JPS60149773A - Formation of cvd film - Google Patents
Formation of cvd filmInfo
- Publication number
- JPS60149773A JPS60149773A JP516984A JP516984A JPS60149773A JP S60149773 A JPS60149773 A JP S60149773A JP 516984 A JP516984 A JP 516984A JP 516984 A JP516984 A JP 516984A JP S60149773 A JPS60149773 A JP S60149773A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- ultrafine powder
- cvd
- furnace
- material gas
- 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.)
- Granted
Links
Classifications
-
- 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
-
- 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
-
- 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
- C23C16/24—Deposition of silicon only
Abstract
Description
【発明の詳細な説明】
〔発明の利用分野〕
この発明は、耐熱性、耐摩耗性、耐食性に優れた表面被
膜を化学的蒸着（以下、ＣＶＤという）により形成する
方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Application of the Invention] The present invention relates to a method for forming a surface coating with excellent heat resistance, wear resistance, and corrosion resistance by chemical vapor deposition (hereinafter referred to as CVD).
近年、メッキ技術は着実な進歩をしており、特に液相メ
ッキ分野で見られる有害廃棄物の処理の難かしさあるい
は電解メッキに可能な材料が限られていること等から、
気相メッキ技術の研究開発が多方面で盛んに行なわれて
おり、一部では実用化の段階に入っている。In recent years, plating technology has made steady progress, especially due to the difficulty of disposing of hazardous waste seen in the liquid phase plating field and the limited materials that can be electrolytically plated.
Research and development of vapor phase plating technology is actively being carried out in many fields, and some of them have reached the stage of practical application.
ＣＶＤは金属材料の表面を硬化する有効な手段の一つで
あるが、そのメカニズムが複雑であるため、安定した性
状の被膜を形成するには蒸着温度、送入ガス温度、組成
および系内圧力等の精密な制御が必要である。CVD is one of the effective means of hardening the surface of metal materials, but its mechanism is complex, so forming a film with stable properties depends on the deposition temperature, gas supply temperature, composition, and system pressure. etc., precise control is required.
一方、工業化のための重要な因子として蒸着速度がある
。ＣｖＤの蒸着速度は対象材料あるいは対象材料が同じ
でも使用する原料の種類にもよシ異なるが、大体０．０
１〜２■／ｈｒ 程度である。On the other hand, the deposition rate is an important factor for industrialization. The deposition rate of CvD varies depending on the target material or the type of raw material used even if the target material is the same, but it is approximately 0.0
It is about 1 to 2 ■/hr.
この蒸着速度はＰ Ｖ Ｄの一方であるスパッタリング
と比べれば優れているものの、工業的には性状の良い膜
が可能な限り早く形成されることが望ましい。Although this vapor deposition rate is superior to sputtering, which is one of the PVD methods, from an industrial perspective it is desirable to form a film with good properties as quickly as possible.
この発明の目的は、核発生を与えることにより柱状晶の
ない厚いＣＶＤ膜を速い見かけ上の蒸着速度で形成する
方法を提供することである。It is an object of this invention to provide a method for forming thick CVD films without columnar crystals at a high apparent deposition rate by providing nucleation.
この発明のＣＶＤ膜の形成方法は、反応炉内に超微粉と
原料ガスを供給し、炉内に超微粉の流動雰囲気を作り、
この中で原料ガスに化学反応を起させてメッキ母材に超
微粉が混在した金属又は金属化合物を析出させることを
特徴とするものである。The method for forming a CVD film of the present invention involves supplying ultrafine powder and raw material gas into a reactor, creating an atmosphere in which the ultrafine powder flows, and
The method is characterized in that a chemical reaction is caused in the raw material gas to precipitate a metal or metal compound mixed with ultrafine powder on the plating base material.
