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US2955998A - Process for carrying out technical operations in a glow discharge - Google Patents

Process for carrying out technical operations in a glow discharge Download PDF

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Publication number
US2955998A
US2955998A US410933A US41093354A US2955998A US 2955998 A US2955998 A US 2955998A US 410933 A US410933 A US 410933A US 41093354 A US41093354 A US 41093354A US 2955998 A US2955998 A US 2955998A
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US
United States
Prior art keywords
glow
work
discharge
electrodes
glow discharge
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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.)
Expired - Lifetime
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US410933A
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English (en)
Inventor
Berghaus Bernhard
Bucek Hans
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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32018—Glow discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/34—Methods of heating
    • C21D1/38—Heating by cathodic discharges
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding

Definitions

  • the invention relates to a method of carrying out technical processes in glow discharges, such as annealing, diffusion-annealing, hardening, nitride hardening, carbonisation, metallisation, the carrying out of chemical processes, such as the production of ammonia etc., and it consists in that the energy of the glow discharge is increased in a predetermined part ,of the discharge space as compared with other parts thereof by the approach of the glow layers on two electrodes.
  • a glow layer is to be understood as that region which follows the so-called dark space covering each electrode surface and which can be measured by the occurrence of the cathode drop in the distribution of the potential be tween the electrodes.
  • the present invention does away with these-called hollow cathode effect described in the literature as being detrimental and to be avoided in all circumstances.
  • a workpiece connected up as a cathode is arranged with its surface to be treated opposite a part also connected as a cathode, for instance, another surface of the same workpiece, another workpiece, or an auxiliary electrode, at such a distance that the overlapping of the glow layers effects an increased ionization.
  • the said surfaces should be arranged so close together that, at the selected gas pressure of the glow discharge, the boundaries of the glow layers at least touch each other.
  • the distance between the metal workpieces, parts of workpieces, and/or auxiliary electrodes having approximately the same electric voltage is chosen to be equal to or greater than a minimum distance corresponding to about double the dark space thickness of theglow discharge for the same pressure.
  • the work-pieces, parts of work-pieces and/or auxiliary electrodes may be either connected together directly so that they have the same electric voltage, or they may have imparted to them the same or approximately the same voltage, for instance by separate electric leads introduced into the discharge vessel, whereby other applications are made possible as regards the control of the discharge, viz. of the concentration or control of the energy within the desired or predetermined region.
  • Negative direct current potentials that is to say, parts connected up as cathodes, have an especially strong effect; however, the process can also be carried out with alternating currents.
  • the proxi 2 imity of the boundaries of the glow layers is controlled by regulating the pressure of the gas discharge.
  • auxiliary electrodes which are arranged opposite the work-pieces or parts of the workpiece.
  • the approach of the boundaries of the glow layers is controlled by adjusting the distance between the electrodes or also by using auxiliary electrodes. The distance between the electrodes is adjusted to 'be equal to, or smaller than double the thickness of the dark spaces.
  • the balance of energy can be additionally controlled according to the the auxiliary electrodes, which are arranged opposite individual parts of the work-piece, if these parts have'to be heated to a suitably high temperature.
  • the auxiliary electrode may partly surround the work-piece. The distance of the auxiliary electrodes from the work-piece, or from parts of the workpiece, is usually according to the invention, in order to obtain uniform eifects.
  • the approach of the boundaries of the glow layers is effected likewise by pressure regulation, for instance, in the case of tubular work-pieces. If in these particular tubular work-pieces, the hollow space has too large a diameter for the boundaries 'of the glow layers to ap-' tions of a second, between long intervals, during which at most a glow discharge of smaller energy is maintained or the glow discharge is completely switched off.
  • This production of energy pulses may be effected, for instance, by suitably supplying the electric energy intermittently, or by suitably changing the discharge pressure, for instance in such a manner that the gas pressure is increased to such a value that a discharge of great energy no longer takes place between the work-pieces.
  • a similar effect can be obtained with a reduction in the gas pressur
  • the process according to the invention is used in the case of gas pressures which are higher than those usually employed in glow discharges, for instance in the case of gas pressures of one mm. Hg and more, in order to be able to operate more particularly with larger energies.
  • FIG. 1 of the accompanying drawing shows diagrammatically a glow discharge apparatus 1 consisting of a base 3 and a removable cover 2.
  • An electric lead 4 passes through the base 3 and is connected to a tubular work-piece 5.
  • a rod-like auxiliary electrode 7 is maintained in the interior of the said tubular piece by means of a support 8.
  • the tube 5 and the auxiliary electrode 7 are connected as cathodes, whilst the base-plate of the vessel is used as an anode.
  • the inner surface 6 of the tube 5 and the rod 7 are each covered by a glow layer so that these two glow layers lie opposite each other. According to the invention, they are so controlled by the adjustment of the gas discharge pressure that finally they touch each other.
  • the work-piece could thereby be maintained at a moderate temperature, whilst the tungsten rod could be heated up to its fusing temperature. Because of the resulting higher rate of disintegration of the tungsten rod than of the workpiece, the net result was a deposit of tungsten on the workpiece.
  • Figure 2 is a cross-section through the iron tube 5 with the centrally arranged rod 7.
  • the inner surface covered with tungsten is indicated by 6.
  • FIG. 3 shows the treatment of a turbine blade 9 instead of the tube 5.
  • the blade is provided on its front edge 11 with a metal coating of tantalum which is ditfused in and therefore adheres and is corrosion and heat resistant.
  • a tantalum sheet 19 acting as an auxiliary electrode, at a distance 12 which is equal to, or smaller than, double the thickness of the dark space which covers the electrodes in the glow discharge which is being used. It was found that although the whole surface of the blade was enriched on its surface with small amounts of tantalum, the part indicated in dash line received a much thicker adherent coating of tantalum.
  • Figure 4 differs from Figure 3 in that, for instance, six turbine blades 14 are subjected to such a treatment, the same being arranged around a central tantalum rod 15.
  • the individual turbine blades as well as the central tantalum rod are again so connected as to act as cathodes, so that the glow layers of the blades and of the tantalum rod are close to, or contact, each other.
  • the surfaces 13 indicated in dash line were strongly enriched with tantalum as in the case of the example shown in Figure 3, so that all the blades were covered with a firmly adhering and corrosion resistant outer layer 13.
  • the step which comprises adjusting the gas pressure and the distance between the cathodes to bring the boundaries of their glow layers at least into contact with each other to effect increase of the energy of the glow discharge in a predetermined part of the discharge space as compared with other parts of the discharge space.
  • a work-piece constitutes one of the cathodes and is arranged with its surface to be treated opposite the other cathode.
  • a workpiece having a hollow space is arranged as one of the cathodes and at least partly surrounds the second cathode.
  • a process for carrying out metallurgical, chemical and other technical processes in a glow discharge between heated electrodes in a low pressure gas atmosphere comprising elfecting increase of the energy of the glow discharge between the electrodes by so relating the gas pressure and the distance between the electrodes that the glow layers on the two electrodes are caused to at least contact each other.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical Vapour Deposition (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
US410933A 1953-02-17 1954-02-17 Process for carrying out technical operations in a glow discharge Expired - Lifetime US2955998A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CH785878X 1953-02-17

