EP0015813A1 - Verfahren zum Borieren metallischer oder metallkeramischer Gegenstände und mit einer borierten Oberfläche versehene Gegenstände - Google Patents

Verfahren zum Borieren metallischer oder metallkeramischer Gegenstände und mit einer borierten Oberfläche versehene Gegenstände Download PDF

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Publication number
EP0015813A1
EP0015813A1 EP80400252A EP80400252A EP0015813A1 EP 0015813 A1 EP0015813 A1 EP 0015813A1 EP 80400252 A EP80400252 A EP 80400252A EP 80400252 A EP80400252 A EP 80400252A EP 0015813 A1 EP0015813 A1 EP 0015813A1
Authority
EP
European Patent Office
Prior art keywords
agent
parts
enclosure
gaseous
fluorinated
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
EP80400252A
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English (en)
French (fr)
Inventor
François Henri Joannes Thevenot
Patrice Marie Victor Goeuriot
Julian Haworth Driver
Jean-Paul Raymond Lebrun
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.)
NOUVELLE des Ets PARTIOT - SOFRATER Ste
Association pour la Recherche et le Developpement des Methodes et Processus Industriels
Original Assignee
NOUVELLE des Ets PARTIOT - SOFRATER Ste
Association pour la Recherche et le Developpement des Methodes et Processus Industriels
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 NOUVELLE des Ets PARTIOT - SOFRATER Ste, Association pour la Recherche et le Developpement des Methodes et Processus Industriels filed Critical NOUVELLE des Ets PARTIOT - SOFRATER Ste
Publication of EP0015813A1 publication Critical patent/EP0015813A1/de
Ceased legal-status Critical Current

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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
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
    • 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
    • C23C8/60—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 solids, e.g. powders, pastes
    • C23C8/62—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 solids, e.g. powders, pastes only one element being applied
    • C23C8/68—Boronising
    • 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
    • C23C8/60—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 solids, e.g. powders, pastes
    • C23C8/62—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 solids, e.g. powders, pastes only one element being applied
    • C23C8/68—Boronising
    • C23C8/70—Boronising of ferrous surfaces
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12951—Fe-base component
    • Y10T428/12958—Next to Fe-base component
    • Y10T428/12965—Both containing 0.01-1.7% carbon [i.e., steel]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12951—Fe-base component
    • Y10T428/12972—Containing 0.01-1.7% carbon [i.e., steel]
    • Y10T428/12979—Containing more than 10% nonferrous elements [e.g., high alloy, stainless]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • Y10T428/2495—Thickness [relative or absolute]
    • Y10T428/24967—Absolute thicknesses specified

