US2927231A - Glow discharge apparatus - Google Patents

Glow discharge apparatus Download PDF

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Publication number
US2927231A
US2927231A US624122A US62412256A US2927231A US 2927231 A US2927231 A US 2927231A US 624122 A US624122 A US 624122A US 62412256 A US62412256 A US 62412256A US 2927231 A US2927231 A US 2927231A
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United States
Prior art keywords
glow discharge
energy
heat
chamber
gas
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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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US624122A
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English (en)
Inventor
Bucek Hans
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.)
Elektrophysikalische Anstalt Bernhard Berghaus
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Elektrophysikalische Anstalt Bernhard Berghaus
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G5/00—Compounds of silver
    • 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

  • This invention relates to a method of surface treatment of bodies by means of bombarding the surfaces involved in the process with ions of a foreign material in an electric glow discharge, a pre-determined temperature being maintained at said surfaces.
  • the above-mentioned group of processes on the surface of bodies in partial vacuum in an electric glow discharge also includes the surface treatment of metallic blanks (nitriding, carburization, purifying, roughening, oxidation, reduction, etc.).
  • metallic blanks nitriding, carburization, purifying, roughening, oxidation, reduction, etc.
  • metallurgical and chemical processes melting, dehydration, etc.
  • these thermal processes working on the glow discharge system present the advantage of being admirably economical, apart from-incidental advantages in technical respects and in the quality of the resulting products. Heat is supplied to the surfaces involved in the process by means of an electric glow discharge produced in the immediate neighborhood of the surfaces.
  • the process according to the present invention belongs to the last-named class and is characterized by the fact that the distribution of the foreign substances diffused into the surface of the body is influenced by means for fast heat dissipation from the surfaces involved in the process and concurrently by increasing the discharge energy on these surfaces at the rate of the energy increase required for maintaining the temperature specified.
  • Fig. 1 shows a longitudinal section through a practical embodiment of a receptacle for the glow discharge treatment of hollow shafts pursuant to the invention
  • Fig.2 shows a diagram Wlith several examples of the trend of the depth of hardness in nitrided steel parts
  • Figs. 3 and 4 each show a longitudinal section through other practical embodiments of devices for glow discharge treatment of blanks according to this invention.
  • the blank 1 to be treated on its outside, for instance by metalizing or. nitriding, is electrically insulated from the metal vessel 2 and represents the one electrode as being concentrically encompassed by a counter-electrode 3. Both electrodes are connected to current lead-ins passing through but insulated from the walls of the vessel, as indicated at 4. Between blank 1 and counter-electrode 3 is applied the tension of the current source 5, for instance 500 volts, by which an electric glow discharge is produced between these parts with different potentials at a gas pressure of 1 to 20 mm. Hg in the vessel. The energy transformation' of this discharge is largely concentrated on to the glow edge and the cathode drop space formed in the immediate neighbourhood of the cathode. Where direct current is used, the negative pole of the tension source 5 must naturally contact the blank 1. However, alternating current of the usual frequency (50 cycles) may also be used.
  • the hollow shaft 1 is'cooled in this case on the inside by a refrigerant, such as oil, flowing ofi through the pipe 7 made of insulating material, such as china.
  • the refrigerant stream can be regulated or shut off by means of the valve 8 at the supply pipe 6 made of insulating material.
  • the discharge vessel 2 provided with double-walls is expediently cooled by a refrigerant flowing in through the sleeve 9 and flowing out through the sleeve 10.
  • the interior of the vessel is maintained at the desired underpressure by means of thevacuum pump '11 through the suction pipe 12.
  • the gas" provided for the process can be-conducted into the interior of the vessel through the valve 13 and the pipe 14.
  • the surface temperature of the blank 1 to be treated is 'monitored by means of a radiation pyrometer 17 through an aperture 15 in the counter-electrode 3 and a window 16 inthe wall of the vessel.