Publications (1)

Publication Number Publication Date
US2955998A true US2955998A (en) 1960-10-11

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ID=4536581

Family Applications (1)

Application Number Title Priority Date Filing Date
US410933A Expired - Lifetime US2955998A (en) 1953-02-17 1954-02-17 Process for carrying out technical operations in a glow discharge

Country Status (7)

Country Link
US (1) US2955998A (fr)
BE (1) BE526527A (fr)
CH (1) CH314340A (fr)
DE (1) DE976529C (fr)
FR (1) FR1097674A (fr)
GB (1) GB785878A (fr)
NL (2) NL83318C (fr)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3180816A (en) * 1961-03-30 1965-04-27 Rordorf Horst Discharge chamber with current lead-in
US3231484A (en) * 1956-10-27 1966-01-25 Berghaus Elektrophysik Anst Method of sustaining a glow discharge in a high pressure area
US3239368A (en) * 1962-04-26 1966-03-08 Nra Inc Method of preparing thin films on substrates by an electrical discharge
US3314873A (en) * 1962-11-28 1967-04-18 Western Electric Co Method and apparatus for cathode sputtering using a cylindrical cathode
US3394066A (en) * 1962-09-20 1968-07-23 Little Inc A Method of anodizing by applying a positive potential to a body immersed in a plasma
US3423562A (en) * 1965-06-24 1969-01-21 Gen Electric Glow discharge apparatus
US3723289A (en) * 1971-08-12 1973-03-27 Celanese Corp Method and apparatus for plasma treatment of substrates
US3983022A (en) * 1970-12-31 1976-09-28 International Business Machines Corporation Process for planarizing a surface
DE2811942A1 (de) * 1977-03-23 1978-10-05 Vide & Traitement Sa Ofen fuer thermochemische behandlung von metallen
FR2546023A1 (fr) * 1983-05-10 1984-11-16 Balzers Hochvakuum Dispositif et procede pour traiter la paroi interieure d'un tube au moyen d'un effluve electrique

