CN111218665A - Method for low-temperature deposition of silicon nitride with adjustable optical performance on flexible substrate - Google Patents
Method for low-temperature deposition of silicon nitride with adjustable optical performance on flexible substrate Download PDFInfo
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- CN111218665A CN111218665A CN202010051521.5A CN202010051521A CN111218665A CN 111218665 A CN111218665 A CN 111218665A CN 202010051521 A CN202010051521 A CN 202010051521A CN 111218665 A CN111218665 A CN 111218665A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/345—Silicon nitride
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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Abstract
The invention provides a method for depositing silicon nitride with adjustable optical performance on a flexible substrate at low temperature, which comprises the steps of providing a substrate and forming the flexible substrate on the substrate; depositing an optically adjustable silicon nitride film on the flexible substrate by an inductively coupled plasma chemical vapor deposition method, wherein the deposition temperature is 25-150 ℃, and introducing a reaction carrier gas, wherein the reaction carrier gas comprises a silicon gas source and a nitrogen gas source, the flow ratio of the nitrogen gas source to the silicon gas source is 0.5-16, and the thickness of the silicon nitride film is 30nm-1000 nm; peeling the flexible substrate from the substrate by a physical mechanical or chemical method; has the advantages that: the silicon nitride film with adjustable optical performance is deposited on the flexible substrate at low temperature, the flexible substrate cannot be softened or fused, the silicon nitride films with different refractive indexes are obtained by adjusting the flow ratio of the nitrogen source and the silicon gas source, and the silicon nitride film can be applied to visible light wave band low-loss waveguide and expand the application range and form of taking silicon nitride as optical device materials.
Description
Technical Field
The invention relates to a method for depositing silicon nitride with adjustable optical performance on a flexible substrate at low temperature.
Background
Silicon nitride is widely used in various fields as an amorphous material. The silicon nitride film has the technical properties of good wear resistance, high mechanical strength, good insulation and resistance to corrosion of alkali metal ions and water vapor, and is widely used for passivation layers and dielectric layers of semiconductor devices and structural support layers of microstructure devices. Secondly, the optical characteristics of the silicon nitride film can be changed by adjusting the flow ratio of reaction gases such as ammonia and silane in the process of depositing the silicon nitride film, and the application of the silicon nitride as an optical waveguide in the field of silicon photons and the application of the silicon nitride as a luminescent material is realized. Therefore, a set of silicon nitride film deposition processes is developed for different application directions of silicon nitride, and the deposition processes are becoming mature.
Currently, the deposition methods of silicon nitride films mainly include Low Pressure Chemical Vapor Deposition (LPCVD) and Plasma Enhanced Chemical Vapor Deposition (PECVD). For the LPCVD deposition method, the deposition temperature is higher than 700 ℃, which limits the application range of LPCVD deposited silicon nitride to a certain extent, for example, low pressure chemical vapor deposition cannot be used in the aspects of IC post-process, silicon photon and IC integration based on silicon nitride optical waveguide, and the like. The temperature range of the PECVD deposited silicon nitride film is 200-400 ℃, which is lower than the LPCVD deposition temperature, which provides a solution for the subsequent silicon nitride deposition of part of ICs and the integration of silicon photons and ICs, but is not suitable for a plurality of devices sensitive to temperature.
High molecular polymer also exhibits various material characteristics as a special material, such as good fracture strength, low young's modulus, high ductility, biocompatibility, chemical inertness, etc., and thus should be used in a large number of fields, such as MEMS, biomedical, radio frequency, and IC. The high molecular polymer also embodies some specific application values, for example, the high molecular polymer can be used as a flexible film, can realize the separation from substrate silicon or glass, and greatly improves the application range of the high molecular polymer.
The SiN film and other materials are deposited on the high polymer film, so that the integrated optical device taking SiN as the waveguide can be separated from the silicon or glass substrate, and the polymer has certain ductility, thereby greatly increasing the application range of the integrated optical device taking SiN and other materials as the waveguide. The film is deposited on a high molecular polymer substrate, the lower the deposition temperature is needed to be, the better the deposition temperature is controlled so as not to damage the molecular structure of the polymer, and the growth temperature of the SiN film which is the mainstream at present is about 400 ℃, and is still too high.
