WO1995010640A1 - Procede de production d'un revetement en ceramique oxydee - Google Patents

Procede de production d'un revetement en ceramique oxydee Download PDF

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Publication number
WO1995010640A1
WO1995010640A1 PCT/JP1994/001718 JP9401718W WO9510640A1 WO 1995010640 A1 WO1995010640 A1 WO 1995010640A1 JP 9401718 W JP9401718 W JP 9401718W WO 9510640 A1 WO9510640 A1 WO 9510640A1
Authority
WO
WIPO (PCT)
Prior art keywords
coating
sol
producing
oxide ceramic
gel
Prior art date
Application number
PCT/JP1994/001718
Other languages
English (en)
Japanese (ja)
Inventor
Taketo Sakuma
Kunichi Miyazawa
Yoshimi Baba
Yoshiki Mizuno
Original Assignee
Kabushiki Kaisya Advance
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kabushiki Kaisya Advance filed Critical Kabushiki Kaisya Advance
Priority to EP94929654A priority Critical patent/EP0677596A1/fr
Publication of WO1995010640A1 publication Critical patent/WO1995010640A1/fr

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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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1254—Sol or sol-gel processing

Definitions

  • the present invention relates to a method for producing an oxide-based ceramic film using a metal compound solution or sol as a raw material.
  • Oxide-based ceramic films take advantage of their features, and as functional materials such as heat-resistant coatings, abrasion-resistant coatings, and anti-reflection coatings, superconducting materials, ionic conductive materials, capacitors, and memory materials. It contributes widely to the development of industries, such as electronic materials, such as sensors and piezoelectric devices that use piezoelectricity and pyroelectricity. Background art
  • Manufacturing methods for ceramic films include physical vapor methods represented by chemical vapor deposition and sputtering, and liquid methods represented by sol-gel methods.
  • the gas phase method is the most industrialized, but generally has low productivity and it is difficult to control complex compositions.
  • the liquid phase method has advantages that a complicated and uniform composition can be easily obtained and the firing temperature is relatively low.
  • the productivity is not always high even in the liquid phase method-For example, in the case of diving by the sol-gel method, only 0.1 to 0.3 zm thin film can be produced by one coating, and several 1 It is necessary to repeat the coating from 0 to several 100 times.
  • Another reason that the sol-gel method makes it difficult to form a thick film is that the gel shrinks during the volatilization and drying of the alcohol in the sol, so it tends to crack, and this tendency becomes more pronounced as the film becomes thicker. That is.
  • the solution is atomized by electrostatic atomization, so that the solution is volatilized between the atomization unit and the object to be processed, and a gel film containing almost no solvent molecules is formed on the surface of the object to be processed.
  • a uniform film without cracks is formed.
  • the present invention is to form a thick film by a one-pass process, and to dramatically improve productivity.
  • the present invention generally comprises three processes for achieving the above-mentioned object.
  • the first process is the preparation of a stock solution.
  • the metal compound or silicon compound serving as the supply source of the constituent elements needs to be dissolved in a solvent, and the vapor pressure is desirably low (for example, 60 mmHg or less).
  • Such reduction compounds e.g., Si (0C 2 H 5) 4, A1 (0C 3 H 7) 3 alkoxy de like, In (C0CH 2 C0CH 3) such as metal Asechiruasete bets, Pb Examples include metal carboxylates such as (CH 3 C00) 2 and Y (C 17 H 35 C00) 3 and nitrates such as Ni (N 0 3 ) 2 and Y (N 0 3 ) 3 .
  • the solvent used in the present invention needs to dissolve the above-mentioned metal compound or silicon compound, and desirably has a low specific heat and a high vapor pressure.
  • solvents include ethyl alcohol, methyl alcohol, isopropyl alcohol, especially c etc. dimethyl Tokishetan the like, compounds having a large hydroxyl group of infrared absorption, to promote volatilization by irradiating infrared rays It is even more desirable because it can.
  • the second process of the method of the present invention is a coating process by electrostatic atomization.
  • the grounded object is used as the anode