上記の構成によると、従来の原料ガスのみによる方法に
比べて、析出物の中に混在された超微粉の量だけ膜が厚
くなる。即ち、一定の膜厚を形成するのに、超微粉を混
在させて形成すれば見かけ上の蒸着速度は速くなる。According to the above configuration, the film becomes thicker by the amount of ultrafine powder mixed in the precipitates, compared to the conventional method using only source gas. That is, if a film having a constant thickness is formed by mixing ultrafine powder, the apparent deposition rate will increase.
以下、この発明の実施例を図面に基づいて説明する。 Embodiments of the present invention will be described below based on the drawings.
第１図は本発明の第１実施例を示すもので、炉の外部で
作った超微粉を供給するＣＶＤの基本プロセスである。FIG. 1 shows a first embodiment of the present invention, which is a basic CVD process in which ultrafine powder produced outside the furnace is supplied.
原料ガス供給装置１において、所定の温度で昇華又は蒸
発させた揮発主金属化合物塩、例えば＋９ｉｃｚ、、Ｗ
ＦＴｌ Ｉ Ｔ＋ｃＪ４、Ｚｒｃ１４と、キャリヤカス
、際の原料となる粒径が１０μｍ以下である超微粉体、
−−！；＝↓４４例えばＳｉＣ、ＺｒＯ，、Ａｔ、０．
などの超微粉が装てんされる。そして前記原料ガスと超
微粉は反応炉３に供給される。反応炉３は加熱装置４に
よって反応に適した温度に加熱され、黒鉛などの加熱ボ
ード５上載置されたメッキ母材６にＣＶ Ｉ）膜を形成
する。７は廃ガス処理装置である。In the raw material gas supply device 1, a volatile main metal compound salt sublimated or evaporated at a predetermined temperature, for example +9icz, W
FTl I T+cJ4, Zrc14, carrier waste, and ultrafine powder with a particle size of 10 μm or less, which is the raw material for the carrier residue.
--! ;=↓44 For example, SiC, ZrO, At, 0.
It is loaded with ultra-fine powder such as. The raw material gas and the ultrafine powder are then supplied to the reactor 3. The reaction furnace 3 is heated to a temperature suitable for the reaction by a heating device 4, and a CV I) film is formed on a plating base material 6 placed on a heating board 5 made of graphite or the like. 7 is a waste gas treatment device.
つぎに、上記実施例の作用を説明する。Next, the operation of the above embodiment will be explained.
予じめメッキ母材６は加熱ボード５によって析出させる
金属又は金属化合物であるメッキ物質の蒸着温度に加熱
されている。そして原料ガスと超微粉が炉内に供給され
ると、超微粉は原料ガスの流□れに乗って拡散され、流
動状態が形成される。The plating base material 6 is heated in advance by the heating board 5 to the deposition temperature of the plating material, which is a metal or metal compound, to be deposited. When the raw material gas and ultrafine powder are supplied into the furnace, the ultrafine powder is spread along with the flow of the raw material gas, forming a fluidized state.
この雰囲気の中で原料ガスは化学反応を起す。この反応
によって、 ＳｉＣ，Ｔｉｅなどのメッキ物質がメッキ
母材５に析出する。この析出過程において、超微粉はメ
ッキ物質に捕えられ、析出物内に混在される。従って、
メッキ母材上に形成されるＣＶＤ膜は超微粉の固体を含
んだ緻密なメッキ物質として形成される。そのため、Ｃ
ＶＤ膜は超微粉が核発生の働きをし、微粒多結晶組織が
達成され、しかも析出物に含捷れた超微粉の量に見合っ
て膜が厚く形成されるので、ＣＶＤ膜の形成速度は見か
け上速くなる。In this atmosphere, the raw material gas undergoes a chemical reaction. Due to this reaction, plating substances such as SiC and Tie are deposited on the plating base material 5. During this precipitation process, the ultrafine powder is captured by the plating material and mixed in the precipitate. Therefore,
The CVD film formed on the plating base material is formed as a dense plating material containing ultrafine solid powder. Therefore, C
In the VD film, the ultrafine powder acts as a nucleator, achieving a fine-grained polycrystalline structure, and the film is formed thickly in proportion to the amount of the ultrafine powder included in the precipitate, so the formation speed of the CVD film is Appears to be faster.