Disclosure of Invention
In order to solve the problem of high temperature required for depositing silicon nitride, the invention provides a method for depositing silicon nitride with adjustable optical performance on a flexible substrate at low temperature.
The invention provides a method for depositing silicon nitride with adjustable optical performance on a flexible substrate at low temperature, which comprises the following steps: ,
step 100: providing a substrate, and forming a flexible substrate on the substrate;
step 200: depositing an optically adjustable silicon nitride film on the flexible substrate by an inductively coupled plasma chemical vapor deposition method;
step 300: peeling the flexible substrate from the substrate by a physical mechanical or chemical method;
it is characterized in that;
in the step 200, the deposition temperature is 25-150 ℃, and reaction carrier gas is introduced, wherein the reaction carrier gas comprises a silicon gas source and a nitrogen gas source, the flow ratio of the nitrogen gas source to the silicon gas source is 0.5-16, and the thickness of the silicon nitride film is 30nm-1000 nm.
Preferably, the refractive index of the silicon nitride film is 1.75-2.2.
Preferably, the flexible substrate is a polymeric material.
Preferably, in step 100, the polymer material is SU-8 resin, polyimide, polydimethylsilane, polyethylene or benzocyclobutene;
preferably, in step 100, the polymer material is spin-coated on the substrate, and the flexible substrate is formed at a pre-baking temperature of 50-120 ℃ for 1-30 minutes.
Preferably, the flexible substrate has a thickness of 1-1000 μm.
Preferably, the substrate is a silicon substrate or glass.
Preferably, the silicon gas source is silane and the nitrogen gas source is ammonia or nitrogen.
Preferably, in step 200, the flow ratio is varied uniformly.
Preferably, in step 200, the flow ratio is varied in steps.
The invention provides a method for depositing silicon nitride with adjustable optical property on a flexible substrate at low temperature, which is characterized in that a silicon nitride film with adjustable optical property is deposited on the flexible substrate made of high polymer materials at low temperature, the flexible substrate is not softened, solidified or melted, the silicon nitride films with different refractive indexes are obtained by adjusting the flow ratio of a nitrogen source and a silicon gas source, and the application range and the application form of taking SiN as optical device materials are greatly expanded.
Drawings
FIG. 1 is a flow chart of a method for low temperature deposition of optical property-tunable silicon nitride on a flexible substrate according to the present invention;
FIGS. 2 a-c are schematic diagrams showing the flow changes of the nitrogen gas source and the silicon gas source in the inductively coupled plasma CVD method according to the present invention.
Detailed Description
The following describes in detail a specific embodiment of the method for low temperature deposition of optical property-tunable silicon nitride on a flexible substrate according to the present invention with reference to the accompanying drawings.
In the drawings, the dimensional ratios of layers and regions are not actual ratios for the convenience of description. When a layer (or film) is referred to as being "on" another layer or substrate, it can be directly on the other layer or substrate, or intervening layers may also be present. In addition, when a layer is referred to as being "under" another layer, it can be directly under, and one or more intervening layers may also be present. In addition, when a layer is referred to as being between two layers, it can be the only layer between the two layers, or one or more intervening layers may also be present. Like reference numerals refer to like elements throughout. In addition, when two components are referred to as being "connected," they include physical connections, including, but not limited to, electrical connections, contact connections, and wireless signal connections, unless the specification expressly dictates otherwise.
