CN117497477A - Composite film and preparation method thereof - Google Patents
Composite film and preparation method thereof Download PDFInfo
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- CN117497477A CN117497477A CN202311251407.7A CN202311251407A CN117497477A CN 117497477 A CN117497477 A CN 117497477A CN 202311251407 A CN202311251407 A CN 202311251407A CN 117497477 A CN117497477 A CN 117497477A
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- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 95
- 239000000758 substrate Substances 0.000 claims abstract description 73
- 238000002347 injection Methods 0.000 claims abstract description 56
- 239000007924 injection Substances 0.000 claims abstract description 56
- 239000010408 film Substances 0.000 claims description 72
- 238000000034 method Methods 0.000 claims description 70
- 239000010409 thin film Substances 0.000 claims description 65
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 37
- 238000002513 implantation Methods 0.000 claims description 32
- 238000005468 ion implantation Methods 0.000 claims description 30
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 26
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 claims description 17
- 239000013078 crystal Substances 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- 239000000919 ceramic Substances 0.000 claims description 9
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- WYOHGPUPVHHUGO-UHFFFAOYSA-K potassium;oxygen(2-);titanium(4+);phosphate Chemical compound [O-2].[K+].[Ti+4].[O-]P([O-])([O-])=O WYOHGPUPVHHUGO-UHFFFAOYSA-K 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 229910052701 rubidium Inorganic materials 0.000 claims description 3
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 13
- 235000012431 wafers Nutrition 0.000 description 32
- 150000002500 ions Chemical class 0.000 description 26
- 238000002955 isolation Methods 0.000 description 22
- 230000008569 process Effects 0.000 description 19
- 239000000377 silicon dioxide Substances 0.000 description 18
- -1 hydrogen ions Chemical class 0.000 description 17
- 239000007943 implant Substances 0.000 description 17
- 235000012239 silicon dioxide Nutrition 0.000 description 16
- 238000005498 polishing Methods 0.000 description 15
- 230000007547 defect Effects 0.000 description 14
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 14
- 238000001994 activation Methods 0.000 description 13
- 230000004913 activation Effects 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 238000000151 deposition Methods 0.000 description 11
- 229920005591 polysilicon Polymers 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 10
- 239000001307 helium Substances 0.000 description 8
- 229910052734 helium Inorganic materials 0.000 description 8
- 238000010884 ion-beam technique Methods 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000000678 plasma activation Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000009713 electroplating Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 241001391944 Commicarpus scandens Species 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001423 beryllium ion Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
- H01L21/6835—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using temporarily an auxiliary support
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/34—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
- H01L21/46—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/428
- H01L21/477—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2221/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof covered by H01L21/00
- H01L2221/67—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere
- H01L2221/683—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere for supporting or gripping
- H01L2221/68304—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere for supporting or gripping using temporarily an auxiliary support
- H01L2221/6835—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere for supporting or gripping using temporarily an auxiliary support used as a support during build up manufacturing of active devices
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2221/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof covered by H01L21/00
- H01L2221/67—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere
- H01L2221/683—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere for supporting or gripping
- H01L2221/68304—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere for supporting or gripping using temporarily an auxiliary support
- H01L2221/68381—Details of chemical or physical process used for separating the auxiliary support from a device or wafer
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Element Separation (AREA)
Abstract
The embodiment of the application provides a composite film and a preparation method thereof, wherein the functional injection sheet is subjected to first annealing treatment, and after the functional injection sheet is bonded with a substrate, the functional injection sheet is subjected to second annealing treatment to fracture an injection layer, and a film layer is transferred onto the substrate to form the composite film. The ion in the injection layer of the functional injection sheet can generate bubbles during the first annealing treatment, so that the injection layer can be broken at relatively low temperature during the second annealing treatment, the separation work of the bonding body is completed, and the problem of bonding body breakage caused by high temperature and long annealing treatment time in the prior art is avoided.
Description
Technical Field
The application relates to the technical field of semiconductors, in particular to a composite film and a preparation method thereof.
Background
Thin film materials are becoming more and more important materials in the semiconductor industry today, and meet the requirements of electronic components for miniaturization, low power consumption and high performance. In recent years, a composite film called an insulator has been attracting more and more attention in industry, and it includes an uppermost active layer, an intermediate insulating dielectric layer and a semiconductor substrate. The active layer may be a semiconductor film (e.g., si, ge, gaAs, siC), a piezoelectric film (lithium niobate and lithium tantalate), or a ferroelectric film, among others.
