EP0280184A2 - Procédé de revêtement de fibres d'une couche de silice - Google Patents

Procédé de revêtement de fibres d'une couche de silice Download PDF

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Publication number
EP0280184A2
EP0280184A2 EP88102328A EP88102328A EP0280184A2 EP 0280184 A2 EP0280184 A2 EP 0280184A2 EP 88102328 A EP88102328 A EP 88102328A EP 88102328 A EP88102328 A EP 88102328A EP 0280184 A2 EP0280184 A2 EP 0280184A2
Authority
EP
European Patent Office
Prior art keywords
fibers
silicon
coated
coating
cathode
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.)
Withdrawn
Application number
EP88102328A
Other languages
German (de)
English (en)
Other versions
EP0280184A3 (fr
Inventor
Werner Prof. Dr. Weisweiler
Gerd Dr. Nagel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Publication of EP0280184A2 publication Critical patent/EP0280184A2/fr
Publication of EP0280184A3 publication Critical patent/EP0280184A3/fr
Withdrawn legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D01F11/16—Chemical after-treatment of artificial filaments or the like during manufacture of carbon by physicochemical methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
    • D01F11/125—Carbon
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
    • D01F11/126—Carbides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04—Physical treatment combined with treatment with chemical compounds or elements

Definitions

  • the invention relates to a method for applying a thin, surface-protecting and adhesion-promoting silicon layer to fibers by sputtering.
  • Carbon fibers are generally in contact with carbide-forming metals, e.g. Aluminum, not stable, so that the fibers intended to reinforce these metals must be provided with a protective diffusion barrier layer before they are embedded in the metal matrix.
  • Protective layers are also necessary for fibers that are exposed to oxidizing media, especially at higher temperatures.
  • Silicon carbide offers itself as a protective surface layer due to its good chemical resistance to metals, its good abrasion resistance, its low density and thermal expansion as well as its resistance to oxidation.
  • carbon fibers are treated as reinforcing components in a matrix made of synthetic resin by various methods such as thermal, wet and electrochemical surface oxidation in order to improve the adhesion to the polymer matrix by creating surface-active groups on the fiber.
  • various methods such as thermal, wet and electrochemical surface oxidation
  • polymer coatings by radiation-induced grafting reactions or electropolymerization processes which are carried out both anodically and cathodically on the fiber surface, are known.
  • the polymer coating acts as an adhesion promoter between the fiber and the matrix.
  • Coating from the gas phase is most commonly used with the so-called CVD (chemical vapor deposition) process.
  • CVD chemical vapor deposition
  • DE-C 32 49 624 describes the production of fibers with a superconducting layer made of a niobium compound by reactive direct current cathode sputtering ("d.c. sputtering") of niobium.
  • d.c. sputtering reactive direct current cathode sputtering
  • JP-A 119 222/85 describes carbon fibers with a ceramic layer, e.g. described from silicon carbide.
  • the coating is preferably carried out by the CVD process, other coating processes, e.g. by sputtering are mentioned without giving any further details.
  • the invention was based on the object of developing a technically simple method for applying a surface-protecting and adhesion-promoting silicon layer on reinforcing fibers, in which a large number of individual fibers combined into a bundle can be coated homogeneously at the same time.
  • cathode sputtering The principle of cathode sputtering is known. In this method, a gas discharge process is maintained between two electrodes in a rare gas plasma. In the field required for this, the positively charged noble gas ions generated by collision processes are accelerated to a cathode. On the one hand, the ions striking the cathode with an energy of a few keV release secondary electrons from the cathode surface, which ensure that the gas discharge is maintained; on the other hand, they knock material out of the cathode. These mostly neutral particles diffuse through the gas space and hit the fibers in the gas space with medium energies of a few eV, with the result that they grow there into a closed layer.
  • Technical embodiments and devices for cathode sputtering are described, for example, in the magazine "Vacuum Technology" 1975, pages 1 to 11.
  • the problem with conventional direct current cathode sputtering is that when coating geometrically complex substrates, such as e.g. Fiber bundle, due to the directed atomization, the individual fibers of the fiber bundle shade each other. Because of the poor scattering power of the particles to be applied, a simultaneous coating of the individual fibers is only possible by direct current cathode sputtering if the fiber bundles have been mechanically fanned out. According to the invention, this problem is solved by high-frequency sputtering. Because of the higher mobility of the electrons during the positive half-wave, considerably more electrons reach the silicon or silicon carbide electrode to be atomized than in the negative half-wave in the applied alternating field. Since silicon or silicon carbide is a semiconductor, i.e.
  • a particular advantage of the method according to the invention is that the cathode sputtering can also be operated reactively.
  • one or more components which are chemically active with respect to the dusted cathode material are added to the noble gas plasma.
  • the noble gas plasma For example, with a silicon cathode by adding hydrocarbons to the plasma, depending on the type and concentration of the hydrocarbon and the atomizing power, coatings of the empirical formula Si x C y H z can be obtained, the properties of which between those of silicon, silicon carbide and those of silicon Carbon-hydrogen plasma polymers lie.