The invention provides a method for depositing silicon nitride with adjustable optical performance on a flexible substrate at low temperature, which comprises the following steps of:
step 100: providing a substrate, and forming a flexible substrate on the substrate;
step 200: depositing an optically adjustable silicon nitride film on the flexible substrate by an inductively coupled plasma chemical vapor deposition method, wherein the deposition temperature is 25-150 ℃, the flexible substrate is not softened or melted, and reaction carrier gas is introduced, the reaction carrier gas comprises a silicon gas source and a nitrogen gas source, the flow ratio of the nitrogen gas source to the silicon gas source is 0.5-16, and the thickness of the silicon nitride film is 30nm-1000 nm; different from the traditional generation mechanism of capacitive coupling radio frequency and other low-pressure high-density plasmas, the Inductive Coupling Plasma Chemical Vapor Deposition (ICPCVD) method applies high-frequency current on an inductive coil, and the coil excites a changing magnetic field under the drive of the radio-frequency current, and the changing magnetic field induces a cyclotron electric field. The electrons do cyclotron motion under the acceleration of a cyclotron electric field, the reaction carrier gas molecules are collided and dissociated, a large number of active plasma groups are generated, the active plasma groups are transported to the surface of the substrate by airflow and are adsorbed, and the silicon nitride film is formed by surface reaction; the cyclotron of electrons in the inductive coupling chemical vapor deposition increases the collision probability with gas molecules, and can generate higher plasma density than the traditional capacitance discharge, so that the low-temperature rapid deposition of high-quality films becomes possible; the silicon nitride film formed in the step has good compactness, small damage to the flexible substrate, good refractive index, adhesiveness, step coverage and stability, low impurity and hole content and high breakdown voltage. The temperature range of the silicon nitride film deposited in the step is 25-150 ℃, which is far lower than the PECVD deposition temperature, the silicon nitride film is deposited on the flexible substrate under the low-temperature process, and the refractive index of the silicon nitride film is adjusted by adjusting the reaction carrier gas, so that the optical performance of the silicon nitride film is adjustable, and the application range can be expanded in different directions such as waveguide tubes or luminescent materials.
Step 300: peeling the flexible substrate from the substrate by a physical mechanical or chemical method; the flexible substrate is separated from the substrate, the substrate can be repeatedly used, the cost is obviously reduced, and meanwhile, the flexible substrate can be attached to other materials, so that the application range of the optical silicon nitride film is greatly expanded.
In this embodiment, the refractive index of the silicon nitride film is 1.75-2.2. The silicon nitride film may be a film having a uniform refractive index or a film having a non-uniform refractive index.
In this embodiment, the flexible substrate is a polymeric material.
In this embodiment, in step 100, the polymer material is SU-8 resin, polyimide, Polydimethylsilane (PDMS), Polyethylene (PEG), benzocyclobutene (BCB), or the like;
correspondingly, in step 100, the polymer material is spin-coated on the substrate, and the flexible substrate is formed at a pre-baking temperature of 50-120 ℃ for 1-30 minutes.
Preferably, the flexible substrate has a thickness of 1-1000 μm.
In this embodiment, the substrate is a silicon substrate or glass. In other embodiments, the substrate may be gallium nitride, polysilicon, single crystal silicon, or other substrates.
In this example, the silicon gas source is silane and the nitrogen gas source is ammonia or nitrogen.
The adjustable silicon nitride with optical performance is realized by adjusting the flow ratio of the nitrogen source and the silicon gas source in the reaction carrier gas, and in practical application, because different use scenes and purposes require silicon nitride films with different optical performance and even more complex optical performance, the control of the flow ratio of the nitrogen source and the silicon gas source is the key for expanding the optical application scene.
As shown in fig. 2a, in order to obtain a silicon nitride film with a uniform refractive index, in step 200, a fixed flow ratio of the silicon gas source to the nitrogen gas source may be adopted, where the ratio of the nitrogen gas source to the silicon gas source is: 0.5, 1, 2 and 4.
As shown in fig. 2b, in order to obtain a silicon nitride film with a varying refractive index, in step 200, the flow ratio of the silicon gas source to the nitrogen gas source is uniformly or non-uniformly varied, wherein the flow ratio of the nitrogen gas source to the silicon gas source is uniformly varied to satisfy the following conditions: x is ny2+ my + k where x is the nitrogen source flow, y is the silicon source flow, 7 ≧ n ≧ 0.3, k ≧ 0, where k is 0 as shown in FIG. 2 b.
In step 200, the nitrogen gas source and the silicon gas source have a stepwise flow ratio, as shown in fig. 2c, in order to obtain a silicon nitride film with a complex refractive index change, such as a silicon nitride film with a layered refractive index structure.