In the process of producing a composite film, annealing treatment is required for a bonded body after bonding a substrate and a film base body so as to prepare an active layer on the surface of the substrate.
However, the bonded body is liable to be broken during the annealing treatment.
Disclosure of Invention
The embodiment of the application provides a composite film and a preparation method thereof, which are used for solving the problem that a bonding body is easy to break during annealing in the prior art.
In a first aspect, an embodiment of the present application provides a method for preparing a composite film, including:
performing ion implantation on the film substrate to obtain a functional implantation sheet, wherein the functional implantation sheet comprises a film layer, an implantation layer and a residual material layer which are sequentially laminated;
performing first annealing treatment on the functional injection sheet, and cooling the functional injection sheet to room temperature;
bonding one side of the film layer with the substrate to prepare a bonding body;
carrying out secondary annealing treatment on the bonding body so as to fracture the injection layer, and transferring the film layer to the substrate to form a composite film;
wherein the temperature of the second annealing treatment is lower than that of the first annealing treatment.
In one possible implementation, the temperature of the first annealing treatment is in the range of 200-300 ℃.
In one possible implementation, the time for the first annealing treatment is in the range of 1h to 10h.
In one possible implementation, the temperature of the second annealing treatment is in the range of 150 ℃ to 200 ℃.
In one possible implementation, the second annealing treatment is performed for a time period ranging from 1h to 5h.
In one possible implementation, the method for preparing a composite film further includes: and after the second annealing treatment is finished, carrying out third annealing treatment on the composite film.
In one possible implementation, the temperature of the third annealing treatment is in the range of 300-600 ℃.
In one possible implementation, the time for the third annealing treatment is in the range of 1h to 24h.
In one possible implementation manner, the material of the thin film substrate is at least one of lithium niobate crystal, lithium tantalate crystal, gallium arsenide, ceramic, lithium tetraborate, gallium arsenide, potassium titanyl phosphate or rubidium titanyl phosphate crystal;
and/or the substrate is made of at least one of silicon, sapphire, quartz, silicon carbide, silicon nitride or quartz glass.
In a second aspect, an embodiment of the present application further provides a composite film, which is prepared according to any one of the above-mentioned preparation methods of the composite film.
The embodiment of the application provides a preparation method of a composite film, which comprises the steps of carrying out first annealing treatment on a functional injection sheet, and carrying out second annealing treatment after the functional injection sheet is bonded with a substrate to fracture an injection layer, and transferring a film layer onto the substrate to form the composite film. The ion in the injection layer of the functional injection sheet can generate bubbles during the first annealing treatment, so that the injection layer can be broken at relatively low temperature during the second annealing treatment, the separation work of the bonding body is completed, and the problem of bonding body breakage caused by high temperature and long annealing treatment time in the prior art is avoided.
The embodiment of the application also provides a composite film, which is prepared by the composite film preparation method in any one of the above schemes, so that the composite film preparation method in any one of the above schemes has all the beneficial effects and is not repeated here.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the present application and do not constitute a limitation on the invention.
In the drawings:
FIG. 1 is a flow chart of a method for preparing a composite film according to an embodiment of the present application;
FIG. 2 is a schematic illustration of a composite film preparation process according to an embodiment of the present application;
FIG. 3 is a schematic illustration of a composite film preparation process according to another embodiment of the present application.
Reference numerals illustrate:
100-a substrate; 200-isolating layer; 300-film substrate; 400-ion; 500-defect layer;
310-a remainder layer; 320-an injection layer; 330-thin film layer.
Detailed Description
In order to better understand the technical solutions in the present application, the following description will clearly and completely describe the technical solutions in the embodiments of the present application with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, shall fall within the scope of the present application.
In the description of the embodiments of the present application, the terms "first," "second," are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present application, the meaning of "plurality" is at least two, such as two, three, etc., unless explicitly defined otherwise.
Thin film materials are becoming more and more important materials in the semiconductor industry today, and meet the requirements of electronic components for miniaturization, low power consumption and high performance. In recent years, a composite film called an insulator has been attracting more and more attention in industry, and it includes an uppermost active layer, an intermediate insulating dielectric layer and a semiconductor substrate. The active layer may be a semiconductor film (e.g., si, ge, gaAs, siC), a piezoelectric film (lithium niobate and lithium tantalate), or a ferroelectric film, among others. The material has good application performance in CPU chips, memories, amplifiers, filters and modulators.