  • By adding other reactive gas components, such as oxygen or nitrogen, oxides or nitrides can be separated. It is also possible to obtain concentration gradients which can be set in a targeted manner in the boundary layer between fiber and coating material. For example, you can first deposit a layer of silicon directly on the fiber and then a layer of silicon carbide.
  • a significant increase in the sputtering rate of a few nm coating thickness per minute which can usually be achieved with cathode sputtering arrangements can be achieved by additionally using a focussing layer in the boundary layer between fiber and Achieve magnetic field.
  • magnetron sputterers by applying a magnetic field perpendicular to the direction of electron movement, the electrons are forced on spiral tracks around the field direction, which increases their path and thus the probability of ionization, which makes higher sputtering rates possible.
  • the cathode material can either consist of ⁇ -SiC, which is atomized as such and deposited on the fibers, or it can consist of Si, which can optionally be reacted with reactive additives to the plasma during the atomization, so that the corresponding reaction products on the fibers be put down.
  • the preferred material for the fibers is carbon; However, fibers of glass, silicon carbide, boron, steel or polymers, such as e.g. aromatic polyamides or polypropylene can be coated.
  • the fibers are in the form of fiber bundles, which can contain up to several thousand individual filaments. Expediently, several fiber bundles are coated at the same time by unwinding them from carrier spools, passing them through the plasma and coating them, and rewinding them on take-up spools.
  • the coating can be carried out with several cathodes connected in series, e.g. can be offset from one another by 180 ° or by 120 ° (in the case of three cathodes).
  • the distance between the electrodes is generally between 2 and 10 cm;
  • the size and shape of the electrodes can be designed as desired, they depend on the geometry of the substrates to be coated.
  • the high-frequency cathode sputtering according to the invention can be operated at a frequency from approximately 10 kHz, preferably greater than 10 MHz. In the Federal Republic of Germany, frequencies of 13.56 and 27.2 MHz are approved by Swiss Post. The maximum achievable power density is around 20 W / cm2. In practice, power densities of around 10 W / cm2 are used.
  • the achievable layer thicknesses can vary between 5 and 1000 nm; thicknesses of 10 to 100 nm are preferred.
  • the device shown in the figure contains a coating chamber 1, which can be evacuated to a residual gas pressure of less than 10 3 Pa via two pump connections 2 with a backing pump 3 and a diffusion pump or a turbomolecular pump 4.
  • An inert gas which is also referred to as plasma or working gas, can be introduced into the interior of the coating chamber via an inlet valve 5 and a flow meter 6 is usually argon.
  • a reactive gas for reactive atomization can be metered into the working gas via a second flow meter 6 and a mixing chamber 7, the proportion of which is analyzed via a quadrupole mass spectrometer 8.
  • a working pressure of, for example, 0.1 to 2 Pa, which is predetermined by the cathode sputtering process and electrode spacing, can be kept constant by supplying the recipient with so much gas through the inlet valve 5 that the desired working pressure is obtained when the gas is pumped out uniformly via a throttle valve 9 sets.
  • the target material 10 e.g. SiC or Si
  • cathodes 11 which in turn are electrically insulated from the walls of the coating chamber
  • the energy required for this can be supplied to the cathodes 11 via a coaxial feed line and an adaptation network 13 from an external high-frequency generator 14.
  • the plasma itself serves as an ionization source for the gases that are used for atomization.
  • the fiber bundles 15 to be coated are guided through the plasma 12 at a distance of 3 to 6 cm from the target surfaces.
  • the fiber bundles 15 are transported by unwinding spools 16, which lie outside the plasma zone and are electrically insulated from the walls of the coating chamber, through the plasma 12 via two deflection rollers 17. There, the fiber bundles are hit by particles which emerge from the target surface by ion bombardment and which grow up to form the actual coating.
  • the coated fibers are wound up by collecting coils 18, which are driven electromechanically from the outside via a vacuum shaft bushing.
  • the fiber bundles can be heated by infrared radiators 19 before the coating.
  • the fibers coated according to the invention have improved adhesion to synthetic resin matrices; coated carbon and silicon carbide fibers show improved oxidation resistance.
  • the fibers coated according to the invention can be used as reinforcing fibers for ceramic and metallic materials, but in particular for the production of plastic composite materials. All conventional thermoplastics and thermosets are suitable as plastics.
  • Table 2 shows the improved mechanical properties of epoxy resin composites with coated fibers.
  • Composites were produced from a commercially available epoxy resin and 60 vol.% Reinforcing fibers made of carbon (HTA 7 from TOHO) or silicon carbide (Nicalon from Nippon Carbon Co.), which were coated with SiC of different thicknesses.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Inorganic Fibers (AREA)
  • Physical Vapour Deposition (AREA)
EP19880102328 1987-02-26 1988-02-18 Procédé de revêtement de fibres d'une couche de silice Withdrawn EP0280184A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19873706218 DE3706218A1 (de) 1987-02-26 1987-02-26 Vorrichtung und verfahren zur kontinuierlichen beschichtung der einzelnen fasern eines faserbuendels mit oberflaechenschuetzenden und haftvermittelnden carbid- oder plasmapolymer-filmen
DE3706218 1987-02-26