Definitions

  • the subject of the invention is a process for treating parts of material from the group consisting of alloys of metals of the iron family (Fe, Ni, Co) and by cermets, in which the parts are brought to an operating temperature of of the order of 850 to 1150 ° C. in the presence of a solid boronizing agent and the boronization is activated by simultaneously subjecting the parts to the action of contact of the current of a gaseous fluorinated agent under operating conditions of pressure and temperature defined.
  • the subject of the invention is also a device for implementing the method and parts boronated on the surface.
  • the parts borided by this known process keep traces of powder stuck due to the appearance of a molten phase, so that they must be subjected to an additional treatment to remove the powder. more or less sintered, more or less adherent on their surface.
  • the activating agent which is consumed, being in the treatment bed, it must be regenerated, for example by quarters, with a new powder after each treatment operation.
  • the object of the invention is to propose a new very economical process and a new device making it possible to avoid the abovementioned drawbacks, in particular by obtaining a single-phase layer as regards carbon steels, and by obtaining clean parts without powder adhesion in all cases.
  • the gaseous fluorinated agent containing trifluorinated boroxole is produced by making pass the starting gas through a pulverulent mass of mineral oxides free of cationic impurities, such as simple or complex oxides of silicon, aluminum and magnesium, for example a silica sand, brought to a temperature at least equal to 450 ° C.
  • the agent introduced into the mass brought to at least 450 ° C. is boron trifluoride
  • the effluent will contain trifluorinated boroxole according to the reaction, in which MO is the simple or complex oxide.
  • the fluorinated agent is diluted in a neutral carrier gas.
  • the boriding agent can be, not only B 4 C l but any boron carbide B n C, in which n is between 4 and 10. It is also according to an advantageous characteristic of the invention that it will be possible to choose to enrich or deplete in B 10 the boron of the solid boronizing agent and / or of the gaseous fluorinating agent of activation or starting gas. In this way, it will be possible to obtain parts with more or less high effective cross section for neutron shutdown by enriching with B 10 with high effective cross section or with B 11 very transparent to neutrons.
  • the solid boronizing agent and the parts to be boronized are subjected to the contact action of the stream of gaseous fluorinated agent outside mutual contact.
  • This embodiment is decisive for enabling the production of clean parts free of more or less sintered powder. This embodiment therefore operates in the gas phase, as will be explained below, hence saving and ease of implementation.
  • the solid boriding agent present with the parts to be borided is interposed in the stream of the gaseous fluorinated agent upstream from the parts to be borided.
  • This embodiment will allow the parts to be borided to be placed directly in a treatment enclosure in order to expose them to the gaseous phase alone. treatment.
  • the solid boronizing agent and the parts to be boronized are out of mutual contact, it is however possible that the solid boronizing agent is arranged in the form of pulverulent solid material constituting treatment bed for the parts to be boronized, as it is known per se.
  • the invention also relates to the parts of carbon steels having undergone a boriding treatment on the surface to a thickness of about 20 to 200 ⁇ m covered with a single-phase layer of Fe 2 B crystals of acicular formation.
  • An installation according to the invention comprises a reactor 1 made of refractory steel.
  • a reactor 1 made of refractory steel.
  • the bottom enclosure 3 is intended to contain the parts to be boronized 6.
  • L the upper enclosure 2 is intended to contain a pulverulent mass of mineral oxides 7.
  • the reactor 1 is in an oven 8, the temperature of which is regulated, in a manner known per se, by means of a thermocouple 9.
  • a pipe 10, controlled by a valve 11 is inserted into the upper wall of the reactor 1, so as to open into the enclosure 2.
  • the enclosure 3 and the reactor 1 are closed, at the bottom, by porous parcels, respectively 12 and 13, the porous wall 13 being closed, on its other face, by a pipe 14 for discharging gaseous effluents.
  • the valve 11 is connected, for the supply of gas, to two gaseous sources, respectively a source 15 of compressed boron trifluoride and a source 16 of diluent inert gas, such as argon or nitrogen. These two sources 15 and 16 are connected to the valve 11 through two flow meters 17 and 18 discharging on a pipe com mune 19.
  • the pipe 14 arrives on a valve 20 connected to a pressure gauge 21 and to a washer assembly 22 by a pipe 23.
  • a distribution valve 25 between a pipe d discharge 26 and a recycling pipe 27, which brings part of the gas effluent to valve 11, which is then a mixing valve.
  • the lower enclosure 3 In the embodiment of FIG. 1, provision has been made for the lower enclosure 3 to contain the boriding agent 5 in the form of a bed coating the parts, as is known per se. But according to the embodiment of Figure 2, the lower enclosure 3 does not contain any powdery or granular bed. In this case, the parts 6 and the solid boronizing agent are separated from each other, the agent is arranged in the form of sintered elements 30 suspended in the lower enclosure 3.