In the process of producing a composite film, annealing treatment is required for a bonded body after bonding a substrate and a film base body so as to prepare an active layer on the surface of the substrate.
However, the bonded body is liable to be broken during the annealing treatment. The temperature for annealing the bonding body in the prior art is 220-320 ℃, and the bonding body can be separated only when the annealing temperature meets the range, but the bonding body formed by the substrate and the functional injection sheet is easy to break due to the difference of the thermal expansion coefficients between the substrate and the functional injection sheet; in addition, separation of the bonded body at this temperature also results in a decrease in yield of the composite film produced, which decreases the yield.
In order to solve the above problems, the embodiments of the present application provide a composite film and a preparation method thereof, and the following will describe the schemes of the embodiments of the present application in detail with reference to the drawings of the specification.
FIG. 1 is a flow chart of a method for preparing a composite film according to an embodiment of the present application; FIG. 2 is a schematic illustration of a composite film preparation process according to an embodiment of the present application; FIG. 3 is a schematic illustration of a composite film preparation process according to another embodiment of the present application.
In a first aspect, referring to fig. 1 to 3, an embodiment of the present application provides a method for preparing a composite film, including:
s100: the thin film substrate 300 is ion-implanted to obtain a functional implant.
Before preparing the composite film, the film base 300 and the substrate 100 are first prepared. Wherein the substrate 100 and the thin film base 300 are heterogeneous substrates.
Further, by way of example, the thin film substrate 300 may be at least one of lithium niobate crystal, lithium tantalate crystal, gallium arsenide, ceramic, lithium tetraborate, gallium arsenide, potassium titanyl phosphate, rubidium titanyl phosphate crystal. The thin film substrate 300 according to the present invention includes, but is not limited to, the single crystal material described above, and is not particularly limited.
The substrate 100 may be at least one of silicon, sapphire, quartz, silicon carbide, silicon nitride, or quartz glass. Likewise, the substrate 100 of the present invention may optionally include, but is not limited to, the substrate materials described above, and is not particularly limited.
In this step, the selected ions 400 are implanted into the thin film substrate 300 by an ion implantation method to obtain a functional implant sheet including the thin film layer 330, the implant layer 320, and the residual material layer 310, which are stacked. Wherein the thin film layer 330 is located at the uppermost layer, the residual material layer 310 is located at the bottommost layer, the implantation layer 320 is located between the thin film layer 330 and the residual material layer 310, and the ions 400 implanted by the ion implantation method are distributed in the implantation layer 320.
In some possible embodiments, the ion beam of the ion implantation method may be selected from at least one of a helium ion beam, a hydrogen ion beam, a nitrogen ion beam, an oxygen ion beam, and an argon ion beam plasma beam. The ion beam selected by the present invention includes, but is not limited to, the implanted ions described above; exemplary, the implant dose range of the ion beam may be 1×10 16 ions/cm 2 -1×10 16 ions/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The implantation energy ranges from 40keV to 600keV, and selected ions have been implanted to the specified location, forming an implanted layer 320.
The method of ion implantation is not particularly limited in the present application, and any method of ion implantation in the prior art may be used, and the implanted ions 400 may be ions 400 that can generate a gas by heat treatment, for example: the implanted ions 400 may be at least one of hydrogen ions, helium ions, nitrogen ions, oxygen ions, or argon ions plasma 400.
For example, when hydrogen ions are implanted, the implantation dose may be 3×10 16 ions/cm 2 ～8×10 16 ions/cm 2 The implantation energy may be 100KeV to 400KeV; when helium ions are injected, the injection dosage can be 1×10 16 ions/cm 2 ～1×10 17 ions/cm 2 The implantation energy may be 50KeV to 1000KeV. For example, in the case of hydrogen ion injection, the injection dose may be 4×10 16 ions/cm 2 The implant energy may be 180KeV; when helium ions are injected, the injection dosage is 4×10 16 ions/cm 2 The implantation energy was 200KeV.