つぎに、本発明の他の実施例を第２図に基づいて説明す
る。Next, another embodiment of the present invention will be described based on FIG. 2.
第２図は超微粉を炉内で形成するようにしだＣＶＤの基
本プロセスである。なお、超微粉を形成する手段を除く
他の構成は第１図に示すＣＶＤの基本プロセスと同じな
ので、同一符号を用いてその説明を省略する。Figure 2 shows the basic process of CVD in which ultrafine powder is formed in a furnace. Note that the other configurations except for the means for forming ultrafine powder are the same as the basic CVD process shown in FIG. 1, so the same reference numerals are used and the explanation thereof will be omitted.
超微粉を作るための原料ガスを超微粉原料ガス供給装置
１０で作り、この超微粉原料ガスを反応炉３に供給十り
。一方、予熱ガス供給装置１１は前記原料ガスを炉内に
おいて反応を起させるための予熱カスを供給する。原料
ガスのキャリヤとしては特に限定しないが、原料カスと
キャリヤだけでは高温になった時にＣＶＤ反応を起さな
いものとする。A raw material gas for producing ultrafine powder is produced by an ultrafine powder raw material gas supply device 10, and this ultrafine powder raw material gas is supplied to the reactor 3. On the other hand, the preheating gas supply device 11 supplies preheating dregs for causing the raw material gas to react in the furnace. The carrier for the raw material gas is not particularly limited, but it is assumed that the raw material residue and the carrier alone do not cause a CVD reaction when the temperature reaches a high temperature.
炉内には超微粉原料ガスの噴射ノズル１２と高温の予熱
ガスの噴射ノズル１３が近接して配置され、前記原料ガ
スの噴出と同時に、予熱ガスが吹き込まれる構造になっ
ている。原料ガスは噴射直後に予熱ガスによって高温に
熱せられ、化学反応を起し、金属又は金属化合物の超微
粉が作られる。In the furnace, an injection nozzle 12 for ultrafine raw material gas and an injection nozzle 13 for high-temperature preheated gas are arranged close to each other, and the preheated gas is blown into the furnace at the same time as the raw material gas is ejected. Immediately after injection, the raw material gas is heated to a high temperature by preheating gas, causing a chemical reaction and producing ultrafine powder of metal or metal compound.
この超微粉はガス流に乗って炉内を流動拡散する。This ultrafine powder flows and diffuses inside the furnace on the gas flow.
この状態において、原料ガス供給装置１から原料ガスを
供給すると、第１図に示すＣＶＤの基本プロセスと同じ
メカニズムでメッキ母材６に超微粉とメッキ物質が混在
したＣＶＤ膜が形成される。In this state, when source gas is supplied from the source gas supply device 1, a CVD film containing a mixture of ultrafine powder and plating material is formed on the plating base material 6 using the same mechanism as the basic CVD process shown in FIG.
上記のＣＶＤプロセスで複合材料の作り方を説明する１
、第３図（５）、の）、（Ｑは複合材料のＣＶＤ模式図
である。Explaining how to make composite materials using the above CVD process 1
, FIG. 3(5), ), (Q is a CVD schematic diagram of the composite material.
例えば、複合材料としてＡｔ２０３＋ Ｚｒ Ｏ２を作
るには、複合材料を構成する金属化合物の一つを第３図
（Ａ）で示すように超微粉として供給するか、又は第３
図（Ｂ）、（Ｑのように共に原料ガスとして供給し、炉
内においてその内の一方の原料カスから超微粉（Ｚ ｒ
（＋２、Ａｚ２０． ）を作ることにｊつ”Ｕ下式ノ
ＣＶＤＺｒＣｌ４＋２Ｈ，＋２ＣＯ，ＺｒＯ，＋ ４Ｈ
Ｃｔ＋ ２Ｃ０２ＡｔＣｌ ｓ ＋３ Ｆ（２＋ ３
ＣＯＡ４０＊ ＋ ６ ＨＣｌ ＋ ３００２−〉
〔発明の効果」
上述のとおり、本発明によれば、ＣＶＤ膜の見かけ上の
形成速度を速めることができると共に、析出過程におい
て、金属又は金属化合物の超微粉が混在するから、核発
生によ、、′Ｚ柱状晶を防ぐことができ、安定した性状
のＣＶＤ膜が形成される。For example, to make At203+ZrO2 as a composite material, one of the metal compounds constituting the composite material is supplied as an ultrafine powder as shown in FIG.