  • the preferred embodiment is that of Figures 3 and 4 which differs from the previous one, by the presence of a retaining grid 31 disposed in the upper part of the lower enclosure 3 for an interposed bed solid borating agent 33 in powder form with a particle size of 1 to 2 ⁇ m on the path of the gaseous activating agent supplied through the powdery mass of mineral oxides 7.
  • the embodiment of FIG. 3 is suitable for small parts which can be coated with powdered silicon carbide 34, as an inert agent.
  • FIG. 4 we simply omitted to place the bed of silicon carbide to deposit the part or parts 6 directly in the enclosure 3.
  • a boronizing agent of known type consisting of a powder of B 4 C at a particle size of 1 to 100 ⁇ m mixed with a powder of silicon carbide of 100 has been placed in enclosure 3. ⁇ m in mass proportion from 2/98 to 100/0.
  • enclosure 2 we put a pure silica sand washed with acids 90% of which passes through a 2 mm sieve.
  • the enclosure is scanned with a neutral gas, nitrogen or argon, at the same time as the temperature is raised.
  • the BF 3 gas possibly diluted, is sent when the temperature reaches approximately 500 to 950 ° C. The latter is chosen as the boronization temperature.
  • the duration of the passage of the activating gas varies from half to the entire time this stay of the parts at 950 ° C., said residence time having been approximately 5 hours. Simultaneously, the temperature of the silica bed 7 was brought to about 850 ° C.
  • FIG. 1 the installation of FIG. 1 was modified as shown in FIGS. 2, 3 and 4.
  • Example 3 In the embodiment of FIG. 2, a piece of carbon steel 6 was placed in the presence, but without contact, of hot sintered pieces 30 made of ⁇ boron, B 4 C and B 10 C. We sent BF 3 through the sand bed 7 of enclosure 2 for 18 h while maintaining the temperature of enclosure 3 at 1000 ° C. FIG. 7 shows a micrographic section of the steel thus borided.
  • Example 4 In the embodiment of FIG. 3, two parts, one made of carbon steel, the other of chromium-nickel 18/10, were placed in the SiC bed of enclosure 3. BF 3 was surrounded by the sand bed 7 of enclosure 2 for 2.5 h while maintaining the temperature of enclosure 3 at 1020 ° C.
  • FIG. 8 shows a micrographic section of the carbon steel thus boronized and in FIG. 9 a section of the chrome-nickel steel thus boronized.
  • FIG. 10 shows a micrographic section of the external surface of the workpiece and in FIG. 11 a micrographic section of the surface of the notch with a saw.
  • FIG. 7 shows the appearance of the borated layer obtained in the case of the reactor of Example 3.
  • the progression of the dendrites is not perpendicular to the surface but has been disturbed by the presence of a phase which appears as perlite after cooling.
  • the boronization speed therefore has an important influence on the progression of the boronized layer in the matrix and the growth direction [001] is not absolute.
  • this part is boronised (FIGS. 10 and 11), not only on the two external faces (90 to 120 ⁇ m), but also on the internal faces defined by the saw cuts.
  • a micrograph of these internal faces shows a borated layer of variable thickness and of discontinuous acicular character which is explained by the only intervention of a gas phase.
  • the invention has made it possible to develop an original process making it possible to boron all steels up to tool steels with total reliability.
  • the previous processes led to poor quality parts on mild steels (formation of two layers FeB + Fe 2 B), the flexibility of the process of the invention combined with the use of an activation moderator (Si0 2 ) allows, including in industrial conditions, to produce parts of consistent and satisfactory quality.
  • Mechanical tests have shown that the behavior of the layers obtained on tool steel was of very good quality.
  • boronization of stainless steel to chromium-nickel 18.10 remains of weak effect.
  • durations, percentages and particle sizes given in the previous description are not limiting. They can be varied as a function of the desired greater or lesser speed of formation and thickness of the layer. Some of these factors have only a slight influence, such as, for example, the particle size of B 4 C and of SiC.
  • boron carbides other than B 4 C such as borides B n C, in which n is between 4 and 10.
  • the main phase detected by X-ray diffraction is CoB; the mixed boride W 2 CoB 2 also seems to be present, on the other hand W 2 B 5 is absent.
  • W-Co mixed borides
  • FIG 12 there is shown a particularly simple embodiment of a reactor for implementing the method of the invention.
  • the lower part of the reactor constitutes the enclosure 3 closed by a watertight cover 40 with seal 41 cooled with water.
  • the enclosure 2 is produced in the form of a container which can be fitted into the reactor before fitting the cover 40.
  • the bottom of the enclosure 2 comprises the grid 4 for retaining the sand and letting the activation gas pass and a grid 31 for retain boron carbide, preferably powdery.
  • a pipe 10 fixed to the enclosure 2 crosses the cover to bring BF 3 through the sand of the enclosure2.
  • the cover is crossed by a central chimney 14 which also crosses, in a sealed manner, the enclosure 2 to end near the bottom of the reactor under a grid 12 for retaining the parts to be borided.
  • the temperature probe 9 can be placed in the chimney 14.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
EP80400252A 1979-02-27 1980-02-22 Verfahren zum Borieren metallischer oder metallkeramischer Gegenstände und mit einer borierten Oberfläche versehene Gegenstände Ceased EP0015813A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR7904991 1979-02-27
FR7904991A FR2450286A1 (fr) 1979-02-27 1979-02-27 Procede et dispositif de boruration de pieces en metal

