissolving lead acetate trihydrate into ethylene glycol ethyl ether to obtain a lead acetate solution; then adding tetraisobutyl titanate to the reaction mixture according to Pb1.3Zr0.35Ti0.65O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.3Zr0.35Ti0.65O3The isopropanol zirconium solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally dripping 3 percent of the mixture by volumeTaking acetylacetone as a chelating agent, fully stirring to obtain a chelated lead zirconate titanate precursor solution with the concentration of 1.0mol/L, and sealing and standing for later use;
(4) and dripping the lanthanum nitrate crystal seed layer solution on the cleaned magnesium oxide substrate, sequentially spinning at 500rpm and 3500rpm, pyrolyzing at 300 ℃ for 20 minutes at a heating rate of 10 ℃/min and a cooling rate of 5 ℃/min.
(5) And (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), pyrolyzing at 200 ℃ for 30min and annealing at 850 ℃ for 5min sequentially at 500rpm and 3000rpm, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, the perovskite crystal film is prepared, the thickness is about 100nm, and the target thickness can be obtained by repeating the steps.
Example 5
(1) Washing a sapphire substrate with ionized water, then sequentially ultrasonically cleaning the sapphire substrate with acetone, deionized water and isopropanol for 10 minutes, and then drying the sapphire substrate in a drying oven at 85 ℃ for later use;
(2) dissolving samarium nitrate hexahydrate in ethylene glycol ethyl ether solution, and stirring until the samarium nitrate is fully dissolved to prepare samarium nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.5Zr0.52Ti0.48O3Dissolving lead acetate trihydrate into ethylene glycol ethyl ether to obtain a lead acetate solution; then the isopropyl titanate is added according to Pb1.5Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.5Zr0.52Ti0.48O3The isopropanol zirconium solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, dropwise adding 3% of acetylacetone in volume ratio as a chelating agent, fully stirring to obtain chelated lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and sealing and standing for later use;
(4) and dripping the samarium nitrate seed crystal layer solution on the cleaned sapphire substrate, sequentially spinning at 500rpm and 3500rpm, pyrolyzing at 450 ℃ for 5 minutes at a heating rate of 10 ℃/min and a cooling rate of 5 ℃/min.
(5) And (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), pyrolyzing at 200 ℃ for 30min and annealing at 800 ℃ for 10min sequentially at 500rpm and 3000rpm, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, and the perovskite crystal film with the thickness of about 50nm is prepared, and the steps are repeated for 3 times and the thickness is about 160 nm. The XRD test curve is shown in figure 3, the lower curve is the XRD curve of a control group of blank sapphire substrate, and the upper curve is the XRD curve of the lead zirconate titanate film, which shows that the lead zirconate titanate film disclosed by the invention can prepare a perovskite crystal film with a single-phase structure under the condition and has the preferred orientation of the (100) direction.
Example 6
(1) Cleaning a silicon wafer substrate by using a standard RCA method, and then drying the silicon wafer substrate in a drying oven at 85 ℃ for later use;
(2) dissolving neodymium nitrate hexahydrate in ethylene glycol monomethyl ether solution, and stirring until the neodymium nitrate hexahydrate is fully dissolved to prepare neodymium nitrate seed crystal layer solution with the concentration of 0.1mol/L for later use;
(3) according to Pb1.1Zr0.8Ti0.2O3Dissolving lead acetate trihydrate into ethylene glycol monomethyl ether, and dissolving lead acetate in the solution; then adding isobutyl titanate to the mixture according to Pb1.1Zr0.8Ti0.2O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.1Zr0.8Ti0.2O3Dropping a zirconium isopropoxide solution according to the atomic ratio; finally, dropwise adding acetylacetone with the volume ratio of 8% as a chelating agent, fully stirring to obtain chelated lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and sealing and standing for later use;
(4) dripping the neodymium nitrate seed crystal layer solution on the cleaned silicon wafer substrate, sequentially spinning at 500rpm and 3500rpm, pyrolyzing at 350 ℃ for 20min, wherein the heating rate is 10 ℃/min, and the cooling rate is 5 ℃/min;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), pyrolyzing at 200 ℃ for 30min and annealing at 650 ℃ for 15min sequentially at 500rpm and 3000rpm, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, the perovskite type crystal film is prepared, the thickness is about 50nm, the perovskite type crystal film is prepared, and the steps are repeated to obtain the target thickness.
