CN115125512A - Substrate surface inert treatment method by using thermal decomposition deposition technology of tetramethyldisiloxane - Google Patents

Substrate surface inert treatment method by using thermal decomposition deposition technology of tetramethyldisiloxane Download PDF

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Publication number
CN115125512A
CN115125512A CN202210813777.4A CN202210813777A CN115125512A CN 115125512 A CN115125512 A CN 115125512A CN 202210813777 A CN202210813777 A CN 202210813777A CN 115125512 A CN115125512 A CN 115125512A
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Prior art keywords
substrate
tetramethyldisiloxane
temperature
hours
silicon
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Pending
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CN202210813777.4A
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Chinese (zh)
Inventor
雷金化
王竹倩
邱化玉
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Hangzhou Normal University
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Hangzhou Normal University
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Priority to CN202210813777.4A priority Critical patent/CN115125512A/en
Publication of CN115125512A publication Critical patent/CN115125512A/en
Pending legal-status Critical Current

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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
    • 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
    • C23C16/56—After-treatment

Abstract

The invention discloses a substrate surface inert treatment method by utilizing a thermal decomposition deposition technology of tetramethyldisiloxane, which comprises the steps of putting a substrate S with a clean surface into a vacuum furnace, vacuumizing to below 10 pascals, introducing 1,1,3, 3-tetramethyldisiloxane into the substrate for 1-20 hours at the temperature of 300-600 ℃, and obtaining a substrate S1 with a carbosilane coating deposited on the surface; and vacuumizing the vacuum furnace to below 10 pascals, and introducing air and water into the substrate S1 with the carbosilane coating deposited on the surface for 1-3 hours at the temperature of 200-400 ℃ to obtain the substrate S2 with the silicon inert surface treated. The silicon oil which is liquid at room temperature and does not contain halogen atoms is used as a chemical vapor deposition silicon source, and the silicon component is firmly combined on the surface of the modified base material through the chemical bonding of the functional group on the surface of the base material and the Si-H in the silicon source.

Description

Substrate surface inert treatment method by using thermal decomposition deposition technology of tetramethyldisiloxane
Technical Field
The invention belongs to a surface inert treatment technology, and relates to a substrate surface inert treatment method by utilizing a tetramethyldisiloxane thermal decomposition deposition technology, wherein the surface comprises the surface of a substrate such as metal, glass, ceramic and the like.
Background
In general, since the surface of a substrate such as metal, glass, and ceramic does not have certain properties (such as chemical adsorption property, catalytic property, corrosion resistance, oxidation resistance, and wear resistance), it is necessary to modify the surface of the substrate, and the present invention particularly refers to the substrate such as metal, glass, and ceramic.
The method for modifying the surface of the base material by adding the coating on the surface of the base material is an effective means for modifying the surface of the base material, and the coating can be deposited on the surface of the base material in a chemical vapor deposition manner, for example, the specific coating needs to be selected and used in combination with the required surface properties, wherein one representative deposited coating is a coating containing a silicon compound, but the prior art uses silane which is gaseous at normal temperature or silane containing halogen at normal temperature; silanes which are gaseous at ambient temperature (e.g. silane SiH) 4 Dimethylsilane (CH) 3 ) 2 SiH 2 Trimethylsilane (CH) 3 ) 3 SiH, etc.), is relatively inconvenient to use and has certain potential safety hazard; halogen-containing silanes (e.g. trimethylchlorosilane (CH) 3 ) 3 SiCl, trichlorosilane HCl 3 Si, etc.), there is a possibility that relatively less noble halogen atoms remain on the modified surface after deposition.
The invention provides the use of 1,1,3, 3-tetramethyldisiloxane which is liquid at room temperature, the operation is safer and more convenient, and the possibility of halogen atom residue does not exist.
Disclosure of Invention
The invention aims to provide a method for inerting the surface of a base material by utilizing a tetramethyldisiloxane thermal decomposition deposition technology aiming at the defects of the prior art, which is to deposit 1,1,3, 3-tetramethyldisiloxane on the surface of the base material in a chemical vapor deposition mode so as to realize the surface property of chemical inertness.
The method comprises the following steps:
and S1, placing the substrate S with the clean surface into a vacuum furnace, vacuumizing to below 10 pascals, introducing 1,1,3, 3-tetramethyldisiloxane into the substrate at the temperature of 300-600 ℃ for 1-20 hours, and controlling the air pressure to be 5-20 Pa to obtain the substrate S1 with the carbosilane coating deposited on the surface.
And S2, vacuumizing the vacuum furnace to below 10 pascals, and introducing air and water into the substrate S1 with the carbosilane coating deposited on the surface for 1-3 hours at the temperature of 200-400 ℃ to obtain the substrate S2 with the silicon inert surface treated.
Preferably, the temperature in step S1 is 500-550 ℃, and the reaction time for introducing 1,1,3, 3-tetramethyldisiloxane is 10-15 hours.
Preferably, the temperature in step S2 is 300-350 ℃, and the time for introducing air and water is 1.5-2.5 hours. The invention has the following beneficial effects:
1) the deposition coating techniques of the present invention can be used for a variety of materials, such as metals, glasses, ceramics, and the like.
2) The manner of deposition by chemical vapor deposition is not limited by the shape of the substrate.
3) The coating and the substrate are firmly combined through the chemical reaction of the silicon hydrogen and the substrate.
4) The surface of the base material obtained by the method has chemical inertness, so that the surface of the base material is covered with a layer of carbosilane material.
Drawings
FIG. 1 is a schematic view of an inert surface treatment.
Detailed Description
As described above, in view of the deficiencies of the prior art, the present inventors have made extensive studies and extensive practices, and propose a technical solution of the present invention, which is mainly based on at least: (1) the invention adopts silicon oil which is liquid at room temperature and does not contain halogen atoms, namely 1,1,3, 3-tetramethyldisiloxane, as a chemical vapor deposition silicon source, and the silicon component is firmly combined on the surface of the modified base material through the chemical bonding of the functional group on the surface of the base material and Si-H in the silicon source. (2) The post-treatment of the silicon source deposition adopts safer and cheaper air and water, and the Si-H bond which is not completely reacted in the first step is subjected to inert treatment, so that the process is safer and has low cost.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
FIG. 1 is a schematic view of an inert surface treatment.
Example 1 inert surface treatment of stainless Steel sheet S
1) And placing the stainless steel sheet S with the clean surface in a vacuum furnace, vacuumizing to below 10 pascals, introducing 1,1,3, 3-tetramethyldisiloxane into the substrate at the temperature of 500 ℃ for 10 hours, and controlling the air pressure to be 8Pa to obtain the stainless steel sheet S1 with the carbosilane coating deposited on the surface.
2) And (2) vacuumizing the vacuum furnace in the step 1) to be less than 10 pascal, and introducing air and water into the stainless steel sheet S1 with the carbosilane coating deposited on the surface at the temperature of 300 ℃ for 1.5 hours to obtain a silicon inert surface treated stainless steel sheet S2.
EXAMPLE 2 ceramic sheet C inert surface treatment
1) And placing the ceramic sheet C with the clean surface into a vacuum furnace, vacuumizing to below 10 pascals, introducing 1,1,3, 3-tetramethyldisiloxane into the substrate for 15 hours at the temperature of 550 ℃, and controlling the air pressure to be 10Pa to obtain the ceramic sheet C1 with the carbosilane coating deposited on the surface.
2) And (2) vacuumizing the vacuum furnace in the step 1) to be less than 10 pascal, and introducing air and water into the ceramic sheet C1 with the carbosilane coating deposited on the surface for 2.5 hours at the temperature of 350 ℃ to obtain a silicon inert surface treated ceramic sheet C2.

