CN102337520A - Method for plating thin film on inner wall of slender pipeline - Google Patents
Method for plating thin film on inner wall of slender pipeline Download PDFInfo
- Publication number
- CN102337520A CN102337520A CN2011102836264A CN201110283626A CN102337520A CN 102337520 A CN102337520 A CN 102337520A CN 2011102836264 A CN2011102836264 A CN 2011102836264A CN 201110283626 A CN201110283626 A CN 201110283626A CN 102337520 A CN102337520 A CN 102337520A
- Authority
- CN
- China
- Prior art keywords
- precursor
- pipeline
- reaction chamber
- coated
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Chemical Vapour Deposition (AREA)
- Chemically Coating (AREA)
Abstract
The invention discloses a method for plating a thin film on an inner wall of a slender pipeline, belonging to the technical field of vacuum film plating. The method comprises the steps of: putting a pipeline to be plated with a film in a reaction chamber, alternatively introducing a gaseous phase precursor to a reactor in a pulse form, wherein the first precursor reaches to the inside of the pipeline and is chemically adsorbed on the inner wall of the pipeline to form a single adsorption layer; introducing a second precursor to react with the first precursor so as to generate a thin film with a single atom layer on the inner wall of the pipeline; cleaning the reactor through inert gas between every two precursor pulses, and repeating the adsorption and reaction processes to generate the thin film layer by layer. The method is used for plating the thin film on the inner wall of the slender pipeline in a gas adsorption and reaction combination manner to solve the problem that the thin film cannot be plated on the inner wall of the slender pipeline in a vacuum film plating method currently; and the method can be used for plating such thin film materials as metal, oxide, nitride, sulfide and fluoride, and the like so as to meet different demands.
Description
Technical field
The invention belongs to technical field of vacuum plating, relate to and a kind ofly be coated with the method for all kinds of films, can be coated with all kinds of thin-film materials such as metal, oxide compound, nitride, sulfide, fluorochemical on the material different surface at inner-walls of duct.
Background technology
Thin film technique is through the development in surplus 100 years, improved relatively till now and ripe, developed into to comprise physical vapor deposition, chemical vapour deposition and other other technical system of wet method film preparing technology three major types.But along with the development of technical need, traditional thin film technique still can not satisfy some special demands.For example, existing various vacuum coating technologies generally can only be coated with film on the not too complicated curved surface of plane or shape; All can't be implemented in the inner-walls of duct plated film; Particularly be coated with film at elongated inner-walls of duct, traditional various film preparing technologies all can't be realized this requirement.
Summary of the invention
The objective of the invention is to the problem that exists in the prior art, provide a kind of and be coated with the method for film, can't realize the technical problem of this requirement to solve existing vacuum coating technology at the slender pipeline inwall.
The present invention is coated with the method for film at the slender pipeline inwall, comprises following process step:
(1) will need the slender pipeline of plated film place with the suitable reaction chamber of pipeline in, reaction chamber is vacuumized.Vacuum ranges is 1 * 10
-2Pa ~ 1 * 10
-3Pa.
(2) in reaction chamber, feed first kind of gas phase precursor A with impulse form, form a single adsorption layer with chemisorption at the inner surface of pipeline of need plated film.
Precursor A is according to the plating material selection, and the presoma kind is a lot, and commonly used have an AlMe
3, TiCl
4, Cu (acac)
2, ZrCl
4, HfCl
4, Pt (acac)
2, WF
6, TaCl
5Or the like.All presomas are gaseous state, as at room temperature being on-gaseous, with heating unit forerunner's volume are heated to be gaseous state.
The flow of gas phase precursor A and pulse duration, general flow range was controlled at 10 ~ 50sccm by concrete presoma decision, and the pulse duration is 2 ~ 10s.
(3) in reaction chamber, feed rare gas element, the unnecessary precursor A of not absorption is got rid of.
Rare gas element is generally selected argon gas for use, its flow 20 ~ 50sccm, time length 5 ~ 30s.
(4) in reaction chamber, feed second kind of gas phase precursor B with impulse form, with the reaction of gas phase precursor A, at monoatomic layer of inner surface of pipeline generation of need plated film.
The gas phase precursor B is according to the plating material selection, and the flow of gas phase presoma and time length are by concrete presoma decision.To with a kind of material that plates, possibly have different presoma combinations.Commonly used have a gaseous state H
2O, H
2, NH
3, O
2, N
2, H
2S etc.The flow of gas phase precursor B generally is controlled at 10 ~ 50sccm, and the pulse duration is 2 ~ 10s.