Example 7
(1) The silicon/silicon nitride substrate is dried in a drying box at 85 ℃ for standby application by a standard RCA method (removing DHF cleaning process);
(2) dissolving lanthanum nitrate in ethylene glycol monomethyl ether solution, stirring until the lanthanum nitrate is fully dissolved to prepare lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.15Zr0.52Ti0.48O3Dissolving lead acetate in ethylene glycol monomethyl ether to obtain a lead acetate solution; then the isopropyl titanate is added according to Pb1.15Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.15Zr0.52Ti0.48O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, acetylacetone with the volume ratio of 5 percent is dripped as a chelating agent, the mixture is fully stirred to obtain a chelated faint yellow lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and the solution is sealed and kept stand for later use;
(4) dripping the lanthanum nitrate seed crystal layer solution on the cleaned silicon/silicon nitride substrate, homogenizing at 500rpm and 3500rpm in sequence, and pyrolyzing at 400 ℃, wherein the heating rate is 10 ℃/min, and the cooling rate is 5 ℃/min;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), pyrolyzing at 200 ℃ for 30min and annealing at 600 ℃ for 15min sequentially at 500rpm and 3000rpm, wherein the heating rate is 10 ℃/min and the cooling rate is 5 ℃/min, so that a perovskite crystal film with the thickness of about 50nm is prepared, and the steps are repeated to obtain the target thickness.
Example 8
(1) The silicon/silicon dioxide substrate is dried in a drying oven at 85 ℃ for standby after being treated by a standard RCA method (removing DHF cleaning process);
(2) dissolving lanthanum nitrate in ethylene glycol monomethyl ether solution, stirring until the lanthanum nitrate is fully dissolved to prepare lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.15Zr0.52Ti0.48O3At an atomic ratio ofDissolving lead acetate trihydrate in ethylene glycol monomethyl ether to obtain a lead acetate solution; then the isopropyl titanate is added according to Pb1.15Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.15Zr0.52Ti0.48O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, acetylacetone with the volume ratio of 5 percent is dripped as a chelating agent, the mixture is fully stirred to obtain a chelated faint yellow lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and the solution is sealed and kept stand for later use;
(4) dripping the lanthanum nitrate crystal seed layer solution on the cleaned silicon/silicon dioxide substrate, firstly carrying out film spinning at 50rpm and 350rpm for 40 seconds, carrying out pyrolysis at 300 ℃, wherein the heating rate is 10 ℃/min, and the cooling rate is 5 ℃/min;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), sequentially spinning at 500rpm and 3000rpm, heating at 240 ℃ for 20min, and finally annealing at 600 ℃ for 10min by a tube furnace at the heating rate of 100 ℃/min and the cooling rate of 50 ℃/min to prepare the perovskite crystal film.
Example 9
(1) Washing the magnesium oxide substrate with deionized water, then sequentially ultrasonically cleaning the magnesium oxide substrate with acetone, deionized water and isopropanol for 10 minutes, and then drying the magnesium oxide substrate in a drying oven at 85 ℃ for later use;
(2) dissolving samarium nitrate in diethylene glycol monomethyl ether solution, stirring until the samarium nitrate is fully dissolved, and preparing lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.15Zr0.52Ti0.48O3Dissolving lead acetate trihydrate into diethylene glycol monomethyl ether to prepare a lead acetate solution; then the isopropyl titanate is added according to Pb1.15Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.15Zr0.52Ti0.48O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, dropwise adding acetylacetone with the volume ratio of 5% as a chelating agent, and fully stirring to obtain a chelated mixed solution; chelating lead zirconate titanate precursorSealing and standing the solution with the concentration of 0.4mol/L for later use;
(4) dripping the samarium nitrate crystal seed layer solution on the cleaned magnesium oxide substrate, firstly spinning at 50rpm and 350rpm for 40 seconds, pyrolyzing at 300 ℃, wherein the heating rate is 10 ℃/min, and the cooling rate is 5 ℃/min;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), sequentially spinning at 500rpm and 3000rpm, heating at 240 ℃ for 20min, and finally annealing at 600 ℃ for 10min by a tube furnace at the heating rate of 100 ℃/min and the cooling rate of 50 ℃/min to prepare the perovskite crystal film.