In ion implantation of the thin film substrate 300, the thickness of the thin film layer 330 may be adjusted by adjusting the ion implantation depth, specifically, the greater the ion implantation depth, the greater the thickness of the prepared thin film layer 330; conversely, the smaller the depth of ion implantation, the smaller the thickness of the prepared thin film layer 330. In addition, the depth of the implant layer 320 may be adjusted by adjusting the ion implantation energy, specifically, the greater the ion implantation energy, the deeper the depth of the implant layer 320; conversely, the smaller the energy of the ion implantation, the shallower the depth of the implanted layer 320.
It will be appreciated that, in ion implantation of the thin film substrate 300, the diffusion width of the implantation layer 320 may be adjusted by adjusting the ion implantation dose, specifically, the larger the ion implantation dose, the wider the diffusion width of the implantation layer 320; conversely, the smaller the dose of ion implantation, the narrower the diffusion width of the implanted layer 320.
S200: and carrying out first annealing treatment on the functional injection sheet, and cooling the functional injection sheet to room temperature.
Illustratively, the first annealing treatment of the functional implant may be performed at a temperature ranging from 200 ℃ to 300 ℃ for a time ranging from 1h to 10h, and the functional implant is cooled to room temperature. After the first annealing process, the implanted layer 320 of the functional implant may generate small bubbles that are separated, for example, hydrogen ions form hydrogen gas, helium ions form helium gas, etc., so as to facilitate the breakage of the implanted layer 320 during the subsequent second annealing process. That is, the implanted layer 320 may fracture at a relatively low temperature in favor of a subsequent second anneal process.
S300: one side of the thin film layer 330 of the function injection sheet is bonded to the substrate 100 to produce a bonded body.
In this step, the thin film layer 330 of the function injection sheet is contact-bonded with the process surface of the substrate 100, so that the thin film layer 330, the injection layer 320, the residual material layer 310, and the substrate 100 are combined to form a bonded body.
Specifically, the bonding surface of the substrate 100 and the bonding surface of the thin film layer 330 of the thin film substrate 300 are cleaned, and the bonding surface of the thin film layer 330 of the cleaned thin film substrate 300 and the bonding surface of the substrate 100 are bonded by a plasma bonding method to form a bonded body.
The bonding method of the bonding surface of the thin film substrate 300 and the substrate 100 is not particularly limited, and any bonding method of bonding the bonding surface of the thin film substrate 300 and the substrate 100 in the prior art may be used, for example, surface activation is performed on the bonding surface of the thin film substrate 300, surface activation is also performed on the bonding surface of the processed substrate 100, and bonding is performed on both activated surfaces to obtain a bonded body.
In addition, the method of surface activation of the process surface of the film substrate 300 is not particularly limited, and any method of surface activation of the film bonding surface in the prior art may be used, for example, plasma activation, chemical solution activation, and the like; similarly, the surface activation method of the bonding surface of the substrate 100 is not particularly limited, and any method of the prior art that can be used for surface activation of the silicon dioxide bonding surface, such as plasma activation, may be used.
Referring to fig. 2, in some examples, an isolation layer 200 may be prepared on a bonding surface of a substrate 100 before bonding a functional implant prepared based on an ion implantation method to the bonding surface of the substrate 100; illustratively, the isolation layer 200 is fabricated by deposition or oxidation, and the isolation layer 200 may be made of at least one of silicon dioxide, silicon nitride, aluminum oxide or aluminum nitride. The deposition method is not limited, and may be Chemical Vapor Deposition (CVD), physical Vapor Deposition (PVD), magnetron sputtering, etc., and the thickness of the isolation layer 200 may be 200nm to 3000nm.
If the isolation layer 200 is prepared by oxidation: the polysilicon layer may be subjected to an oxidation process, wherein one side of the polysilicon layer away from the substrate 100 is oxidized to form a silicon dioxide layer, and one side of the polysilicon layer near the substrate 100 is not oxidized; the oxidation temperature may be 900-1000 ℃.
In the above embodiment, the steps are adopted in which the substrate 100 on which the isolation layer 200 has been prepared on the surface is prepared first. The thin film layer 330 is contact-bonded with the isolation layer 200 on the substrate 100 such that the thin film layer 330, the injection layer 320, the residual material layer 310, the isolation layer 200, and the substrate 100 are combined to form a bonded body.
