CN102443851B - Stripping method of thin-film material - Google Patents
Stripping method of thin-film material Download PDFInfo
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- CN102443851B CN102443851B CN201010504760.8A CN201010504760A CN102443851B CN 102443851 B CN102443851 B CN 102443851B CN 201010504760 A CN201010504760 A CN 201010504760A CN 102443851 B CN102443851 B CN 102443851B
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- film
- lithium
- ion implantation
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- lithium tantalate
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Abstract
A technical process for manufacturing a monocrystal lithium niobate thin film or a monocrystal lithium tantalate thin-film material. After bonding of wafers, reduction of crystal lattice intensity of a damage layer caused by ion implantation and differences of thermal expansion coefficients between a silicon dioxide layer and a lithium niobate (lithium tantalate) crystal are utilized to select an appropriate heat treatment process and form stress in wafer set, so as to strip the film. The process can substantially reduce ion implantation dosage, thereby reducing production cost and increasing film quality.
Description
Technical field
The present invention relates to a kind of technological process of making monocrystalline Lithium niobium trioxide film or monocrystalline lithium tantalate thin film material.
Background technology
Have the monocrystalline Lithium niobium trioxide film of high index-contrast or monocrystalline lithium tantalate thin film material in integrated optics, photoelectron element, has application prospect very widely in nonlinear optics.Document 1 and 2 has been reported respectively the method for making lithium niobate monocrystal film and monocrystalline lithium tantalate film, and its basic step comprises ion implantation, the deposition of silicon-dioxide and polishing, and sample cleans, Direct Bonding, thermal treatment is separated, the techniques such as film polishing.The process that its basic producing principle can be introduced with document 3 is explained: to lithium niobate crystal chip or lithium tantalate wafer carry out (hydrogen or helium) ion implantation, ion enters after wafer, energy loses gradually, speed reduces, final ion rests in the aspect of a certain degree of depth (this one deck is called as affected layer), then this wafer bonding is coated with on the wafer of silicon-dioxide to other a slice, then this wafer set being put into annealing furnace heats, in the process of heating, the ion injecting becomes hydrogen molecule or helium atom, gather together gradually, form bubble, with the rising of annealing temperature or the prolongation of annealing time, bubble density increases gradually, volume strengthens gradually, final all bubbles join together, bubble layer finally breaks, film is just stripped from.As can be seen here, forming bubble is one of key condition of making Lithium niobium trioxide (lithium tantalate) film.The increase of the formation of bubble, expansion, density is the mechanism that film is peeled off.So, in document 1 and 2, ion implantation dosage all larger (4 * 10
16ions/cm
2above), to ensure enough ions, produce highdensity bubble, but heavy dose of ion implantation two shortcomings of having brought, the one, the time of injecting is long, corresponding cost of manufacture is just high, and the secondth, heavy dose of implantation membership damages the crystalline structure of film, makes the physical properties variation of film.In document 4, the ion implantation nonlinear optical coefficients of Lithium niobium trioxide film that cause of heavy dose of helium are reduced to about half of body material.The technical problem to be solved in the present invention: propose a kind of novel stripping means, can reduce ion implantation dosage, and then reduce production costs, improve film quality.
Summary of the invention
Through research, we find the mechanism that exists a kind of diverse Lithium niobium trioxide (lithium tantalate) film to peel off, and have produced thus a kind of new stripping means, and we are referred to as stress stripping method.In this method, wafer is first carried out to the ion implantation (such as 3 * 10 of low dose
16ions/cm
2), ion can be hydrogen ion or helium ion, in the affected layer forming, crystalline network is destroyed, corresponding chemical bond is weakened, lattice strength decreased, then this wafer bonding is coated with on the wafer of silicon-dioxide to other a slice, this wafer set is heated up or lowers the temperature processing, wafer set is in the process of temperature change, because the thermal expansivity of silicon-dioxide and Lithium niobium trioxide (lithium tantalate) wafer is different, produced internal stress, this internal stress is applied in the middle of the wafer of ion implantation mistake, because other parts of the relative crystal of lattice intensity of affected layer are low, so first the lattice of affected layer can rupture, film will be stripped from.As can be seen here, the core of stress stripping method is to utilize the ion implantation lattice strength decreased that causes affected layer, and the difference of silicon dioxide layer and Lithium niobium trioxide (lithium tantalate) Thermal Expansion in Crystals coefficient, utilizes temperature variation to produce internal stress, thereby film is peeled off.In this process, we find, smaller dose ion implantation (such as 3 * 10
16ions/cm
2) just can enough reduce the intensity of lattice, cause film successfully to be peeled off.Stress stripping method can reduce ion implantation dosage greatly, thereby reduces production costs, and improves film quality.