Example 10
(1) Respectively carrying out ultrasonic treatment on the sapphire substrate in an ultrasonic cleaning instrument using acetone, dilute hydrochloric acid, deionized water and isopropanol as cleaning liquids for 10 minutes, and then drying the sapphire substrate in a drying oven at 85 ℃ for later use;
(2) dissolving lanthanum nitrate in ethylene glycol monomethyl ether solution, stirring until the lanthanum nitrate is fully dissolved to prepare lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.15Zr0.52Ti0.48O3Dissolving lead acetate trihydrate into ethylene glycol monomethyl ether to prepare a lead acetate solution; then the isopropyl titanate is added according to Pb1.15Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.15Zr0.52Ti0.48O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, acetylacetone with the volume ratio of 5 percent is dripped as a chelating agent, the mixture is fully stirred to obtain a chelated faint yellow lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and the solution is sealed and kept stand for later use;
(4) dripping the lanthanum nitrate seed crystal layer solution on the cleaned sapphire substrate, spin-coating at 500rpm for 5 seconds, spin-coating at 3500rpm for 40 seconds, heating at 440 ℃ for 5min, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, and repeating the steps for 3 times;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), firstly carrying out film spinning at 3000rpm and 500rpm for 40 seconds, heating at 200 ℃ for 5 minutes, finally carrying out annealing at 650 ℃ for 10 minutes in a tube furnace, wherein the heating rate is 10 ℃/min, the cooling rate is 5 ℃/min, and repeating the steps for 3 times to prepare the perovskite crystal film with the thickness of about 160 nm.
(6) Spin-coating sol-gel silica on the PZT thin film, heating at 120 deg.C for 2h, heating at 150 deg.C for 2h to obtain upper cladding, and making into slab waveguide structure with cross-sectional Scanning Electron Microscope (SEM) image as shown in FIG. 4, sol-gel silica thickness of 1.7um, and PZT thin film thickness of 160 nm. FIG. 5 is a schematic view of a slab waveguide and an electrode designed according to the present invention, wherein the electrode is an aluminum electrode formed by heating and evaporating a coating film, and the thickness of the aluminum electrode is about 200 nm. The optical test is carried out on the slab waveguide by adopting 1550nm and 1310nm semiconductor lasers and an infrared camera, fig. 6 is a light receiving test graph of the infrared camera, the wavelength is 1550nm, and as shown in fig. 6, the lead zirconate titanate film prepared by the invention has high transparency and small absorption to optical signals of communication bands. The aluminum coplanar electrodes were connected by probes and the light was subjected to electro-optic modulation testing by applying an alternating voltage.
Example 11
(1) The silicon/silicon dioxide substrate is dried in a drying oven at 85 ℃ for standby after being treated by a standard RCA method (removing DHF cleaning process);
(2) dissolving lanthanum nitrate in ethylene glycol monomethyl ether solution, stirring until the lanthanum nitrate is fully dissolved to prepare lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.15Zr0.52Ti0.48O3Dissolving lead acetate trihydrate into ethylene glycol monomethyl ether to obtain a lead acetate solution; then the isopropyl titanate is added according to Pb1.15Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.15Zr0.52Ti0.48O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, dropwise adding acetylacetone with the volume ratio of 5% as a chelating agent, and fully stirring to obtain a chelated mixed solution; mixing the chelated mixed solution with a lead acetate solution, and stirring until the solution is clear and transparent to prepare a light yellow lead zirconate titanate precursor solution with the concentrationSealing and standing at 0.4mol/L for later use;
(4) dripping the lanthanum nitrate crystal seed layer solution on the cleaned silicon/silicon dioxide substrate, sequentially spinning at 500rpm and 3500rpm, heating at 400 ℃ for 10min, wherein the heating rate is 10 ℃/min, and the cooling rate is 5 ℃/min;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), spin-coating at 500rpm for 5 seconds, spin-coating at 3000rpm for 40 seconds, heating at 240 ℃ for 2min, finally annealing at 600 ℃ for 10min by a tube furnace, repeating the steps for three times, wherein the heating rate is 100 ℃/min, and the cooling rate is 50 ℃/min, so as to prepare the perovskite crystal film.