Claims (5)

1. The inert treatment method for the surface of the base material by utilizing the thermal decomposition deposition technology of the tetramethyldisiloxane is characterized by comprising the following steps of:
s1, placing the substrate S with the clean surface into a vacuum furnace, vacuumizing to below 10 pascals, introducing 1,1,3, 3-tetramethyldisiloxane into the substrate at the temperature of 300-600 ℃ for 1-20 hours, and controlling the air pressure to be 5-20 Pa to obtain a substrate S1 with a carbosilane coating deposited on the surface;
and S2, vacuumizing the vacuum furnace to below 10 pascals, and introducing air and water into the substrate S1 with the carbosilane coating deposited on the surface for 1-3 hours at the temperature of 200-400 ℃ to obtain the substrate S2 with the silicon inert surface treated.
2. The method according to claim 1, wherein the temperature in step S1 is 500-550 ℃.
3. The method according to claim 1 or 2, wherein the reaction time for introducing 1,1,3, 3-tetramethyldisiloxane in step S1 is 10 to 15 hours.
4. The method according to claim 1, wherein the temperature in step S2 is 300-350 ℃.
5. The method according to claim 1 or 4, wherein the time for introducing air and water in step S2 is 1.5-2.5 hours.
CN202210813777.4A 2022-07-11 2022-07-11 Substrate surface inert treatment method by using thermal decomposition deposition technology of tetramethyldisiloxane Pending CN115125512A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210813777.4A CN115125512A (en) 2022-07-11 2022-07-11 Substrate surface inert treatment method by using thermal decomposition deposition technology of tetramethyldisiloxane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210813777.4A CN115125512A (en) 2022-07-11 2022-07-11 Substrate surface inert treatment method by using thermal decomposition deposition technology of tetramethyldisiloxane

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CN115125512A true CN115125512A (en) 2022-09-30

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102741452A (en) * 2009-10-27 2012-10-17 西尔科特克公司 Chemical vapor deposition coating, article, and method
CN103397307A (en) * 2010-02-04 2013-11-20 气体产品与化学公司 Method to prepare silicon-containing film
CN105112886A (en) * 2015-09-18 2015-12-02 杭州天净检测技术有限公司 Inert surface treating technique
CN107523809A (en) * 2017-08-23 2017-12-29 无锡荣坚五金工具有限公司 A kind of preparation method of Silicone hard nano protecting coating

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102741452A (en) * 2009-10-27 2012-10-17 西尔科特克公司 Chemical vapor deposition coating, article, and method
CN106319477A (en) * 2009-10-27 2017-01-11 西尔科特克公司 Chemical vapor deposition coating, article, and method
CN103397307A (en) * 2010-02-04 2013-11-20 气体产品与化学公司 Method to prepare silicon-containing film
CN105112886A (en) * 2015-09-18 2015-12-02 杭州天净检测技术有限公司 Inert surface treating technique
CN107523809A (en) * 2017-08-23 2017-12-29 无锡荣坚五金工具有限公司 A kind of preparation method of Silicone hard nano protecting coating

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