Publications (2)

Publication Number Publication Date
EP0280184A2 true EP0280184A2 (fr) 1988-08-31
EP0280184A3 EP0280184A3 (fr) 1991-07-03

Family

ID=6321837

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19880102328 Withdrawn EP0280184A3 (fr) 1987-02-26 1988-02-18 Procédé de revêtement de fibres d'une couche de silice

Country Status (4)

Country Link
US (1) US4971673A (fr)
EP (1) EP0280184A3 (fr)
JP (1) JPS63309672A (fr)
DE (1) DE3706218A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5021258A (en) * 1990-08-08 1991-06-04 The Dow Chemical Company Method of coating fibers with metal or ceramic material
FR2729659A1 (fr) * 1991-05-17 1996-07-26 Minnesota Mining & Mfg Fibres revetues
EP0928345A4 (fr) * 1996-09-17 1999-08-11
DE19828843A1 (de) * 1998-06-27 1999-12-30 Daimler Chrysler Ag Verfahren zur Herstellung von beschichteten Kurzfasern
WO2015197299A1 (fr) * 2014-06-25 2015-12-30 Siemens Aktiengesellschaft Fibres de carbone à surface modifiée et procédé de modification d'une surface de fibre de carbone et utilisation des fibres de carbone

Families Citing this family (21)

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Publication number Priority date Publication date Assignee Title
DE3832692A1 (de) * 1988-09-27 1990-03-29 Leybold Ag Dichtungselement mit einem absperrkoerper aus einem metallischen oder nichtmetallischen werkstoff und verfahren zum auftragen von hartstoffschichten auf den absperrkoerper
DE3837306C2 (de) * 1988-09-27 2002-05-16 Knut Enke Kolben und Kolbenstange für einen Schwingungsdämpfer in Kraftfahrzeugen
US4981071A (en) * 1988-11-03 1991-01-01 Leybold Aktiengesellschaft Machine element with coating
US5413851A (en) * 1990-03-02 1995-05-09 Minnesota Mining And Manufacturing Company Coated fibers
JP2588985B2 (ja) * 1990-03-09 1997-03-12 財団法人国際超電導産業技術研究センター 酸化物薄膜の成膜方法
CA2049916C (fr) * 1990-08-29 1997-11-18 Takafumi Uemiya Methode de formation d'un film mince aux extremites de fibres
US5190631A (en) * 1991-01-09 1993-03-02 The Carborundum Company Process for forming transparent silicon carbide films
JPH04300327A (ja) * 1991-03-22 1992-10-23 Ibiden Co Ltd 複合炭素繊維及びｃ／ｃ複合体
JPH09508178A (ja) * 1994-01-21 1997-08-19 ザ カーボランダム カンパニー 炭化ケイ素のスパッタリングターゲット
US7294391B2 (en) * 2003-01-09 2007-11-13 Kabushiki Kaisha Suzutora Contamination resistant fiber sheet
US7282261B2 (en) * 2003-02-13 2007-10-16 National University Of Singapore Method of enhancing the stability of electroactive polymers and redox active materials
ITMI20042323A1 (it) * 2004-12-03 2005-03-03 M & H S R L Procedimento di finitura e coloraziione superficiale di un articolo
US9199227B2 (en) 2011-08-23 2015-12-01 Advanced Ceramic Fibers, Llc Methods of producing continuous boron carbide fibers
US10954167B1 (en) 2010-10-08 2021-03-23 Advanced Ceramic Fibers, Llc Methods for producing metal carbide materials
US8940391B2 (en) * 2010-10-08 2015-01-27 Advanced Ceramic Fibers, Llc Silicon carbide fibers and articles including same
US9275762B2 (en) 2010-10-08 2016-03-01 Advanced Ceramic Fibers, Llc Cladding material, tube including such cladding material and methods of forming the same
US10208238B2 (en) 2010-10-08 2019-02-19 Advanced Ceramic Fibers, Llc Boron carbide fiber reinforced articles
US9803296B2 (en) 2014-02-18 2017-10-31 Advanced Ceramic Fibers, Llc Metal carbide fibers and methods for their manufacture
DE102015014170A1 (de) * 2015-11-03 2017-05-04 Ernst-Moritz-Arndt-Universität Greifswald Vorrichtung zur Behandlung eines faserstrangartigen Objekts mit Schmelzphasenelementen und unter Plasmaeinwirkung
US10793478B2 (en) 2017-09-11 2020-10-06 Advanced Ceramic Fibers, Llc. Single phase fiber reinforced ceramic matrix composites
CN109053205B (zh) * 2018-08-13 2021-01-22 陕西科技大学 一种可控正交排布Si-CF增强HA复合材料及其制备方法和用途