(6) Spin-coating sol-gel silica on the PZT thin film, heating at 120 ℃ for 2h, heating at 150 ℃ for 2h, and the thickness is 300 nm. Then, the SiO film is prepared by the standard photoetching process and the standard etching process in sequence, as shown in FIG. 72A strip structure is subjected to standard photoetching process again to prepare a metal electrode, and the SiO based on the lead zirconate titanate film shown in figure 7 is obtained2A ridge waveguide structure. The optical test is carried out on the slab waveguide by adopting 1550nm and 1310nm semiconductor lasers and an infrared camera, fig. 9 is a light receiving test graph of the infrared camera, the wavelength is 1550nm, and as shown in fig. 9, the lead zirconate titanate film prepared by the invention has high transparency and small absorption to optical signals of communication bands. The coplanar electrodes are connected through the probes, and the electro-optic coefficient of the test piece is measured to be larger than 240pm/V by applying alternating voltage to perform modulation test on light.
Example 12
(1) The silicon/silicon nitride substrate is dried in a drying box at 85 ℃ for standby application by a standard RCA method (removing DHF cleaning process);
(2) dissolving lanthanum nitrate in ethylene glycol monomethyl ether solution, stirring until the lanthanum nitrate is fully dissolved to prepare lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.15Zr0.3Ti0.7O3Dissolving lead acetate trihydrate into ethylene glycol monomethyl ether to obtain a lead acetate solution; then the isopropyl titanate is added according to Pb1.15Zr0.3Ti0.7O3Atomic ratio ofDripping into lead acetate solution, and adding into the solution according to Pb1.15Zr0.3Ti0.7O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, dropwise adding acetylacetone with the volume ratio of 5% as a chelating agent, and fully stirring to obtain a chelated mixed solution; mixing the chelated mixed solution with a lead acetate solution, stirring until the solution is clear and transparent to prepare a light yellow lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and sealing and standing for later use;
(4) dripping the lanthanum nitrate seed crystal layer solution on the cleaned silicon/silicon nitride substrate, spin-coating at 500rpm for 5 seconds, spin-coating at 3500rpm for 40 seconds, heating at 200 ℃ for 30 minutes at a heating rate of 10 ℃/min and a cooling rate of 5 ℃/min;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), spin-coating at 500rpm for 5 seconds, spin-coating at 3000rpm for 40 seconds, heating at 240 ℃ for 20min, finally annealing at 600 ℃ for 10min by a tube furnace, repeating the steps for three times, wherein the heating rate is 100 ℃/min, and the cooling rate is 50 ℃/min, so as to prepare the perovskite crystal film.
(6) Preparing a silicon nitride film with the thickness of 200nm on the PZT film by PECVD, and then sequentially carrying out a standard photoetching process and a standard etching process to obtain Si shown in figure 83N4A ridge waveguide structure is processed by standard photoetching process again to prepare a metal electrode, and the Si based on the lead zirconate titanate film as shown in figure 8 is obtained3N4The ridge waveguide structure is connected with the coplanar electrode through the probe, and the electro-optic coefficient of the ridge waveguide structure is measured to be larger than 68pm/V by applying alternating voltage to perform modulation test on light.
Example 13
(1) Cleaning a silicon substrate by a standard RCA method, and then drying the silicon substrate in a drying oven at 85 ℃ for later use;
(2) preparing a layer of metal electrode on the silicon wafer cleaned in the step (1) with the thickness of about 200nm, and preparing SiO with the thickness of about 2um by PECVD2As the lower cladding.