Referring to fig. 3, a defect layer 500 may be first prepared on a substrate 100, and then an isolation layer 200 may be prepared on the defect layer 500. Illustratively, the material of the defect layer 500 may be at least one of polysilicon, amorphous silicon, or poly-germanium. For example, the defect layer 500 may be formed by depositing polysilicon using a deposition method, amorphous silicon using a deposition method, polycrystalline germanium using a deposition method, etching the substrate 100 using an etching method, or implanting the substrate 100 using an implantation method to generate implantation damage. Then, a deposition method or an oxidation method is used to manufacture the isolation layer 200 on the defect layer 500, and the isolation layer 200 is made of at least one of silicon dioxide, silicon oxynitride or silicon nitride. The thickness of the defect layer 500 may be 300nm to 5000nm.
The defect layer 500 has lattice defects with a certain density, and can capture carriers existing between the isolation layer 200 and the substrate 100, so that the carriers at the interface between the isolation layer 200 and the substrate 100 are prevented from being aggregated, and the loss of the composite film is reduced.
In some possible embodiments, when the defect layer 500 is a polysilicon layer, the polysilicon layer is oxidized, and the isolation layer 200 is made of silicon dioxide. The method of preparing the isolation layer 200 by deposition is not limited, and may be a Chemical Vapor Deposition (CVD), a Physical Vapor Deposition (PVD), a magnetron sputtering, or the like.
In the above embodiment, the steps adopted are that the substrate 100 is prepared first, then the defect layer 500 is prepared on the substrate 100, then the isolation layer 200 is prepared on the defect layer 500 to form the composite substrate 100, and the prepared isolation layer 200 of the composite substrate 100 is contacted and bonded with the thin film layer 330 of the function injection sheet, so that the thin film layer 330, the injection layer 320, the residual material layer 310, the isolation layer 200, the defect layer 500 and the substrate 100 are combined to form a bonded body.
S400: the bond is subjected to a second annealing process to fracture the implanted layer 320 and the thin film layer 330 is transferred to the substrate 100 to form a composite thin film.
And (3) carrying out a second annealing treatment on the bonding body, so that the residual material layer 310 is peeled off from the bonding body along the injection layer 320, and the film layer 330 is transferred onto the substrate 100, wherein the temperature of the second annealing treatment is lower than that of the first annealing treatment. In this step, the bond formed in the previous step is heat annealed, illustratively by placing the bond in an annealing furnace, heating to 150-200 ℃ for 1-5 hours, to strip the remainder layer 310 from the bond along the implant layer 320, and transferring the thin film layer 330 to the substrate 100. Since the first annealing treatment is performed on the functional implant, and the small bubbles are formed in the implant layer 320, after the functional implant is bonded to the substrate 100, the temperature of the second annealing treatment is lower than the separation temperature in the annealing treatment in the prior art by about 50-100 ℃, and the separation time is shortened by 5-10 hours than the normal separation time.
In the prior art, since the functional implant sheet is not subjected to the first annealing treatment, it is necessary to anneal the bond at a temperature of 200-300 c, and during the treatment, the thin film layer 330 is easily broken in the bond due to the high temperature and the difference in thermal expansion coefficient between the substrate 100 and the thin film layer 330. If the annealing temperature is lowered, it is necessary to lengthen the annealing time, but too long annealing time may also cause cracking of the thin film layer 330 in the bond. Because the solution of the embodiment of the present application can make the ions 400 in the injection layer 320 of the functional injection sheet generate bubbles during the first annealing treatment, so that the injection layer 320 can be broken at a relatively low temperature during the second annealing treatment, and the separation of the bonding body is completed, thereby avoiding the occurrence of the problem of breakage of the bonding body caused by high temperature and long annealing treatment time in the prior art.
S500: and carrying out third annealing on the composite film.
With continued reference to fig. 1-3, in some examples, the composite film preparation method further includes: and after the second annealing treatment is finished, carrying out third annealing treatment on the composite film, wherein the temperature range of the third annealing treatment is 300-600 ℃, and the time range of the third annealing treatment is 1-24 h. Thereby eliminating damage to the thin film layer 330 during ion implantation. Finally, the thin film layer 330 can be polished and thinned to 50nm-3000nm, and the composite thin film is obtained.
In a second aspect, an embodiment of the present application further provides a composite film, which is prepared according to any one of the above-mentioned preparation methods of the composite film.
For a better detailed description of the embodiments of the present application, three specific embodiments will be given below.