Publications (1)

Publication Number Publication Date
EP0015813A1 true EP0015813A1 (de) 1980-09-17

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EP80400252A Ceased EP0015813A1 (de) 1979-02-27 1980-02-22 Verfahren zum Borieren metallischer oder metallkeramischer Gegenstände und mit einer borierten Oberfläche versehene Gegenstände

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US (3) US4289545A (de)
EP (1) EP0015813A1 (de)
ES (1) ES489003A0 (de)
FR (1) FR2450286A1 (de)

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US6478887B1 (en) * 1998-12-16 2002-11-12 Smith International, Inc. Boronized wear-resistant materials and methods thereof
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US20060074491A1 (en) * 2004-09-30 2006-04-06 Depuy Products, Inc. Boronized medical implants and process for producing the same
US7459105B2 (en) * 2005-05-10 2008-12-02 University Of Utah Research Foundation Nanostructured titanium monoboride monolithic material and associated methods
US20070078521A1 (en) * 2005-09-30 2007-04-05 Depuy Products, Inc. Aluminum oxide coated implants and components
US20110159210A1 (en) * 2007-03-14 2011-06-30 Hubert Patrovsky Metal halide reactor deposition method
US7955569B2 (en) * 2007-03-14 2011-06-07 Hubert Patrovsky Metal halide reactor for CVD and method
US20100176339A1 (en) * 2009-01-12 2010-07-15 Chandran K S Ravi Jewelry having titanium boride compounds and methods of making the same
US9068260B2 (en) 2012-03-14 2015-06-30 Andritz Iggesund Tools Inc. Knife for wood processing and methods for plating and surface treating a knife for wood processing
CN106637267A (zh) * 2015-10-28 2017-05-10 通用电气公司 用于从金属基材去除氧化物的方法和装置
WO2018169827A1 (en) 2017-03-14 2018-09-20 Bwt Llc Boronizing powder compositions for improved boride layer quality in oil country tubular goods and other metal articles
US10870912B2 (en) 2017-03-14 2020-12-22 Bwt Llc Method for using boronizing reaction gases as a protective atmosphere during boronizing, and reaction gas neutralizing treatment
KR102344996B1 (ko) * 2017-08-18 2021-12-30 삼성전자주식회사 전구체 공급 유닛, 기판 처리 장치 및 그를 이용한 반도체 소자의 제조방법
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FR1040863A (fr) * 1950-07-20 1953-10-19 Procédé d'ennoblissement et d'amélioration des surfaces métalliques, y compris du fer et de l'acier, au moyen d'un traitement de diffusion
US2844492A (en) * 1953-02-26 1958-07-22 Siemens Plania Werke Ag Fuer K Method of producing heat resisting metallic materials and formed bodies
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US4289545A (en) 1981-09-15
FR2450286A1 (fr) 1980-09-26
ES489003A0 (es) 1981-11-16
US4348980A (en) 1982-09-14
US4404045A (en) 1983-09-13
FR2450286B1 (de) 1982-09-03

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