(3) Dissolving lanthanum nitrate in ethylene glycol monomethyl ether solution, stirring until the lanthanum nitrate is fully dissolved to prepare lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(4) according to Pb1.15Zr0.52Ti0.48O3Dissolving lead acetate trihydrate into ethylene glycol monomethyl ether to obtain a lead acetate solution; then the isopropyl titanate is added according to Pb1.15Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.15Zr0.52Ti0.48O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, dropwise adding acetylacetone with the volume ratio of 5% as a chelating agent, fully stirring to obtain chelated lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and sealing and standing for later use;
(5) dripping the lanthanum nitrate seed crystal layer solution on the cleaned silicon/silicon dioxide substrate, spin-coating for 5 seconds at 500 revolutions per minute, spin-coating for 40 seconds at 3500 revolutions per minute, volatilizing an organic solvent at 200 ℃, annealing for 10 minutes at 430 ℃ in a tubular furnace, wherein the heating rate is 10 ℃/min, and the cooling rate is 5 ℃/min;
(6) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), spin-coating at 500rpm for 5 seconds, spin-coating at 3000rpm for 40 seconds, heating at 240 ℃ for 20min, finally annealing at 600 ℃ for 10min by a tube furnace, repeating the steps for three times, wherein the heating rate is 100 ℃/min, and the cooling rate is 50 ℃/min, so as to prepare the perovskite crystal film.
(6) Spin-coating sol-gel silica on the PZT film, heating at 120 deg.C for 2h, heating at 150 deg.C for 2h, and the thickness is 2 um. Then, metal electrodes were prepared, and a slab waveguide based on the lead zirconate titanate thin film upper and lower electrode structure as shown in fig. 10 was obtained.
Example 14
(1) Cleaning a silicon substrate by a standard RCA method, and then drying the silicon substrate in a drying oven at 85 ℃ for later use;
(2) preparing a layer of metal electrode on the silicon wafer cleaned in the step (1) with the thickness of about 200nm, and then preparing Si with the thickness of about 2um by PECVD3N4As the lower cladding.
(3) Dissolving lanthanum nitrate in ethylene glycol monomethyl ether solution, stirring until the lanthanum nitrate is fully dissolved to prepare lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(4) according to Pb1.3Zr0.52Ti0.48O3Dissolving lead acetate trihydrate into ethylene glycol monomethyl ether, and stirring until the solution is clear and transparent to obtain a lead acetate solution; then the isopropyl titanate is added according to Pb1.3Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.3Zr0.52Ti0.48O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, dropwise adding acetylacetone with the volume ratio of 5% as a chelating agent, fully stirring to obtain chelated lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and sealing and standing for later use;
(5) dripping the lanthanum nitrate seed crystal layer solution on the cleaned silicon/silicon dioxide substrate, spin-coating for 5 seconds at 500 revolutions per minute, spin-coating for 40 seconds at 3500 revolutions per minute, volatilizing an organic solvent at 200 ℃, annealing for 10 minutes at 430 ℃ in a tubular furnace, wherein the heating rate is 10 ℃/min, and the cooling rate is 5 ℃/min;
(6) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), spin-coating at 500rpm for 5 seconds, spin-coating at 3000rpm for 40 seconds, heating at 240 ℃ for 20min, finally annealing at 600 ℃ for 10min by a tube furnace, repeating the steps for three times, wherein the heating rate is 100 ℃/min, and the cooling rate is 50 ℃/min, so as to prepare the perovskite crystal film.
(6) Preparation of a layer of Si on a PZT thin film by PECVD3N4As an upper cladding. Then, metal electrodes were prepared, and a slab waveguide based on the lead zirconate titanate thin film upper and lower electrode structure as shown in fig. 11 was obtained.