Figure (B), (Q) Both are supplied as raw material gases, and ultrafine powder (Z r
To make (+2, Az20.), the following formula was used: CVDZrCl4+2H, +2CO, ZrO, +4H
Ct+ 2C02AtCl s +3 F(2+ 3
COA40* + 6 HCl + 3002-> [Effects of the Invention] As described above, according to the present invention, the apparent formation speed of a CVD film can be increased, and in the precipitation process, ultrafine powder of metal or metal compound is Because of the coexistence of , 'Z columnar crystals can be prevented due to nucleation, and a CVD film with stable properties can be formed.
第１図は、本発明に係るＣｖＤの基本プロセス図、第２
図は本発明に係る他の実施例のＣＶＤの基本プロセス図
、第３図（ト）、（１３）、０は複合材料を作るＣＶＤ
の模式図である。
１・・・原料ガス供給装置、２・・・超微粉供給装置、
３・・・反応炉、６・・・メッキ母材、１０・・・超微
粉原料ガス供給装置、１１・・・予熱カス供給装置。
第１図
第２図
第３図
□２ワワｍ
手続補正書
昭和５９年３１７７日
特許庁長官 殿
１ 事件の表示
昭和５９年 特許願 第 ５１６９ 号２、発明の名称
ＣＶＤ膜の形成方法
３ 補正をする者
事件との関係 特許出願人
名称 （５９０）三井造船株式会社
４代理人
７、 補正の対象
明細書の発明の詳細な説明の欄。
８、補正の内容
（１）明細書第３頁第４行の「一方」を１−法」に改め
る。
（２１明細書第４頁第２０行の「加熱デート」を「加熱
ゲート」に改める。Figure 1 is a basic process diagram of CvD according to the present invention;
The figure is a basic process diagram of CVD of another embodiment according to the present invention.
FIG. 1... Raw material gas supply device, 2... Ultrafine powder supply device,
3... Reaction furnace, 6... Plating base material, 10... Ultrafine powder raw material gas supply device, 11... Preheating dregs supply device. Figure 1 Figure 2 Figure 3 □2 Wawam Procedural amendment dated 3177/1980 Commissioner of the Patent Office 1 Indication of the case 1981 Patent Application No. 5169 2 Title of invention Method for forming CVD film 3 Amendment Name of patent applicant (590) Mitsui Engineering & Shipbuilding Co., Ltd. 4 Agent 7 Column for detailed explanation of the invention in the specification to be amended. 8. Contents of the amendment (1) Change "one side" in the fourth line of page 3 of the specification to "1-method". ("Heating date" on page 4, line 20 of the 21 Specification is changed to "heating gate."