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DE878585C (de) * 1951-03-02 1953-06-05 Heraeus Gmbh W C Verfahren zur Herstellung duenner Schichten von Verbindungen durch Kathodenzerstaeubung
US3627663A (en) * 1968-03-25 1971-12-14 Ibm Method and apparatus for coating a substrate by utilizing the hollow cathode effect with rf sputtering
FR1594182A (fr) * 1968-12-06 1970-06-01
US4209375A (en) * 1979-08-02 1980-06-24 The United States Of America As Represented By The United States Department Of Energy Sputter target
US4309261A (en) * 1980-07-03 1982-01-05 University Of Sydney Method of and apparatus for reactively sputtering a graded surface coating onto a substrate
DE3107914A1 (de) * 1981-03-02 1982-09-16 Leybold-Heraeus GmbH, 5000 Köln Verfahren und vorrichtung zum beschichten von formteilen durch katodenzerstaeubung
US4414085A (en) * 1981-10-08 1983-11-08 Wickersham Charles E Method of depositing a high-emissivity layer
DE3246361A1 (de) * 1982-02-27 1983-09-08 Philips Patentverwaltung Gmbh, 2000 Hamburg Kohlenstoff enthaltende gleitschicht
EP0102489B1 (fr) * 1982-07-31 1987-02-04 BROWN, BOVERI & CIE Aktiengesellschaft Supra-conducteur à filaments multiples et procédé de fabrication
JPS59106572A (ja) * 1982-12-06 1984-06-20 信越化学工業株式会社 炭素繊維の表面処理方法
JPS60119222A (ja) * 1983-12-01 1985-06-26 Mitsubishi Rayon Co Ltd セラミツクス・コ−テイング炭素繊維
US4619865A (en) * 1984-07-02 1986-10-28 Energy Conversion Devices, Inc. Multilayer coating and method

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5021258A (en) * 1990-08-08 1991-06-04 The Dow Chemical Company Method of coating fibers with metal or ceramic material
FR2729659A1 (fr) * 1991-05-17 1996-07-26 Minnesota Mining & Mfg Fibres revetues
EP0928345A4 (fr) * 1996-09-17 1999-08-11
US7498013B2 (en) 1996-09-17 2009-03-03 Hyperion Catalysis International, Inc. Plasma-treated carbon fibrils and method of making same
DE19828843A1 (de) * 1998-06-27 1999-12-30 Daimler Chrysler Ag Verfahren zur Herstellung von beschichteten Kurzfasern
US6143376A (en) * 1998-06-27 2000-11-07 Daimlerchrysler Method for manufacturing coated short fibers
DE19828843B4 (de) * 1998-06-27 2007-02-22 Daimlerchrysler Ag Verfahren zur Herstellung von beschichteten Kurzfasern
WO2015197299A1 (fr) * 2014-06-25 2015-12-30 Siemens Aktiengesellschaft Fibres de carbone à surface modifiée et procédé de modification d'une surface de fibre de carbone et utilisation des fibres de carbone

Also Published As

Publication number Publication date
JPS63309672A (ja) 1988-12-16
US4971673A (en) 1990-11-20
DE3706218A1 (de) 1988-09-08
EP0280184A3 (fr) 1991-07-03

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