EP1143031A2 - Boruration au plasma - Google Patents

Boruration au plasma Download PDF

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Publication number
EP1143031A2
EP1143031A2 EP01110904A EP01110904A EP1143031A2 EP 1143031 A2 EP1143031 A2 EP 1143031A2 EP 01110904 A EP01110904 A EP 01110904A EP 01110904 A EP01110904 A EP 01110904A EP 1143031 A2 EP1143031 A2 EP 1143031A2
Authority
EP
European Patent Office
Prior art keywords
gas
reactor
plasma
treatment
boron
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.)
Ceased
Application number
EP01110904A
Other languages
German (de)
English (en)
Other versions
EP1143031A3 (fr
Inventor
Emilio Rodriguez Cabeo
Günther LAUDIEN
Kyong-Tschong Rie
Swen Biemer
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.)
Volkswagen AG
Original Assignee
Volkswagen AG
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 Volkswagen AG filed Critical Volkswagen AG
Publication of EP1143031A2 publication Critical patent/EP1143031A2/fr
Publication of EP1143031A3 publication Critical patent/EP1143031A3/fr
Ceased legal-status Critical Current

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    • 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
    • C23C8/38—Treatment of ferrous surfaces
    • 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
    • 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
    • C23C8/08—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 only one element being applied

Definitions

  • the present invention relates to a device for producing a boride layer a surface by plasma working comprising a reactor, the one Boron-containing gas medium can be supplied and in which one Glow discharge is generated.
  • the device according to the invention is thereby characterized in that it has a plasma generator which has a pulsed DC voltage with a variable pulse width and / or pulse pause.
  • the device according to the invention preferably has at least one Mass flow meter on for measuring and / or adjusting the composition and / or the flow of one or more of the gases in the gas medium.
  • One can, for example, by changing the gas composition influence the layer formation during the process, this in turn possibly depending on the results of the analysis of the determined Particle composition in plasma.
  • a gas medium which contains two or three components, for example a boron trihalide, hydrogen and a rare gas.
  • one is used for the device according to the invention gas-independent pressure meter to measure the treatment pressure.
  • the pressure meter which is independent of the type of gas, is preferably controlled by a computer.
  • the distribution of the gas in the treatment room of the reactor can e.g. B. via a Carry out a gas shower.
  • the reactor has an additional heater.
  • the present invention also relates to a method of the aforementioned Genre, that by means of a device with the features of one of the device claims 1 to 10 is carried out.
  • FIG. 1 shows a diagram of the Plant structure of a plant as used in the production method according to the invention a boride layer on a surface can be used by plasma working.
  • the attachment comprises a reactor 10 with a treatment room 11 in which the plasma is generated.
  • the treatment room 11 of the reactor 10 is charged with a boron donor medium, that reaches the treatment room 11 via a gas inlet 12 and the feed line 13.
  • a total of three feed lines are connected to the feed line 13, via which the individual components of the treatment gas are supplied.
  • These components are on the one hand the boron trihalide, e.g. As boron trichloride or boron trifluoride, which over the Branch line 14 is fed, which opens into the feed line 13.
  • the second Component is hydrogen gas, which is supplied via branch line 15, which is also opens into the feed line 13.
  • the third component is an inert gas, e.g. B. Argon that is supplied via the branch line 16, which also opens into the supply line 13.
  • mass flow meters 17, 18 and 19 by means of which the flow of the respective component of the treatment gas can be adjusted and is measurable.
  • the reactor 10 further comprises a charging plate 20, which is located in the reactor chamber 11 and rests on two support insulators and the live support (not shown).
  • the voltage supply for generating the glow discharge is carried out schematically shown voltage supply line 21.