Example 15
(1) The silicon/silicon oxide substrate is dried in a drying box at 85 ℃ for standby application by a standard RCA method (removing DHF cleaning process);
(2) dissolving lanthanum nitrate in ethylene glycol monomethyl ether solution to prepare lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.15Zr0.52Ti0.48O3By dissolving lead acetate trihydrate in ethylene glycolStirring the solution in methyl ether until the solution is clear and transparent to obtain a lead acetate solution; then the isopropyl titanate is added according to Pb1.15Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.15Zr0.52Ti0.48O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, dropwise adding acetylacetone with the volume ratio of 5% as a chelating agent, fully stirring to obtain chelated lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and sealing and standing for later use;
(4) dripping the lanthanum nitrate seed crystal layer solution on the cleaned silicon/silicon dioxide substrate, spin-coating for 5 seconds at 500 revolutions per minute, spin-coating for 40 seconds at 3500 revolutions per minute, volatilizing an organic solvent at 200 ℃, annealing for 10 minutes at 430 ℃ in a tubular furnace, wherein the heating rate is 10 ℃/min, and the cooling rate is 5 ℃/min;
(6) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), spin-coating at 500rpm for 5 seconds, spin-coating at 3000rpm for 40 seconds, heating at 240 ℃ for 20min, finally annealing at 600 ℃ for 10min by a tube furnace, repeating the steps for three times, wherein the heating rate is 100 ℃/min, and the cooling rate is 50 ℃/min, so as to prepare the perovskite crystal film.
(6) The PZT ridge waveguide structure shown in fig. 11 is prepared by a standard photolithography process and an etching process, and the metal electrode shown in the figure is prepared by a standard photolithography process, so that the lead zirconate titanate-based thin film ridge waveguide structure shown in fig. 12 is obtained.
Example 16
1) The silicon/silicon nitride substrate is dried in a drying box at 85 ℃ for standby application by a standard RCA method (removing DHF cleaning process);
(2) dissolving lanthanum nitrate in ethylene glycol monomethyl ether solution to prepare lanthanum nitrate seed crystal layer solution with the concentration of 0.036mol/L for later use;
(3) according to Pb1.15Zr0.52Ti0.48O3Dissolving lead acetate trihydrate into ethylene glycol monomethyl ether, and stirring until the solution is clear and transparent to obtain a lead acetate solution; then the isopropyl titanate is added according to Pb1.15Zr0.52Ti0.48O3Is dripped into a lead acetate solution according to the atomic ratio of the lead and then is added according to the Pb1.15Zr0.52Ti0.48O3The zirconium n-propoxide solution is dripped into the solution according to the atomic ratio, and the mixture is uniformly stirred; finally, dropwise adding acetylacetone with the volume ratio of 5% as a chelating agent, fully stirring to obtain chelated lead zirconate titanate precursor solution with the concentration of 0.4mol/L, and sealing and standing for later use;
(4) dripping the lanthanum nitrate seed crystal layer solution on the cleaned silicon/silicon dioxide substrate, spin-coating for 5 seconds at 500 revolutions per minute, spin-coating for 40 seconds at 3500 revolutions per minute, volatilizing an organic solvent at 200 ℃, annealing for 10 minutes at 430 ℃ in a tubular furnace, wherein the heating rate is 10 ℃/min, and the cooling rate is 5 ℃/min;
(5) and (3) dropwise adding the PZT precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), spin-coating at 500rpm for 5 seconds, spin-coating at 3000rpm for 40 seconds, heating at 240 ℃ for 20min, finally annealing at 600 ℃ for 10min by a tube furnace, repeating the steps for three times, wherein the heating rate is 100 ℃/min, and the cooling rate is 50 ℃/min, so as to prepare the perovskite crystal film.