Example 1
Step 1, preparing a silicon wafer and a lithium tantalate wafer with 6 inches, respectively fixing the silicon wafer or the lithium tantalate wafer on a porous ceramic sucker of polishing equipment, performing chemical mechanical polishing treatment to obtain a smooth surface, and then performing semiconductor RCA cleaning on the two wafers to obtain a clean surface.
And 2, depositing polycrystalline silicon (PolySI) on the cleaned silicon wafer by adopting an LPCVD process to form a defect layer 500, wherein the deposition temperature can be controlled at 580-650 ℃, and the deposition thickness is 300nm.
And 3, manufacturing a silicon dioxide layer on the polycrystalline silicon (PolySI) by adopting an LPCVD method (including but not limited to sputtering, evaporation, electroplating and the like) to form an isolation layer 200, then performing chemical mechanical polishing to a thickness of 100-700nm to obtain a smooth surface, and cleaning with RCA to obtain a clean surface.
Step 4, nitrogen ions are injected into the processed lithium tantalate wafer by adopting an ion injection method, so that a residual material layer 310, an injection layer 320 and a lithium tantalate film layer 330 are sequentially formed on the lithium tantalate wafer from the injection surface, and the injected nitrogen ions are distributed on the injection layer 320, so that a functional injection sheet made of lithium tantalate material is obtained; by ion implantationWhen nitrogen ions are injected by the method, the injection dosage parameters are as follows: the implantation dose is 2×10 16 ions/cm 2 The implantation energy was 200keV.
Step 5, performing primary annealing treatment on the functional injection sheet obtained in the step 4, wherein the annealing temperature is 200 ℃, the annealing time is 10 hours, and cooling the functional injection sheet to room temperature after annealing; in this process, ions 400 in the implanted layer 320 chemically react to become gas molecules or atoms and generate minute bubbles.
Step 6, cleaning the thin film layer 330 and the silicon dioxide layer of the functional injection sheet made of lithium tantalate respectively, and bonding the process surface of the cleaned thin film layer 330 with the silicon dioxide layer isolation layer 200 by adopting a plasma bonding method to form a bonded body;
step 7, carrying out secondary annealing treatment on the bonding body, wherein the annealing temperature is 150 ℃, and the heat preservation is carried out for 5 hours; until the residual material layer 310 is separated from the bonded body to form a lithium tantalate composite film. The heat preservation process is carried out in a vacuum environment or in a protective atmosphere formed by at least one gas of nitrogen and inert gas; the bubbles in the implanted layer 320 become more and the volume becomes gradually larger during the secondary annealing. When these bubbles are connected together, separation of the residual material layer 310 from the injection layer 320 is achieved, thereby transferring the thin film layer 330 onto the separation layer 200 and forming a composite thin film.
Step 8, carrying out third annealing treatment on the composite film in heating equipment, wherein the annealing temperature is 300 ℃ and the annealing time is 24 hours; the purpose is to eliminate ion implantation damage. This step can promote bonding forces greater than 10MPa and can restore damage to the thin film layer 330 from ion implantation, such that the resulting lithium tantalate thin film layer 330 approximates the properties of a lithium tantalate wafer.
And 9, fixing the composite film on a porous ceramic sucker of polishing equipment, performing chemical mechanical polishing to remove 80nm, and finally performing RCA cleaning to obtain the composite film.
Example 2
Step 1, preparing a silicon wafer and a lithium niobate wafer with 6 inches, respectively fixing the silicon wafer and the lithium niobate wafer on a porous ceramic sucker of polishing equipment, performing chemical mechanical polishing treatment to obtain a smooth surface, and then performing semiconductor RCA cleaning on the two wafers to obtain a clean surface.
Step 2, a silicon dioxide layer is manufactured on a silicon wafer by LPCVD (including but not limited to sputtering, evaporation, electroplating, etc.) as an isolation layer 200, and then chemical mechanical polishing is performed to a thickness of 100nm to obtain a smooth surface, and RCA cleaning is performed to obtain a clean surface.
And 3, implanting oxygen ions into the lithium niobate wafer processed in the step 1 by adopting a stripping ion implantation method, so that a residual material layer 310, an implantation layer 320 and a thin film layer 330 are sequentially formed on the lithium niobate wafer from the implantation surface, and the implanted oxygen ions are distributed on the implantation layer 320, thereby obtaining the single crystal lithium niobate wafer implantation sheet.