The invention provides a method for depositing silicon nitride with adjustable optical property at low temperature on a flexible substrate, which is characterized in that a silicon nitride film with adjustable optical property is deposited at low temperature on the flexible substrate without softening, solidifying or melting the flexible substrate, and the silicon nitride films with different refractive indexes are obtained by adjusting the flow ratio of a nitrogen source and a silicon gas source, so that the application range and the form of taking SiN as an optical device material are greatly expanded.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The method for depositing the silicon nitride with adjustable optical performance on the flexible substrate at low temperature comprises the following steps: ,
step 100: providing a substrate, and forming a flexible substrate on the substrate;
step 200: depositing an optically adjustable silicon nitride film on the flexible substrate by an inductively coupled plasma chemical vapor deposition method;
step 300: peeling the flexible substrate from the substrate by a physical mechanical or chemical method;
it is characterized in that;
in the step 200, the deposition temperature is 25-150 ℃, and reaction carrier gas is introduced, wherein the reaction carrier gas comprises a silicon gas source and a nitrogen gas source, the flow ratio of the nitrogen gas source to the silicon gas source is 0.5-16, and the thickness of the silicon nitride film is 30nm-1000 nm.
2. The method of claim 1, wherein the silicon nitride film has a refractive index of 1.75-2.2.
3. The method of claim 1, wherein the flexible substrate is a polymeric material.
4. The method according to claim 3, wherein the polymer material is SU-8 resin, polyimide, polydimethylsilane, polyethylene or benzocyclobutene, etc. in step 100.
5. The method of claim 4, wherein in step 100, the polymeric material is spin coated on the substrate, and the flexible substrate is formed at a pre-bake temperature of 50-120 ℃ for 1-30 minutes.
6. The method as claimed in claim 1, wherein the flexible substrate has a thickness of 1-
1000μm。
7. The method of claim 1, wherein the substrate is a silicon substrate or glass.
8. The method of claim 1, wherein the silicon gas source is silane and the nitrogen gas source is ammonia or nitrogen.
9. The method of claim 1, wherein the flow ratio is varied uniformly in step 200.
10. The method of claim 1, wherein in step 200, the flow ratio is varied in steps.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113818010A (en) * | 2021-10-26 | 2021-12-21 | 华中科技大学 | Method for modifying organic polymer material and modified organic polymer material |
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| US20070184181A1 (en) * | 2003-03-25 | 2007-08-09 | Kazuo Wada | Device and method for forming film for organic electro-luminescence element using inductive coupling CVD |
| CN101510575A (en) * | 2009-03-27 | 2009-08-19 | 南开大学 | Method for producing medlin plastic substrate flexible silicon-based film solar battery integrated component |
| CN107993918A (en) * | 2017-11-09 | 2018-05-04 | 信利半导体有限公司 | A kind of preparation method of flexible display |
| CN108172543A (en) * | 2018-01-12 | 2018-06-15 | 武汉华星光电半导体显示技术有限公司 | The stripping means and underlay substrate of a kind of flexible substrates |
| CN109449076A (en) * | 2018-08-02 | 2019-03-08 | 中山大学 | A kind of silicon-rich silicon nitride thin films low temperature preparation method |
| CN110408909A (en) * | 2018-04-26 | 2019-11-05 | Spts科技有限公司 | The method for depositing SiN film |
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2020
- 2020-01-17 CN CN202010051521.5A patent/CN111218665A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070184181A1 (en) * | 2003-03-25 | 2007-08-09 | Kazuo Wada | Device and method for forming film for organic electro-luminescence element using inductive coupling CVD |
| CN101510575A (en) * | 2009-03-27 | 2009-08-19 | 南开大学 | Method for producing medlin plastic substrate flexible silicon-based film solar battery integrated component |
| CN107993918A (en) * | 2017-11-09 | 2018-05-04 | 信利半导体有限公司 | A kind of preparation method of flexible display |
| CN108172543A (en) * | 2018-01-12 | 2018-06-15 | 武汉华星光电半导体显示技术有限公司 | The stripping means and underlay substrate of a kind of flexible substrates |
| CN110408909A (en) * | 2018-04-26 | 2019-11-05 | Spts科技有限公司 | The method for depositing SiN film |
| CN109449076A (en) * | 2018-08-02 | 2019-03-08 | 中山大学 | A kind of silicon-rich silicon nitride thin films low temperature preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113818010A (en) * | 2021-10-26 | 2021-12-21 | 华中科技大学 | Method for modifying organic polymer material and modified organic polymer material |
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