(6) A Mach-Zehnder (Mach-Zehnder) structure shown in fig. 13 is prepared through a standard photoetching process and an etching process, and a metal electrode shown in the figure is prepared through the standard photoetching process to obtain the lead zirconate titanate film-based Mach-Zehnder (Mach-Zehnder) electro-optic modulator shown in fig. 13.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and although the invention has been described in detail with reference to the foregoing examples, it will be apparent to those skilled in the art that various changes in the form and details of the embodiments may be made and equivalents may be substituted for elements thereof. All modifications, equivalents and the like which come within the spirit and principle of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A method for preparing a lead zirconate titanate film facing next-generation high-speed communication is characterized by comprising the following steps:
(1) substrate cleaning
Cleaning the substrate, removing organic and inorganic impurities on the substrate, and drying; the substrate is an inorganic substrate or a composite substrate formed by growing an inorganic film on the inorganic substrate;
(2) disposing a seed layer solution
Dissolving lanthanide nitrate in n-propanol or ether alcohol solvent to obtain lanthanide nitrate solution as seed crystal layer solution;
(3) preparation of lead zirconate titanate PbxZryTi1-yO3Precursor solution
Firstly, preparing a lead acetate solution, wherein the solute is lead acetate, and the solvent is an ether alcohol solvent; then dissolving any one of tetraethyl titanate, isopropyl titanate or tetraisobutyl titanate in a lead acetate solution according to the atomic ratio in the chemical formula, dripping a zirconium n-propoxide or zirconium isopropoxide solution according to the atomic ratio in the chemical formula, and uniformly stirring; finally, acetylacetone is dripped as a chelating agent, the mixture is fully stirred to obtain a chelated lead zirconate titanate precursor solution, and the solution is sealed and kept stand.
(4) Preparing a seed layer
Dripping the seed crystal layer solution prepared in the step (2) on the substrate cleaned in the step (1), and then sequentially carrying out spin coating and pyrolysis treatment to prepare a seed crystal layer; the thickness of the film is adjusted by adjusting the spin-coating speed and the spin-coating times in the preparation process;
(5) preparation of lead zirconate titanate film
Dripping the lead zirconate titanate precursor solution prepared in the step (3) on the seed crystal layer prepared in the step (4), and sequentially performing spin coating and annealing treatment to prepare a lead zirconate titanate crystal film; the thickness of the film is adjusted by adjusting the spin-coating speed and the spin-coating times in the preparation process.
2. The method for preparing a lead zirconate titanate film facing next generation high speed communication according to claim 1, wherein in the step (2), the concentration of the prepared lanthanide nitrate solution is 0.01-0.4 mol/L;
in the step (3), the concentration of the prepared PZT precursor solution is 0.02-1.0 mol/L.
3. The method for preparing a lead zirconate titanate thin film facing next generation high-speed communication according to claim 1, wherein in the step (4), the pyrolysis temperature is 200 to 450 ℃;
in the step (5), the annealing temperature is 500-850 ℃.
4. The method for producing a lead zirconate titanate thin film for next-generation high-speed communications according to claim 1, wherein in the step (3), lead zirconate titanate (Pb) is usedxZryTi1-yO3In the precursor solution, x is 1.0-1.5, and y is 0.2-0.8.
5. The method for preparing a lead zirconate titanate thin film facing next generation high speed communication according to claim 1, wherein in the step (3), acetylacetone is added in an amount of 0.5 to 8% by volume.
6. The method of producing a lead zirconate titanate thin film facing next-generation high-speed communications according to claim 1, wherein in the step (1), the substrate is selected from the group consisting of silicon, aluminum oxide, magnesium oxide, glass, and a composite substrate formed by growing any one of silicon nitride, silicon dioxide, titanium dioxide, and aluminum nitride on an inorganic substrate.
7. The method for producing a lead zirconate titanate thin film facing next-generation high-speed communications according to claim 1, wherein the ether alcohol solvent in each of the steps (2) and (3) is selected from one or more of ethylene glycol methyl ether, diethylene glycol methyl ether, and ethylene glycol ethyl ether.
8. A lead zirconate titanate thin film produced by the process of any one of the preceding claims.
9. An electro-optic modulator made of the lead zirconate titanate thin film of claim 8, characterized in that a cladding thin film or a strip waveguide or a Mach-Zehnder structure is prepared on the lead zirconate titanate thin film by a micro-nano processing technique, and a corresponding electrode structure is prepared, to obtain a corresponding electro-optic modulator.
10. The electro-optic modulator of claim 9, wherein the cladding film is made of SiO2、TiO2Or Si3N4The strip waveguide and Mach-Zehnder structure are made of lead zirconate titanate (PZT) and SiO2、TiO2、Si3N4The electrode material adopts gold, silver, copper, titanium, aluminum and nickel.
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