  • the solution atomizer is used as the cathode
  • a negative high voltage is applied to this to create an electrostatic field between the two electrodes, and the atomized fine particles are negatively charged.
  • This is a method of efficiently coating the object to be treated, which is the opposite pole.
  • the high voltage range is preferably between 30 and 120 kV, more preferably between 30 and 70 kV (the distance between the electrodes is preferably between 5 and 40 cm, more preferably between 10 and 30 cm).
  • the distance is larger than 40 cm, the electrostatic field is weakened and the coating efficiency may be lowered, which is not preferable.On the other hand, if the distance is smaller than 10 cm, the solvent fine particles may be difficult to volatilize. preferred not properly. If there is a 10- 8 Scn] or more electrically conductive solution may be a static voltage and the solution so as to keep the insulation state immediately before atomization.
  • At least the surface of the object to be processed must be conductive in order to be grounded. However, there is no great limitation on the shape of the object, and a uniform film can be formed even on a curved surface.
  • the surface to be treated preferably has a high wettability with the bull, and if low, may be subjected to a surface treatment.
  • Preferred examples of the object to be processed include various metals such as iron and copper, conductive glass, and a silicon substrate on which platinum is deposited.
  • the volatilization of the solvent molecules can be promoted by irradiating infrared rays or microphone mouth waves between the electrodes.
  • the infrared ray generating device is not particularly limited.
  • a device in which the infrared lamp light is converted into parallel light by a gold mirror can be used.
  • the output of the microwave is not particularly limited, but is preferably 500 to 3000 W, more preferably 1000 to 2000 W.
  • the third process of the method of the present invention is a process of firing the object to be treated, and may be performed in the air, in a nitrogen atmosphere, or in a vacuum depending on the purpose. It can be performed in the air, in a nitrogen atmosphere, or in a vacuum depending on the purpose.
  • the firing temperature varies depending on the type of ceramics, but the desired ceramics can be obtained preferably at about 400 to 1200 ° C. It is desirable to control the heating and cooling process with a programming temperature controller.
  • Lead acetate (E) trihydrate (special grade, manufactured by Wako Pure Chemical Industries, Ltd.) was dried by heating at 120 ° C. in a vacuum for 3 hours to obtain anhydrous lead acetate. 64.9 g of this was added to the solution prepared above so as not to coagulate. At this point, the lead acetate does not dissolve. Furthermore, by adding 40 g of distilled water diluted with isopropyl alcohol dropwise with stirring, lead acetate can be completely dissolved and a uniform sol can be obtained, and this can be used as a coating sol. did.
  • a 304 stainless steel plate (10 cm x 10 cm x l.5 mm thick) was heat-treated at 1050 ° C for 1 hour in the air, and was used after mirror polishing.
  • paint spraying was performed using Iwata Coating's electrostatic coating machine ESG-110. The output was adjusted to 1 Z second and the atomizing air pressure was adjusted to 3 kg f Z crf. A voltage of 60 kV was applied to the needle electrode of the electrostatic ionization section.
  • the distance between the stainless steel plate to be treated and the coating machine was maintained at 22 cra, and the coating machine was scanned from right to left at a speed of 20 cm / sec to perform electrostatic atomization coating. This scanning can be repeated several times to increase the film thickness.
  • the film thickness after firing obtained by one scan was about 0.35 m.
  • the stainless steel plate coated by three scans was left to dry for about 2 minutes, then dried in an electric furnace (Matsufull furnace, AMF-20-2P manufactured by Asahi Rika Seisakusho) at a speed of 15 minutes to 600 ° C.
  • the mixture was heated, kept at 600 ° C for 1 hour, and allowed to cool.
  • a uniform lead-free zirconate titanate film without cracks was obtained, and a perovskite structure unique to this compound was confirmed by X-ray diffraction.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Chemically Coating (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)