(5) in reaction chamber, feed rare gas element, the unnecessary precursor B of not absorption is got rid of.Rare gas element is generally selected argon gas for use, and its flow control is at 20 ~ 50sccm, time length 5 ~ 30s.
(6) repeat above-mentioned steps (2) ~ (5), the every repetition once generates a monoatomic layer, and every layer thickness is greatly about 0.03 ~ 0.15nm.According to different materials that are coated with and required thickness, can confirm to react multiplicity.
The present invention compared with prior art has the following advantages:
1, the present invention has realized being coated with film at the slender pipeline inwall, has solved existing various vacuum coating technology, generally can only on the not too complicated curved surface of plane or shape, be coated with film, all can't be implemented in the technical problem of inner-walls of duct plated film.
2, the present invention can be coated with film in various complex surfaces, and the thickness of film has good homogeneity.
3, film coating method of the present invention is simple, and process controllability is strong.
4, flexibility of the present invention is strong, can be coated with all kinds of thin-film materials such as metal, oxide compound, nitride, sulfide, fluorochemical on the material different surface, to satisfy different demands.
Description of drawings
Fig. 1 is the synoptic diagram of film growth of the present invention.
Embodiment
Through specific embodiment the present invention is elaborated in the method that the slender pipeline inwall is coated with film below.
Embodiment 1: with trimethylaluminium and water vapour reaction, generating aluminium sesquioxide is the example explanation.
(1) will need the slender pipeline of plated film to be positioned in the reaction chamber that (inwall of this reaction chamber should be suitable with the outer wall of pipeline, and preferably with slender pipeline insertion reaction chamber interior walls, the inwall that makes pipeline and the inwall of reaction chamber are with on simultaneously.With reference to accompanying drawing 1, wherein 1 is reaction chamber, and 2 is pipeline, and 3 is reaction precursor body A, and 4 is reaction precursor body B), reaction chamber is evacuated to 1 * 10
-3Pa.
(2) in reaction chamber, feed gas-phase reaction precursor A trimethylaluminium (TMA) with impulse form, flow 15sccm, time length 5s forms a single adsorption layer at the inner surface of pipeline of need plated film with chemisorption.
(3) in reaction chamber, feed argon gas (Ar), flow 25sccm, time length 15s gets rid of the unnecessary precursor A trimethylaluminium of not absorption.
(4) in reaction chamber, feed second kind of gas-phase reaction precursor B water vapour (H with impulse form
2O), flow 20sccm, time length 10s with the precursor A trimethylaluminium reaction that is adsorbed on inner-walls of duct, generates the monoatomic layer of an aluminum oxide at the inner surface of pipeline of need plated film.
(5) in reaction chamber, feed argon gas (Ar), flow 25sccm, time length 15s gets rid of unreacted unnecessary presoma water vapour.
(6) repeat above-mentioned steps (2) ~ (5), the every repetition once generates an aluminium sesquioxide monoatomic layer, and every layer thickness is approximately 0.1nm, till thicknesses of layers meets the demands.
Embodiment 2: with trimethylaluminium and hydrogen reaction, generating aluminium is the example explanation.
(1) will need the pipeline of plated film to be positioned in the reaction chamber (pipeline is at the modes of emplacement copper embodiment 1 of reaction chamber), reaction chamber will be evacuated to 2 * 10
-3Pa.
(2) in reaction chamber, feed first kind of gas-phase reaction precursor A trimethylaluminium (TMA) with impulse form, flow 18sccm, time length 6s forms a single adsorption layer at the inner surface of pipeline of need plated film with chemisorption;
(3) in reaction chamber, feed argon gas (Ar), flow 25sccm, time length 15s gets rid of the unnecessary presoma trimethylaluminium of not absorption.
(4) in reaction chamber, feed second kind of gas-phase reaction precursor B hydrogen (H with impulse form
2), flow 15sccm, time length 8s is with precursor A trimethylaluminium (TMA) reaction, at monoatomic layer of inner surface of pipeline generation of need plated film;
(5) in reaction chamber, feed argon gas (Ar), flow 25sccm, time length 15s gets rid of unreacted unnecessary precursor A trimethylaluminium.