When oxygen ions are injected by adopting a stripping ion implantation method, the implantation dosage parameters are as follows: the ion implantation method is to implant oxygen ion with a depth of 440nm, an implantation energy of 300kev, and an implantation dose of 1×10 16 ions/cm 2 。
Step 4, carrying out primary annealing treatment on the single crystal lithium niobate wafer injection sheet obtained in the step 3, wherein the annealing temperature is 300 ℃, the annealing time is 1h, and cooling the injection sheet to room temperature after annealing; in this process, ions 400 in the implanted layer 320 chemically react to become gas molecules or atoms and generate minute bubbles.
And 5, cleaning the thin film layer 330 of the single crystal lithium niobate wafer injection sheet and the silicon dioxide layer, and bonding the process surface of the cleaned lithium niobate thin film layer 330 with the silicon dioxide layer by adopting a plasma bonding method to form a bonded body.
The method for surface-activating the technical surface of the lithium niobate thin film is not particularly limited, and any method in the prior art for surface-activating the technical surface of the thin film can be adopted, for example, plasma activation, chemical solution activation and the like; similarly, the surface activation method of the silica bonding surface is not particularly limited, and any method that can be used for surface activation of the silica bonding surface in the prior art, for example, plasma activation, can be used.
Step 6, then placing the bonded body into heating equipment for secondary annealing treatment, wherein the temperature of the secondary annealing is 200 ℃, and preserving heat for 1h; until the residual material layer 310 is separated from the bonded body to form a lithium niobate composite thin film.
The thermal insulation process is performed under a vacuum environment or under a protective atmosphere formed by at least one of nitrogen and inert gas, and during the secondary annealing, more and more bubbles are injected into the layer 320, and the volume is gradually increased. When these bubbles are connected together, separation of the residual layer 310 from the injection layer 320 is achieved, thereby transferring the thin film layer 330 onto the separation layer 200 and forming a composite structure.
Step 7, carrying out third annealing treatment on the composite film in heating equipment, wherein the temperature of the third annealing is 600 ℃, and the annealing time is 1h; the aim is to eliminate implantation damage. The link can promote bonding force to be more than 10MPa, and can recover damage of ion implantation to the thin film layer 330, so that the obtained lithium tantalate thin film layer 330 approximates to the property of a lithium tantalate wafer.
And 8, fixing the composite film on a porous ceramic sucker of polishing equipment, then performing chemical mechanical polishing to remove 20nm, and finally performing RCA cleaning to obtain the clean composite film.
Example 3
Step 1, preparing a 3-inch silicon wafer and a lithium niobate wafer, respectively fixing the silicon wafer or the lithium niobate wafer on a porous ceramic sucker of polishing equipment, performing chemical mechanical polishing treatment to obtain a smooth surface, and then performing semiconductor RCA cleaning on the two wafers to obtain a clean surface.
Step 2, a polysilicon layer is formed on the cleaned silicon wafer by PECVD (including but not limited to sputtering, evaporation, electroplating, etc.), and the thickness of the polysilicon layer is 1 μm as the defect layer 500.
Step 3, a silicon dioxide layer is formed on the polysilicon layer by LPCVD (including but not limited to sputtering, evaporation, electroplating, etc.) as an isolation layer 200, and then chemical mechanical polishing is performed to obtain a smooth surface with a thickness of 1 μm, and RCA cleaning is performed to obtain a clean surface.
And 4, implanting helium ions (He+) into the lithium niobate wafer processed in the step 1 by adopting a stripping ion implantation method, so that a residual layer 310, an implanted layer 320 and a thin film layer 330 are sequentially formed on the lithium niobate wafer from the implantation surface, and the implanted helium ions (He+) are distributed on the implanted layer 320, thereby obtaining the single crystal lithium niobate wafer implanted sheet.
When he+ is injected by adopting the stripping ion implantation method, the implantation dosage parameters are as follows: the depth of ion implantation was 840nm, the implantation energy was 250kev, and the implantation dose was 2×10 16 ions/cm 2 。
Step 5, carrying out primary annealing treatment on the injection sheet obtained in the step 4, wherein the annealing temperature is 250 ℃, the annealing time is 5 hours, and cooling the injection sheet to room temperature after annealing; in this process, ions 400 in the implanted layer 320 chemically react to become gas molecules or atoms and generate minute bubbles.