Abstract

L'invention concerne un procédé de production d'un revêtement en céramique oxydée à partir d'une solution comprenant une solution de composé métallique permettant de résoudre les problèmes rencontrés dans divers procédés de production d'un revêtement en céramique oxydée tels que les procédés en phase vapeur dont les procédés de dépôt de vapeur chimiques et physiques dont la productivité est généralement faible, ainsi que le procédé sol-gel également à faible productivité qui ne permet de former qu'une couche fine de 0,1 à 0,3 νm d'épaisseur en une opération d'enduction, une couche plus épaisse risquant de se fissurer lors du retrait du gel lorsque le composant alcoolique s'évapore du sol. Le procédé selon l'invention permet de produire un revêtement en céramique oxydé uniforme par atomisation électrostatique d'une solution contenant une solution de composé métallique ou silicié de manière à former sur la surface d'un substrat un revêtement ne contenant pratiquement pas de molécules de solvant, suivie d'une cuisson.
PCT/JP1994/001718 1993-10-14 1994-10-13 Procede de production d'un revetement en ceramique oxydee WO1995010640A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP94929654A EP0677596A1 (fr) 1993-10-14 1994-10-13 Procede de production d'un revetement en ceramique oxydee

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP5/280291 1993-10-14
JP28029193A JPH07173634A (ja) 1993-10-14 1993-10-14 酸化物系セラミックス膜の製造方法

Publications (1)

Publication Number Publication Date
WO1995010640A1 true WO1995010640A1 (fr) 1995-04-20

Family

ID=17622942

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP1994/001718 WO1995010640A1 (fr) 1993-10-14 1994-10-13 Procede de production d'un revetement en ceramique oxydee

Country Status (3)

Country Link
EP (1) EP0677596A1 (fr)
JP (1) JPH07173634A (fr)
WO (1) WO1995010640A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007030585A1 (de) * 2007-06-27 2009-01-02 Siemens Ag Verfahren zum Erzeugen einer keramischen Schicht auf einem Bauteil
CN107146670A (zh) * 2017-04-19 2017-09-08 安泰科技股份有限公司 一种稀土永磁材料的制备方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4998732A (fr) * 1973-01-29 1974-09-18
JPS5191949A (en) * 1975-02-12 1976-08-12 Surariitoryono tosohoho
JPS61107974A (ja) * 1984-07-06 1986-05-26 ピ−タ−　リブニツツ 中空缶体の内部塗装装置
JPS63277770A (ja) * 1987-05-09 1988-11-15 Nippon Soda Co Ltd 超電導セラミックス薄膜形成用組成物および超電導セラミックス薄膜の製造方法
JPS63291665A (ja) * 1987-05-21 1988-11-29 Nisshin Steel Co Ltd 耐指紋性、耐摩耗性に優れたステンレス鋼板およびその製造方法
JPH05246701A (ja) * 1992-03-04 1993-09-24 Sekisui Chem Co Ltd 金属酸化物被覆体の製造方法
JPH06137805A (ja) * 1992-10-27 1994-05-20 Matsushita Electric Ind Co Ltd ひずみゲージおよびその製造方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4998732A (fr) * 1973-01-29 1974-09-18
JPS5191949A (en) * 1975-02-12 1976-08-12 Surariitoryono tosohoho
JPS61107974A (ja) * 1984-07-06 1986-05-26 ピ−タ−　リブニツツ 中空缶体の内部塗装装置
JPS63277770A (ja) * 1987-05-09 1988-11-15 Nippon Soda Co Ltd 超電導セラミックス薄膜形成用組成物および超電導セラミックス薄膜の製造方法
JPS63291665A (ja) * 1987-05-21 1988-11-29 Nisshin Steel Co Ltd 耐指紋性、耐摩耗性に優れたステンレス鋼板およびその製造方法
JPH05246701A (ja) * 1992-03-04 1993-09-24 Sekisui Chem Co Ltd 金属酸化物被覆体の製造方法
JPH06137805A (ja) * 1992-10-27 1994-05-20 Matsushita Electric Ind Co Ltd ひずみゲージおよびその製造方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP0677596A4 *

Also Published As

Publication number Publication date
EP0677596A1 (fr) 1995-10-18
EP0677596A4 (fr) 1995-08-23
JPH07173634A (ja) 1995-07-11

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