(6) repeat above-mentioned steps (2) ~ (5), the every repetition once generates an aluminium monoatomic layer, and every layer thickness is approximately 0.03nm, till thicknesses of layers meets the demands.
Embodiment 3: with titanium tetrachloride and ammonia gas react, generating titanium nitride is the example explanation.
(1) will need the pipeline of plated film to be positioned in the reaction chamber (pipeline is at the modes of emplacement copper embodiment 1 of reaction chamber), reaction chamber will be evacuated to 1 * 10
-3Pa.
(2) in reaction chamber, feed first kind of gas-phase reaction precursor A titanium tetrachloride (TiCl with impulse form
4), flow 20sccm, time length 5s forms a single adsorption layer at the inner surface of pipeline of need plated film with chemisorption.
(3) in reaction chamber, feed argon gas (Ar), flow 20sccm, time length 10s gets rid of the unnecessary precursor A titanium tetrachloride of not absorption.
(4) in reaction chamber, feed second kind of gas-phase reaction precursor B ammonia (NH with impulse form
3), with the precursor A titanium tetrachloride reaction that is adsorbed on inner-walls of duct, generate the monoatomic layer of a titanium nitride at the inner surface of pipeline of need plated film.
(5) in reaction chamber, feed argon gas (Ar), flow 25sccm, time length 8s gets rid of unreacted unnecessary presoma ammonia.
(6) repeat above-mentioned steps (2) ~ (5), the every repetition once, the monoatomic layer of a titanium nitride of generation, every layer thickness is approximately 0.05nm, till thicknesses of layers meets the demands.
Claims (8)
1. one kind is coated with the method for film at the slender pipeline inwall, comprises following process step:
(1) will need the slender pipeline of plated film place with the suitable reaction chamber of pipeline in, reaction chamber is vacuumized;
(2) in reaction chamber, feed first kind of gas phase precursor A with impulse form, form a single adsorption layer with chemisorption at the inner surface of pipeline of need plated film;
(3) in reaction chamber, feed rare gas element, the unnecessary precursor A of not absorption is got rid of;
(4) in reaction chamber, feed second kind of gas phase precursor B with impulse form, with the precursor A reaction, at monoatomic layer of inner surface of pipeline generation of need plated film;
(5) in reaction chamber, feed rare gas element, unreacted unnecessary precursor B is got rid of;
(6) repeat above-mentioned steps (2) ~ (5), the every repetition once generates a monoatomic layer, till thicknesses of layers meets the demands.
2. be coated with the method for film according to claim 1 at the slender pipeline inwall, it is characterized in that: the vacuum tightness in the said reaction chamber of step (1) is 1 * 10
-2Pa ~ 1 * 10
-3Pa.
3. be coated with the method for film according to claim 1 at the slender pipeline inwall, it is characterized in that: the said gas phase precursor A of step (2) is AlMe
3, TiCl
4, Cu (acac)
2, ZrCl
4, HfCl
4, Pt (acac)
2, WF
6, TaCl
5, SnCl
4, InCl
3, CdMe
2, MoCl
5, GaCl
3, ZnCl
2, SiCl
4, CCl
3, BCl
3
4. be coated with the method for film according to claim 1 at the slender pipeline inwall, it is characterized in that: the flow of the said gas phase precursor A of step (2) is 10 ~ 50sccm, and the pulse duration is 2 ~ 10s.
5. be coated with the method for film according to claim 1 at the slender pipeline inwall, it is characterized in that: the said rare gas element of step (3) is an argon gas, and its flow is 20 ~ 50sccm, and the time length is 5 ~ 30s.
6. be coated with the method for film according to claim 1 at the slender pipeline inwall, it is characterized in that: the said gas phase precursor B of step (4) can be gaseous state H
2O, H
2, NH
3, O
2, N
2, H
2S, AsH
3, PH
3, H
2S, H
2Se, HF.
7. be coated with the method for film according to claim 1 at the slender pipeline inwall, it is characterized in that: the flow of the said gas phase precursor B of step (4) is 10 ~ 50sccm, and the pulse duration is 2 ~ 10s.