And 6, cleaning the thin film layer 330 of the single crystal lithium niobate wafer injection sheet and the silicon dioxide layer, and bonding the process surface of the cleaned lithium niobate thin film layer 330 with the silicon dioxide layer by adopting a plasma bonding method to form a bonded body.
The method for surface-activating the technical surface of the lithium niobate thin film is not particularly limited, and any method in the prior art for surface-activating the technical surface of the thin film can be adopted, for example, plasma activation, chemical solution activation and the like; similarly, the surface activation method of the silica bonding surface is not particularly limited, and any method that can be used for surface activation of the silica bonding surface in the prior art, for example, plasma activation, can be used.
Step 7, then placing the bonding body into heating equipment for secondary annealing treatment, wherein the temperature of the secondary annealing is 180 ℃, and preserving heat for 2 hours; until the residual material layer 310 is separated from the bonded body to form a lithium niobate composite thin film. The thermal insulation process is performed under a vacuum environment or under a protective atmosphere formed by at least one of nitrogen and inert gas, and during the secondary annealing, more and more bubbles are injected into the layer 320, and the volume is gradually increased. When these bubbles are connected together, separation of the residual layer 310 from the injection layer 320 is achieved, thereby transferring the thin film layer 330 onto the separation layer 200 and forming a composite structure.
Step 8, carrying out third annealing treatment in the composite film heating equipment, wherein the temperature of the third annealing treatment is 400 ℃, and the annealing time is 10 hours; the aim is to eliminate implantation damage. The link can promote bonding force to be more than 10MPa, and can recover damage of ion implantation to the thin film layer 330, so that the obtained lithium niobate thin film layer 330 approximates to the property of a lithium niobate wafer.
And 9, fixing the composite film on a porous ceramic sucker of polishing equipment, performing chemical mechanical polishing to remove 20nm, and finally performing RCA cleaning to obtain the clean composite film.
It is to be understood that, based on the several embodiments provided in the present application, those skilled in the art may combine, split, reorganize, etc. the embodiments of the present application to obtain other embodiments, where none of the embodiments exceed the protection scope of the present application.
The foregoing detailed description of the embodiments of the present application has further described the objects, technical solutions and advantageous effects thereof, and it should be understood that the foregoing is merely a specific implementation of the embodiments of the present application, and is not intended to limit the scope of the embodiments of the present application, and any modifications, equivalent substitutions, improvements, etc. made on the basis of the technical solutions of the embodiments of the present application should be included in the scope of the embodiments of the present application.
Claims (10)
1. A method for preparing a composite film, comprising:
performing ion implantation on the film substrate to obtain a functional implantation sheet, wherein the functional implantation sheet comprises a film layer, an implantation layer and a residual material layer which are sequentially laminated;
performing primary annealing treatment on the function injection sheet, and cooling the function injection sheet to room temperature;
bonding one side of the film layer with a substrate to prepare a bonding body;
carrying out a second annealing treatment on the bonding body so as to fracture the injection layer, and transferring the film layer onto the substrate to form a composite film;
wherein the temperature of the second annealing treatment is lower than the temperature of the first annealing treatment.
2. The method of claim 1, wherein the first annealing is performed at a temperature ranging from 200 ℃ to 300 ℃.
3. The method of claim 1, wherein the first annealing is performed for a time period ranging from 1h to 10h.
4. The method of claim 1, wherein the second annealing is performed at a temperature in the range of 150 ℃ to 200 ℃.
5. The method of claim 1, wherein the second annealing treatment is performed for a period of time ranging from 1h to 5h.
6. The method for producing a composite film according to any one of claims 1 to 5, further comprising: and after the second annealing treatment is finished, carrying out third annealing treatment on the composite film.
7. The method of claim 6, wherein the third annealing is performed at a temperature ranging from 300 ℃ to 600 ℃.
8. The method of claim 6, wherein the third annealing is performed for a period of time ranging from 1h to 24h.
9. The method according to any one of claims 1 to 5, wherein the material of the thin film substrate is at least one of lithium niobate crystal, lithium tantalate crystal, gallium arsenide, ceramic, lithium tetraborate, gallium arsenide, potassium titanyl phosphate or rubidium titanyl phosphate crystal;
and/or the substrate is made of at least one of silicon, sapphire, quartz, silicon carbide, silicon nitride or quartz glass.
10. A composite film prepared by the method of any one of claims 1 to 9.
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