  • the plasma generator supplies a pulsed DC voltage with a variable pulse width or pulse pause as below is explained.
  • the composition and the flow of the treatment gas are determined using the Mass flow meters 17, 18, 19 set.
  • the measurement of the treatment pressure takes place via a gas meter-independent pressure meter and is also computer-controlled regulated.
  • the pressure measurement and pressure control is carried out using the in the diagram with 22 designated device, which is connected via line 23 to the treatment room 11 is.
  • a vacuum pump 24 is connected downstream of this pressure control 22 to this line 23 connected.
  • This vacuum pump 24 is located in this Exhaust pipe a device 25 for exhaust gas purification, which is sufficient Exhaust gas treatment ensures.
  • the temperature of the plasma generator is regulated via the Temperature control device 26 and the line 27.
  • the system according to the invention also has an additional heater 28 which in Reactor 10 is housed to achieve the desired treatment temperature in the Treatment room 11.
  • the method according to the invention for producing a boride layer preferably works in the low pressure range, e.g. B. in the range of 1 to 10 hPa, and is by an electrical Activation of the gas atmosphere is supported.
  • the components to be treated (borating) are connected cathodically against the container wall of the treatment room.
  • the preferably made of boron trihalide, e.g. As boron trichloride or boron trifloride, hydrogen and Existing gas medium is placed in the treatment room 11 and experienced in addition to thermal, electrical activation by glow discharge.
  • the Treatment temperature depends on the material to be borated Components and is for example above 700 ° C, preferably at 800 ° C or about that.
  • a pulsed DC voltage is preferably applied in order to enable the surface to be activated by the noble gas ion bombardment before the treatment phase.
  • active excited boron particles are generated during the treatment, which reach the surface of the component and form borides there primarily by diffusion.
  • the reduction of the halogen present in the atmosphere, which is generated from the boron trihalide, is favored by the atomic hydrogen generated in the plasma, which is produced from the H 2 gas supplied.
  • the diagram according to FIG. 2 shows an example of a possible voltage curve in FIG Dependence on the time for a pulsed direct current as it is for an inventive one
  • the method is particularly advantageous.
  • the voltage is z. B. in a medium range 650 volts, the voltage pulse being maintained, for example, 160 ⁇ s and the Pulse pause, for example, is 50 ⁇ s.
  • the pulse pause is therefore about a factor of 3 shorter than the duration of the DC voltage pulse.
  • the period is in Embodiment 210 microseconds and thus the frequency is 4.762 kHz.
  • the duty cycle defined as the ratio of the length of the pulse duration to the pulse pause within one Pulses is 3.2 in the exemplary embodiment. It was found that Using a relatively high voltage requires a longer pulse pause.
  • argon can also be used in the treatment gas at relatively low levels Tensions, e.g. B. achieve good results in the range above 500 volts.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Chemical Vapour Deposition (AREA)
  • Electron Sources, Ion Sources (AREA)
  • Primary Cells (AREA)
  • Apparatus For Radiation Diagnosis (AREA)
  • Plasma Technology (AREA)
EP01110904A 1997-12-15 1998-12-11 Boruration au plasma Ceased EP1143031A3 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19755595 1997-12-15
DE19755595 1997-12-15
EP98965249A EP1044289B1 (fr) 1997-12-15 1998-12-11 Boruration au plasma

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
EP98965249A Division EP1044289B1 (fr) 1997-12-15 1998-12-11 Boruration au plasma

Publications (2)

Publication Number Publication Date
EP1143031A2 true EP1143031A2 (fr) 2001-10-10
EP1143031A3 EP1143031A3 (fr) 2004-04-28

Family

ID=7851902

Family Applications (2)

Application Number Title Priority Date Filing Date
EP01110904A Ceased EP1143031A3 (fr) 1997-12-15 1998-12-11 Boruration au plasma
EP98965249A Expired - Lifetime EP1044289B1 (fr) 1997-12-15 1998-12-11 Boruration au plasma

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP98965249A Expired - Lifetime EP1044289B1 (fr) 1997-12-15 1998-12-11 Boruration au plasma

Country Status (8)