8. be coated with the method for film according to claim 1 at the slender pipeline inwall, it is characterized in that: the said rare gas element of step (5) is an argon gas, and its flow is 20 ~ 50sccm, and the time length is 5 ~ 30s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102836264A CN102337520A (en) | 2011-09-22 | 2011-09-22 | Method for plating thin film on inner wall of slender pipeline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102836264A CN102337520A (en) | 2011-09-22 | 2011-09-22 | Method for plating thin film on inner wall of slender pipeline |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102337520A true CN102337520A (en) | 2012-02-01 |
Family
ID=45513463
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102836264A Pending CN102337520A (en) | 2011-09-22 | 2011-09-22 | Method for plating thin film on inner wall of slender pipeline |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102337520A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112746265A (en) * | 2020-12-29 | 2021-05-04 | 兰州空间技术物理研究所 | Method for preparing coating on inner surface of spray pipe |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5120785A (en) * | 1974-08-14 | 1976-02-19 | Hitachi Ltd | Cvd makunokeiseihoho |
| CN1826425A (en) * | 2003-07-17 | 2006-08-30 | 三菱商事塑料株式会社 | Method of manufacturing gas barrier film coated plastic container |
| CN101330014A (en) * | 2007-06-22 | 2008-12-24 | 中芯国际集成电路制造(上海)有限公司 | Method for depositing atomic layer and semiconductor device formed by the same |
| CN101864562A (en) * | 2010-07-07 | 2010-10-20 | 南京大学 | Method for preparing oxide surface on metal medical appliance by Atomic Layer Deposition (ALD) technology |
| CN101974734A (en) * | 2010-11-30 | 2011-02-16 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing substrate material with multilayer composite protective film |
-
2011
- 2011-09-22 CN CN2011102836264A patent/CN102337520A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5120785A (en) * | 1974-08-14 | 1976-02-19 | Hitachi Ltd | Cvd makunokeiseihoho |
| CN1826425A (en) * | 2003-07-17 | 2006-08-30 | 三菱商事塑料株式会社 | Method of manufacturing gas barrier film coated plastic container |
| CN101330014A (en) * | 2007-06-22 | 2008-12-24 | 中芯国际集成电路制造(上海)有限公司 | Method for depositing atomic layer and semiconductor device formed by the same |
| CN101864562A (en) * | 2010-07-07 | 2010-10-20 | 南京大学 | Method for preparing oxide surface on metal medical appliance by Atomic Layer Deposition (ALD) technology |
| CN101974734A (en) * | 2010-11-30 | 2011-02-16 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing substrate material with multilayer composite protective film |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112746265A (en) * | 2020-12-29 | 2021-05-04 | 兰州空间技术物理研究所 | Method for preparing coating on inner surface of spray pipe |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101974734B (en) | Method for preparing substrate material with multilayer composite protective film | |
| EP2053143A3 (en) | High quality silicon oxide films by remote plasma cvd from disilane precursors | |
| TW200940738A (en) | Method for forming a titanium-containing layer on a substrate using an ALD process | |
| JP2007277723A5 (en) | ||
| TWI680882B (en) | Laminated body and gas barrier film | |
| EP2067876A3 (en) | ALD or CVD process for producing germanium-antimony-tellurium films | |
| WO2010062582A3 (en) | Vapor deposition method for ternary compounds | |
| TW200615396A (en) | Method of depositing lead containing oxides films | |
| MY159272A (en) | Silicon thin film solar cell having improved haze and methods of making the same | |
| JP5967982B2 (en) | Chemical vapor deposition film formed by plasma CVD method | |
| CN108149225A (en) | A kind of vacuum reaction device and reaction method | |
| CN106068335A (en) | Germanium or the ald of germanium oxide | |
| JP2013185206A5 (en) | ||
| MY141845A (en) | Method of selective region vapor phase aluminizing | |
| CN110528003B (en) | Composite preparation method of coating | |
| CN103938185B (en) | A kind of preparation method of tubular member internal coating | |
| CN102337520A (en) | Method for plating thin film on inner wall of slender pipeline | |
| US8906457B2 (en) | Method of atomic layer deposition using metal precursors | |
| CN110055513A (en) | A kind of powder atomic layer deposition apparatus and its deposition method and application | |
| CN105154853A (en) | Method for depositing film on inner surface of tubular base | |
| CN105132886A (en) | Method for improving uniformity of film deposited on inner surface of tubular base | |
| TW200801227A (en) | Method of depositing chalcogenide film for phase-change memory | |
| CN110724931A (en) | Method for preparing rhenium disulfide film by atomic layer deposition | |
| TW200727345A (en) | Method of forming silicon film by two step deposition | |
| CN110318040B (en) | Atomic layer deposition system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120201 |