  • hollow shaft surface is supervised on the indicator 17 .and the energy transformation inthe glow discharge is stepped up to a corresponding degree, either by increasing the gas pressure in the vessel 2 or by increasing the difference of tension between the hollow shaft 1 and the counter-electrode 3.
  • the refrigerant stream is boosted until the desired energydensity in watt per sq. cm. of surface of the hollow shaft 1 is attained, while at the same time the energy transformation is steadily increased so as to maintainthe surface temperature specified-
  • an automatic pilot may be provided for controlling the rate of heat dissipation and the increase of energy, this pilot being governed by the radiation pyrometer 17.
  • the process for reaching'a specific penetration'depth of the intro-diffused substance is shortened, which represents a definite progress over the diffusion methods hitherto in common use, because it has been generally assumed that the diffusion speed cannot be influenced at a particular surface temperature.
  • the quality of the surface portion produced by introdilfusion differs from that of the nitriding layers-obtained without energy increase, in particular in respect of surface hardness and also of the hardness depth trend and the mechanical properties, such as chipping resistance, ductility, porosity and change in volume.
  • a detachable cooling device is mounted on to the outside jacket of thepipe 20 to be treated, this device consisting for instance of the cooling cylinder 21, the end walls 22 and 23 of which are provided each with a bore fitting the pipe 20, against which these end walls are sealed by means of the elastic packings 24 and 25, respectively.
  • a circular space 26 is formed around the pipe 20, through which a liquid or eeevasl gaseous cooling agent can how by way of inlet 27 and outlet 28.
  • the two mouths of the pipe 20 protrude from the cooling cylinder 21 into dome-like extensions formed by the caps 29 and 30 secured in a gas-tight manner to the end walls 22 and 23 respectively.
  • the two domelike extensions are interconnected by the bore of the pipe 20 and jointly form the glow discharge space.
  • a hollow counter-electrode 31 extends through the pipe 20 and is passed through the caps 29 and 30 with insulators 32 and 33, respectively. This hollow electrode 31 is connected to one of the poles of the tension source 34, while the other pole stands in connection with the cooling cylinder 21, and, through the lead 35, with the pipe 20.
  • Through pipes 36 and 37, the treating gas is conducted into the gas discharge chamber and pumped out of it, respectively.
  • a glow discharge is generated between the inside wall of the pipe 20 and the hollow electrode 31, and when the pipe 20 operates at least intermittently as the cathode, this discharge heats up the inside wall.
  • the hollow electrode 31 can also be cooled from the inside by a stream of liquid or gas. This is expedient when alternating current is used, for instance, for the purpose of avoiding an excessive heating up of the hollow electrode acting intermittently as the cathode.
  • direct current is used in conjunction with a hollow electrode acting as the anode, it might be expedient to cool the electrode in order to dissipate the heat originating from the inside wall of the pipe.
  • the means to be provided pursuant to the process of this invention for the fast dissipation of heat from the surfaces involved in the process do not necessarily require a coolant stream as in the practical examples indicated in Figs. 1 and 3.
  • cooling might be satisfactorily effected merely by intense heat dissipation or heat radiation.
  • a practical example of this case is outlined in Fig. 4, in which all minor details are omitted.
  • This example pertains to the surface treatment of the inside wall of a metal sleeve 40.
  • the sleeve 40 is inserted into a massive metal block 41 of good heat conductivity, for instance of copper, this block presenting an accurately fitting bore 42.
  • the mouth of the sleeve 40 faces a discharge chamber 43 formed by a cowl 45 secured to the block 41 with the insulating ring 44 in an electrically insulated and gastight fashion.
  • An electrode bar 47 is fitted inside the cowl with insulator 46 in a gastight fashion, this bar extending into the sleeve 40 and being connected outside the cowl 45 to one of the poles of a tension source 48, this pole also contacting the metal block 41.
  • the other pole of the tension source 48 is connected to the metal cowl 45 insulated from the block 41 and from the electrode bar 47.
  • the heat produced in this manner on the inside wall of the sleeve 40 is dissipated fast by the large mass of the metal block 41.