Claims (1)
物塩からなる原料ガスを供給し、高温に加熱されたメッ
キ母材に金属又は金属化合物を析出させるＣＶＤ膜の形
成方法において、前記原料ガスと共に金属又は金属化合
物の超微粉を供給し、この超微粉を炉内で流動状態にし
、この雰囲気の中で原料ガスに化学反応を起させてメッ
キ母材に超微粉が混在した金属又は金属化合物を析出さ
せるようにしたＣＶＤ膜の形成方法。 （２） 前記超微粉が原料ガスから析出されるメッキ物
質と同じ組成であることを特徴とする特許請求の範囲第
１項記載のＣＶＤ膜の形成方法。 （３）前記超微粉が原料ガスから析出されるメッキ物質
と異なる組成であることを特徴とする特許請求の範囲第
１項記載のＣＶＤ膜の形成方法。 （４）前記超微粉が炉内において作られることを特徴と
する特許請求の範囲第１項記載のＣＶ Ｉ）膜の形成方
法。[Claims] (],) A CVD film in which a raw material gas consisting of a volatile metal compound salt vaporized at a low temperature is supplied to a reactor, and metals or metal compounds are deposited on a plating base material heated to a high temperature. In the forming method, ultrafine powder of a metal or metal compound is supplied together with the raw material gas, this ultrafine powder is brought into a fluid state in a furnace, and the raw material gas is caused to undergo a chemical reaction in this atmosphere to form a super fine powder on the plating base material. A method for forming a CVD film in which a metal or metal compound mixed with fine powder is deposited. (2) The method for forming a CVD film according to claim 1, wherein the ultrafine powder has the same composition as a plating substance precipitated from a raw material gas. (3) The method for forming a CVD film according to claim 1, wherein the ultrafine powder has a composition different from that of the plating material deposited from the raw material gas. (4) The CV I) film forming method according to claim 1, wherein the ultrafine powder is produced in a furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP516984A JPS60149773A (en) | 1984-01-13 | 1984-01-13 | Formation of cvd film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP516984A JPS60149773A (en) | 1984-01-13 | 1984-01-13 | Formation of cvd film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60149773A true JPS60149773A (en) | 1985-08-07 |
| JPH05470B2 JPH05470B2 (en) | 1993-01-06 |
Family
ID=11603732
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP516984A Granted JPS60149773A (en) | 1984-01-13 | 1984-01-13 | Formation of cvd film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60149773A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61106769A (en) * | 1984-10-30 | 1986-05-24 | Mitsubishi Electric Corp | Self-lubricating hard film forming device for utilizing gas phase reaction |
| EP0226898A2 (en) * | 1985-12-24 | 1987-07-01 | Sumitomo Electric Industries, Ltd. | Composite powder, composite bodies and process for their production |
| JPH02240263A (en) * | 1989-03-15 | 1990-09-25 | Ulvac Corp | Method and device for chemical vapor deposition mixed with fine objects |
| US7854962B2 (en) * | 2002-08-23 | 2010-12-21 | Tokyo Electron Limited | Gas supply method using a gas supply system |
| CN110182841A (en) * | 2018-11-22 | 2019-08-30 | 中国科学院过程工程研究所 | A kind of steady fluidization process of low temperature Jie prepares TiOxCyNzThe system and method for coated powder |
-
1984
- 1984-01-13 JP JP516984A patent/JPS60149773A/en active Granted
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61106769A (en) * | 1984-10-30 | 1986-05-24 | Mitsubishi Electric Corp | Self-lubricating hard film forming device for utilizing gas phase reaction |
| JPS6346147B2 (en) * | 1984-10-30 | 1988-09-13 | Mitsubishi Electric Corp | |
| EP0226898A2 (en) * | 1985-12-24 | 1987-07-01 | Sumitomo Electric Industries, Ltd. | Composite powder, composite bodies and process for their production |
| US5672382A (en) * | 1985-12-24 | 1997-09-30 | Sumitomo Electric Industries, Ltd. | Composite powder particle, composite body and method of preparation |
| JPH02240263A (en) * | 1989-03-15 | 1990-09-25 | Ulvac Corp | Method and device for chemical vapor deposition mixed with fine objects |
| US7854962B2 (en) * | 2002-08-23 | 2010-12-21 | Tokyo Electron Limited | Gas supply method using a gas supply system |
| CN110182841A (en) * | 2018-11-22 | 2019-08-30 | 中国科学院过程工程研究所 | A kind of steady fluidization process of low temperature Jie prepares TiOxCyNzThe system and method for coated powder |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05470B2 (en) | 1993-01-06 |
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