The present invention and the difference of the manufacturing technology of disclosed Lithium niobium trioxide (lithium tantalate) film can clearly be found out by following experimental result: in Figure of description, Fig. 1 left side is the manufacturing technology of utilizing document 3 reports, a part for ion implantation wafer is bonded on substrate, rest part unsettled (not carrying out bonding), after thermal treatment separation, inject the optical microscope photograph of ion wafer.The right half part of picture is bonding region, the Lithium niobium trioxide surface of this part come off (disbonded ragion), rest on another piece substrate, form Lithium niobium trioxide film (film photo is not included in this picture), the left-half of picture is the region that there is no bonding, because helium atom has formed bubble in heat-processed, the shape of bubble shows clearly (residual district) on picture.Fig. 2 is the stress stripping method of utilizing the present invention to introduce, and a part for ion implantation wafer is bonded on substrate, and rest part unsettled (not carrying out bonding), after stress stripping method is processed, injects the optical microscope photograph of ion wafer.The right half part of picture is bonding region, the surface of this part come off (disbonded ragion), rest on substrate, form Lithium niobium trioxide film (film photo is not included in this picture), the left-half of picture is the region that there is no bonding, in this region, vestige (residual district) without any bubble, Fig. 2 clearly shows, stress stripping method does not rely on the formation of bubble, just film can be stripped down from body material.
Technical characterictic of the present invention is, after carrying out wafer bonding, selects suitable heat treatment process, at the inner formation of wafer set stress, thereby film is peeled off.Suitable heat treatment process mainly comprises two steps, the first step is to be warmed up between 100 ℃ to 200 ℃, keep for some time, make bond strength reach maximum, second step is within the shorter time, by wafer set temperature change, the speed changing is in 10 ℃/min left and right, thereby cause larger internal stress, cause the fracture of affected layer, film is peeled off.
The invention has the beneficial effects as follows, can make ion implantation dosage reduce (lower than 4 * 10
16ions/cm
2), and then reduce production costs, improve film quality.
Accompanying drawing explanation
In Figure of description, Fig. 1 to Fig. 2 is the present invention and the difference test result schematic diagram of the manufacturing technology of disclosed Lithium niobium trioxide (lithium tantalate) film.
Fig. 1 adopts the method for document 3, peels off after Lithium niobium trioxide film the optical microscope photograph of ion implantation wafer.In photo, left side is the region (residual district) that film does not strip down, and right side is the region staying (disbonded ragion) after film is stripped from.
Fig. 2 adopts after stress stripping method, the optical microscope photograph of ion implantation wafer.In photo, left side is the region (residual district) that film does not strip down, and right side is the region (disbonded ragion) staying after film is stripped from.
Embodiment
Mode 1
Lithium niobium trioxide (or lithium tantalate) wafer A is carried out to helium ion implantation, implantation dosage can be 1 * 10
16ions/cm
2to 4 * 10
16ions/cm
2between, by polishing after another sheet lithium niobate crystal (or lithium tantalate) sheet B surface deposition layer of silicon dioxide.By after A and B bonding, be warming up to 170 ℃ of left and right, stop 10 hours, make wafer reach best bond strength, then, in 10 minutes, temperature is elevated to 230 ℃, the internal stress that this temperature change causes departs from film, just obtains Lithium niobium trioxide (or lithium tantalate) film after polishing.
Mode 2
Lithium niobium trioxide (or lithium tantalate) wafer A is carried out to helium ion implantation, implantation dosage can be 1 * 10
16ions/cm
2to 4 * 10
16ions/cm
2between, by polishing after another sheet Lithium niobium trioxide (lithium tantalate) wafer B surface deposition layer of silicon dioxide.By after A and B bonding, be warming up to 170 ℃ of left and right, stop 10 hours, make wafer reach best bond strength, then, in 20 minutes, temperature is reduced to subzero 60 ℃, the internal stress that this temperature change causes is peeled off film, just obtains Lithium niobium trioxide (or lithium tantalate) film after polishing.
Reference
1.P.Rabiei，and?W.H.Steier，Lithium?niobate?ridge?waveguides?and?modulators?fabricated?using?smart?guide，Appl.Phys.Lett.86，161115(2005)
2.A.Tauzin，J.Dechamp，F.Madeira，F.Mazen，M.Zussy，C.Deguet，L.Clavelier，J.-S.Moulet，C.Richtarch，T.Akatsu，M.Yoshimi?and?A.Rigny，3-inch?single-crystal?LiTaO
3?films?onto?metallic?electrode?using?Smart?Cuttechnology，Electronics?Letters，Vol.44，No.13，doi：10.1049/el：20081057(2008)
3.A.Guarino，G.Poberaj，D.Rezzonico，R.Degl’innocenti，and?P.Günter，Electro-optically?tunable?microringresonators?in?lithium?niobate，Nature?Photonics，1，407-410(2007)
4.Michel?Bruel，Separation?of?silicon?wafers?by?the?smart-cut?method，Mat?Res?Innovat?3：9-13(1999)
Claims (2)
1. a technological process, be used for making monocrystalline Lithium niobium trioxide film or monocrystalline lithium tantalate thin film material, it is characterized in that, after bonding Lithium niobium trioxide and silica sphere or bonding lithium tantalate and silica sphere, be warming up to 170 degrees Celsius of left and right, stop 10 hours, then in 10 minutes, temperature is elevated to 230 degrees Celsius, at the inner formation of wafer set stress, thereby film is peeled off.