  • the intense radiation and air cooling achieved by virtue of the large outside surface of the block 41 is sutficient to prevent the temperature of the inside wall of 6 the sleeve 40 from increasing beyond the value specified. If not, an additional liquid or gas system can be provided for cooling the block 41.
  • the described heating up of the sleeve 40 by means of the hollow cathode effect can be effectively influenced with this type of apparatus by regulating the gas pressure in the chamber 43, thus permitting safe control.
  • the efiect desired can be obtained both with a direct current source and an alternating current source.
  • This hollow cathode eifect can also be applied for the purpose of producing a higher energy transformation in the predetermined ranges of the surfaces involved in the process.
  • the increased energy density of the glow discharge results in a more intensive ionic bombardment on the surface acting as the cathode, it being possible that both the mean kinetic energy and the number of gas ions impinging per unit of time increase.
  • the metal surface as a result is heated more intensely, which, incidentally, is exactly compensated by the fast heat dissipation to the coolant, it is probable that a deeper penetration into the outer layers of the lattice structure of the body and a larger quantity of atomic gas at the limit layer play a part.
  • Apparatus for the diffusion treatment of a metallic body in a gaseous atmosphere comprising a discharge chamber having connections for evacuating the same and having at least one insulated current lead-in, gas supply and gas suction lines connected to said chamber, means for suspending a metallic body within the chamber and for electrically insulating the same from the walls of the chamber, means for electrically connecting the body with a current lead-in which is at least periodically connected to the negative pole of a source of current, a metallic member providing a counter-electrode for producing with the said body a glow discharge therebetween, the other pole of the source of current being connected to said metallic member, said metallic body being hollow, and electrically insulated means for conducting a cooling agent to and from the holow interior of said body and in direct contact therewith to promote the withdrawal of heat.
  • Apparatus for the diffusion treatment of a cylindri cal metallic body in a gaseous atmosphere comprising a metallic discharge chamber adapted to surround said body and having gas supply and gas suction conduits connected thereto, at least one electrically insulated cur rent lead-in connected with said body in the interior of the chamber, said lead-in being adapted to be connected externally of the chamber and at least temporarily with the negative pole of a source of current, the other pole of the source of current being connected with the wall of the chamber, a cooling jacket about the chamber and providing an annular cooling space, conduits for charging a cooling agent into and discharging the same from said jacket, and means for directing a current of cooling agent into direct contact with said metallic body to promote the withdrawal of heat.
  • Apparatus for the diffusion treatment of a cylindrical metallic body in a gaseous atmosphere comprising a metallic discharge chamber adapted to surround said body and having gas supply and gas suction conduits connected thereto, at least one electrically insulated current lead-in connected with said body in the interior of the chamber, said lead-in being adapted to be connected externally of the chamber and at least temporarily with the negative pole of a source of current, the other pole of the source of current being connected with the wall of the chamber, a cooling jacket about the chamber and providing an annular cooling space, conduits for charging a cooling agent into and discharging the same from said jacket, and electrically insulated supply and discharge conduits for cooling agent connected with the hollow interior of the cylindrical body for directing a current'of cooling agent into direct contact with said metallic body to promote the withdrawal of heat.
  • Apparatus for the diffusion treatment of the interior surfaces of hollow metallic bodies of relatively small dimensions in a gaseous atmosphere comprising a discharge chamber composed of a massive metallic block provided with a bore forming a socket and a cowl overlying said block, means for evacuating the chamber, gas a supply and gas suction conduits connected with the chamber, at least one current lead-in electrically insulated from the metallic socket, said lead-in being connected exter- References Cited in the file of this patent UNITED STATES PATENTS 2,371,27 Berghaus et-al Mar. 13, 1945 2, 77,071 I'Carne Apr.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Discharge Heating (AREA)
US624122A 1955-11-22 1956-11-23 Glow discharge apparatus Expired - Lifetime US2927231A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CH852070X 1955-11-22