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3256818A (en) * 1955-11-26 1966-06-21 Berghaus Bernhard Method of reducing barrel wear
DE1271267B (de) * 1961-04-14 1968-06-27 Litton Systems Inc Niederdruck-Quecksilberdampfentladungsroehre
CH551496A (de) * 1970-09-21 1974-07-15 Berghaus Bernhard Elektrophysi Verfahren zur verfestigung der oberflaeche von werkstuecken aus eisen und stahl.
DE3029339C2 (de) * 1979-09-14 1984-11-22 Hitachi, Ltd., Tokio/Tokyo Glimmentladungs-Oberflächenbehandlungsverfahren und -vorrichtung
GB8431422D0 (en) * 1984-12-13 1985-01-23 Standard Telephones Cables Ltd Plasma reactor vessel
US4749589A (en) * 1984-12-13 1988-06-07 Stc Plc Method of surface treatment
DE19652634C2 (de) * 1996-09-13 2002-12-19 Euromat Ges Fuer Werkstofftech Verfahren zum Innenbeschichten eines metallischer Bauteils, insbesondere eines Bauteils mit einem zylindrischen Hohlraum, eine Vorrichtung zu dessen Durchführung sowie die Verwendung des Verfahrens
DE19722056A1 (de) * 1997-05-27 1998-12-03 Roland Dr Gesche Verfahren und Anordnung zum Herstellen dünner Schichten mittels Niederdruck-Gasentladung in einer Hohlkathode
CN102844459B (zh) 2009-08-07 2016-03-30 世伟洛克公司 低真空下的低温渗碳
WO2013109415A1 (fr) 2012-01-20 2013-07-25 Swagelok Company Écoulement concourant de gaz d'activation pour carburation à basse température

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1162149A (en) * 1914-10-22 1915-11-30 Engelhardt A Eckhardt Process of making wear-withstanding coat.
US2164595A (en) * 1936-12-07 1939-07-04 Siemens Ag Method of coating electrodes
GB510993A (en) * 1937-08-26 1939-08-11 Bernhard Berghaus Improvements in and relating to the coating of articles by means of thermally vaporised material
US2237328A (en) * 1938-02-19 1941-04-08 Birdseye Electric Corp Metal-coating bulbs or the like
US2256771A (en) * 1937-08-15 1941-09-23 Berghaus Method of coating articles by cathode disintegration
US2434931A (en) * 1944-12-01 1948-01-27 Bell Telephone Labor Inc Method and apparatus for ionic discharge coating
US2438561A (en) * 1942-04-30 1948-03-30 Gen Electric Electrothermal deposition apparatus

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL163085B (nl) * 1950-08-03 Siemens Ag Schakelinrichting voor het overdragen van berichten over een uit verscheidene parallel geschakelde lijnen bestaande overdrachtsweg.

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1162149A (en) * 1914-10-22 1915-11-30 Engelhardt A Eckhardt Process of making wear-withstanding coat.
US2164595A (en) * 1936-12-07 1939-07-04 Siemens Ag Method of coating electrodes
US2256771A (en) * 1937-08-15 1941-09-23 Berghaus Method of coating articles by cathode disintegration
GB510993A (en) * 1937-08-26 1939-08-11 Bernhard Berghaus Improvements in and relating to the coating of articles by means of thermally vaporised material
US2237328A (en) * 1938-02-19 1941-04-08 Birdseye Electric Corp Metal-coating bulbs or the like
US2438561A (en) * 1942-04-30 1948-03-30 Gen Electric Electrothermal deposition apparatus
US2434931A (en) * 1944-12-01 1948-01-27 Bell Telephone Labor Inc Method and apparatus for ionic discharge coating

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3231484A (en) * 1956-10-27 1966-01-25 Berghaus Elektrophysik Anst Method of sustaining a glow discharge in a high pressure area
US3180816A (en) * 1961-03-30 1965-04-27 Rordorf Horst Discharge chamber with current lead-in
US3239368A (en) * 1962-04-26 1966-03-08 Nra Inc Method of preparing thin films on substrates by an electrical discharge
US3394066A (en) * 1962-09-20 1968-07-23 Little Inc A Method of anodizing by applying a positive potential to a body immersed in a plasma
US3314873A (en) * 1962-11-28 1967-04-18 Western Electric Co Method and apparatus for cathode sputtering using a cylindrical cathode
US3423562A (en) * 1965-06-24 1969-01-21 Gen Electric Glow discharge apparatus
US3983022A (en) * 1970-12-31 1976-09-28 International Business Machines Corporation Process for planarizing a surface
US3723289A (en) * 1971-08-12 1973-03-27 Celanese Corp Method and apparatus for plasma treatment of substrates
DE2811942A1 (de) * 1977-03-23 1978-10-05 Vide & Traitement Sa Ofen fuer thermochemische behandlung von metallen
US4200805A (en) * 1977-03-23 1980-04-29 Philippe Le Francois Multicathode thermochemical processing oven
FR2546023A1 (fr) * 1983-05-10 1984-11-16 Balzers Hochvakuum Dispositif et procede pour traiter la paroi interieure d'un tube au moyen d'un effluve electrique

Also Published As

Publication number Publication date
CH314340A (de) 1956-06-15
DE976529C (de) 1963-10-24
FR1097674A (fr) 1955-07-08
GB785878A (en) 1957-11-06
BE526527A (fr)
NL83318C (fr)
NL178001B (nl)

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