2. a technological process, be used for making monocrystalline Lithium niobium trioxide film or monocrystalline lithium tantalate thin film material, it is characterized in that, after bonding Lithium niobium trioxide and silica sphere or bonding lithium tantalate and silica sphere, be warming up to 170 degrees Celsius of left and right, stop 10 hours, then in 20 minutes, temperature is reduced to subzero 60 degrees Celsius, at the inner formation of wafer set stress, thereby film is peeled off.
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|---|---|---|---|
| CN201010504760.8A CN102443851B (en) | 2010-10-13 | 2010-10-13 | Stripping method of thin-film material |
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| CN201010504760.8A CN102443851B (en) | 2010-10-13 | 2010-10-13 | Stripping method of thin-film material |
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| CN102443851A CN102443851A (en) | 2012-05-09 |
| CN102443851B true CN102443851B (en) | 2014-08-20 |
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|---|---|---|---|---|
| CN104078407B (en) * | 2013-03-29 | 2018-12-04 | 济南晶正电子科技有限公司 | The method of film and manufacture film |
| CN104868050B (en) * | 2014-06-09 | 2017-11-17 | 济南晶正电子科技有限公司 | The method that film is manufactured in the substrate different from the thermal coefficient of expansion of original substrate |
| CN104862784B (en) * | 2014-06-09 | 2018-01-09 | 济南晶正电子科技有限公司 | A kind of method for the monocrystal thin films for manufacturing near stoichiometric proportion |
| CN104779143B (en) * | 2015-02-13 | 2017-07-04 | 济南晶正电子科技有限公司 | A kind of film being arranged in substrate and preparation method thereof |
| JP6396852B2 (en) * | 2015-06-02 | 2018-09-26 | 信越化学工業株式会社 | Method for manufacturing composite wafer having oxide single crystal thin film |
| CN105321806A (en) * | 2015-08-21 | 2016-02-10 | 济南晶正电子科技有限公司 | Composite single crystal thin film and method for manufacturing composite single crystal thin film |
| CN107059128B (en) * | 2016-12-21 | 2019-04-16 | 济南晶正电子科技有限公司 | Lithium tantalate or lithium niobate monocrystal film in a kind of micron silicon substrate and preparation method thereof |
| CN108493334B (en) * | 2018-03-15 | 2020-06-30 | 中国科学院上海微系统与信息技术研究所 | Preparation method of thin film heterostructure |
| CN109554668A (en) * | 2018-12-17 | 2019-04-02 | 合肥鑫晟光电科技有限公司 | The method of crucible nozzle arrangements, crucible and nozzle clearing |
| WO2021035486A1 (en) * | 2019-08-26 | 2021-03-04 | 福建晶安光电有限公司 | Lithium tantalate wafer and blackening method therefor |
| CN110867381B (en) * | 2019-11-07 | 2022-10-14 | 上海新硅聚合半导体有限公司 | Silicon-based lithium tantalate single crystal thin film substrate with bottom electrode and preparation method and application thereof |
| CN112382563A (en) * | 2020-11-13 | 2021-02-19 | 济南晶正电子科技有限公司 | Ion implantation thin film wafer separation method, single crystal thin film, and electronic component |
| CN113714649B (en) * | 2021-08-25 | 2023-07-14 | 深圳市大族半导体装备科技有限公司 | Method for manufacturing wafer |
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|---|---|---|---|---|
| CN1291349A (en) * | 1998-02-17 | 2001-04-11 | 纽约市哥伦比亚大学托管会 | Crystal ion-slicing of single crystal films |
| CN1385906A (en) * | 2002-05-24 | 2002-12-18 | 中国科学院上海微系统与信息技术研究所 | Generalized semiconductor film material on isolator and preparation method thereof |
| CN1897258A (en) * | 2002-03-26 | 2007-01-17 | 夏普公司 | Semiconductor device and its fabricating method, soi substrate and its production method and display device |
-
2010
- 2010-10-13 CN CN201010504760.8A patent/CN102443851B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1291349A (en) * | 1998-02-17 | 2001-04-11 | 纽约市哥伦比亚大学托管会 | Crystal ion-slicing of single crystal films |
| CN1897258A (en) * | 2002-03-26 | 2007-01-17 | 夏普公司 | Semiconductor device and its fabricating method, soi substrate and its production method and display device |
| CN1385906A (en) * | 2002-05-24 | 2002-12-18 | 中国科学院上海微系统与信息技术研究所 | Generalized semiconductor film material on isolator and preparation method thereof |
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| CN102443851A (en) | 2012-05-09 |
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