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US (1) US2927231A (de)
CH (1) CH349284A (de)
DE (1) DE1060217B (de)
FR (1) FR1210232A (de)
GB (1) GB852070A (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3096221A (en) * 1959-09-15 1963-07-02 To A Kako Kabushiki Kaisha Method of quick nitrification in which fluidized particles are employed
US3099589A (en) * 1959-09-15 1963-07-30 To A Kako Kabushiki Kaisha Method of cementation in which fluidized carbon powder particles are employed
US3423562A (en) * 1965-06-24 1969-01-21 Gen Electric Glow discharge apparatus
US4878570A (en) * 1988-01-25 1989-11-07 Dana Corporation Surface hardened sprags and rollers
EP0833366A3 (de) * 1996-09-30 1998-06-24 Becton, Dickinson and Company Gerät zur Abscheidung einer Sperrschicht auf dreidimensionale Gegenstände
WO2010081827A1 (de) 2009-01-15 2010-07-22 Robert Bosch Gmbh Verfahren und vorrichtung zur wärmebehandlung von bauteilen mittels plasmabeheizung
US20190256973A1 (en) * 2018-02-21 2019-08-22 Southwest Research Institute Method and Apparatus for Depositing Diamond-Like Carbon Coatings

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH409694A (de) * 1962-11-06 1966-03-15 Berghaus Elektrophysik Anst Verfahren zur Behandlung von Teilen eines Kugelschreibers
FR2332336A1 (fr) * 1975-11-21 1977-06-17 Vide & Traitement Sa Procede et four pour la realisation de traitements de metaux par bombardement ionique
FR2446327A1 (fr) * 1979-01-09 1980-08-08 Fours Indls Cie Procede de traitement thermochimique de la paroi interne de corps ouverts a deux bouts par bombardement ionique, et dispositif pour la mise en oeuvre
FR2525636A1 (fr) * 1982-04-23 1983-10-28 Creusot Loire Methode et dispositif de nitruration ionique d'orifices allonges de petits diametres de pieces en aciers
CH659346A5 (de) * 1983-05-10 1987-01-15 Balzers Hochvakuum Vorrichtung zum behandeln der innenwand eines rohres.

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB427623A (en) * 1932-07-19 1935-04-23 Deutsche Edelstahlwerke Ag A method of treating metallic articles or the metallic surface layers or coatings of articles
GB529544A (en) * 1938-06-08 1940-11-22 Bernhard Berghaus Improvements in and relating to the thermal obtention of metals from metal compounds
US2371278A (en) * 1938-01-25 1945-03-13 Electric reaction furnace
US2677071A (en) * 1948-06-30 1954-04-27 Rca Corp Voltage reference tube
US2755159A (en) * 1953-05-19 1956-07-17 Sylvania Electric Prod Vapor filling process for discharge lamps

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB427623A (en) * 1932-07-19 1935-04-23 Deutsche Edelstahlwerke Ag A method of treating metallic articles or the metallic surface layers or coatings of articles
US2371278A (en) * 1938-01-25 1945-03-13 Electric reaction furnace
GB529544A (en) * 1938-06-08 1940-11-22 Bernhard Berghaus Improvements in and relating to the thermal obtention of metals from metal compounds
US2677071A (en) * 1948-06-30 1954-04-27 Rca Corp Voltage reference tube
US2755159A (en) * 1953-05-19 1956-07-17 Sylvania Electric Prod Vapor filling process for discharge lamps

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3096221A (en) * 1959-09-15 1963-07-02 To A Kako Kabushiki Kaisha Method of quick nitrification in which fluidized particles are employed
US3099589A (en) * 1959-09-15 1963-07-30 To A Kako Kabushiki Kaisha Method of cementation in which fluidized carbon powder particles are employed
US3423562A (en) * 1965-06-24 1969-01-21 Gen Electric Glow discharge apparatus
US4878570A (en) * 1988-01-25 1989-11-07 Dana Corporation Surface hardened sprags and rollers
EP0833366A3 (de) * 1996-09-30 1998-06-24 Becton, Dickinson and Company Gerät zur Abscheidung einer Sperrschicht auf dreidimensionale Gegenstände
WO2010081827A1 (de) 2009-01-15 2010-07-22 Robert Bosch Gmbh Verfahren und vorrichtung zur wärmebehandlung von bauteilen mittels plasmabeheizung
US20190256973A1 (en) * 2018-02-21 2019-08-22 Southwest Research Institute Method and Apparatus for Depositing Diamond-Like Carbon Coatings

Also Published As

Publication number Publication date
FR1210232A (fr) 1960-03-07
DE1060217B (de) 1959-06-25
GB852070A (en) 1960-10-26
CH349284A (de) 1960-10-15

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