Country Link
US (1) US6783794B1 (fr)
EP (2) EP1143031A3 (fr)
JP (1) JP4588213B2 (fr)
KR (1) KR100583262B1 (fr)
CN (1) CN1198953C (fr)
AT (1) ATE215132T1 (fr)
DE (1) DE59803574D1 (fr)
WO (1) WO1999031291A2 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE524493C2 (sv) * 2002-02-25 2004-08-17 Telia Ab Uppskattningsenhet och metod för att bestämma positionen för en mobil station i ett mobilt kommunikationssystem
CA2623650A1 (fr) * 2005-09-22 2007-04-05 Skaffco Engineering & Manufacturing, Inc. Procede de boruration au plasma
MX2008013386A (es) * 2006-04-20 2009-01-26 Skaff Corp Of America Inc Partes mecanicas que tienen resistencia incrementada contra el desgaste.
US8012274B2 (en) * 2007-03-22 2011-09-06 Skaff Corporation Of America, Inc. Mechanical parts having increased wear-resistance
US8338317B2 (en) * 2011-04-06 2012-12-25 Infineon Technologies Ag Method for processing a semiconductor wafer or die, and particle deposition device
CN104233425B (zh) * 2014-09-29 2017-01-25 河海大学常州校区 微弧渗硼催化溶液和微弧渗硼溶液以及微弧渗硼方法
US10388524B2 (en) * 2016-12-15 2019-08-20 Tokyo Electron Limited Film forming method, boron film, and film forming apparatus

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US3677799A (en) * 1970-11-10 1972-07-18 Celanese Corp Vapor phase boron deposition by pulse discharge
JPS5118944A (ja) * 1974-08-07 1976-02-14 Suwa Seikosha Kk Kisohokaho
JPS56105627A (en) * 1980-01-28 1981-08-22 Fuji Photo Film Co Ltd Manufacture of amorphous semiconductor
DE3322341A1 (de) 1983-06-22 1985-01-03 Siegfried Dr.-Ing. 5135 Selfkant Strämke Verfahren und vorrichtung zur oberflaechenbehandlung von werkstuecken durch glimmentladung
DE3908200C1 (fr) * 1989-03-14 1989-09-07 Degussa Ag, 6000 Frankfurt, De
DE4003623A1 (de) 1990-02-07 1991-08-08 Kloeckner Ionon Verfahren zur steuerung einer anlage zur plasmabehandlung von werkstuecken
US5286534A (en) * 1991-12-23 1994-02-15 Minnesota Mining And Manufacturing Company Process for plasma deposition of a carbon rich coating
US5374456A (en) 1992-12-23 1994-12-20 Hughes Aircraft Company Surface potential control in plasma processing of materials
US5354381A (en) * 1993-05-07 1994-10-11 Varian Associates, Inc. Plasma immersion ion implantation (PI3) apparatus
FR2708624A1 (fr) * 1993-07-30 1995-02-10 Neuville Stephane Procédé de dépôt d'un revêtement protecteur à base de pseudo carbone diamant amorphe ou de carbure de silicium modifié.
JPH07286254A (ja) * 1994-04-21 1995-10-31 Sumitomo Metal Ind Ltd 耐二次加工脆性に優れた鋼板およびその製造方法
JP3050361B2 (ja) * 1994-07-19 2000-06-12 株式会社ライムズ 金属部材のイオン窒化方法
DE4427902C1 (de) * 1994-08-06 1995-03-30 Leybold Durferrit Gmbh Verfahren zum Aufkohlen von Bauteilen aus kohlungsfähigen Werkstoffen mittels einer impulsförmig betriebenen Plasmaentladung
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Also Published As

Publication number Publication date
DE59803574D1 (de) 2002-05-02
KR20010033075A (ko) 2001-04-25
WO1999031291A3 (fr) 1999-09-10
US6783794B1 (en) 2004-08-31
CN1282383A (zh) 2001-01-31
EP1044289A2 (fr) 2000-10-18
KR100583262B1 (ko) 2006-05-25
ATE215132T1 (de) 2002-04-15
JP2002508448A (ja) 2002-03-19
JP4588213B2 (ja) 2010-11-24
EP1143031A3 (fr) 2004-04-28
EP1044289B1 (fr) 2002-03-27
CN1198953C (zh) 2005-04-27
WO1999031291A2 (fr) 1999-06-24

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