CN100398497C - Sintered part and the method for the production thereof - Google Patents

Sintered part and the method for the production thereof Download PDF

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Publication number
CN100398497C
CN100398497C CNB2004800137403A CN200480013740A CN100398497C CN 100398497 C CN100398497 C CN 100398497C CN B2004800137403 A CNB2004800137403 A CN B2004800137403A CN 200480013740 A CN200480013740 A CN 200480013740A CN 100398497 C CN100398497 C CN 100398497C
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China
Prior art keywords
sintered compact
sintering
gas phase
metal
plasma exciatiaon
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Expired - Fee Related
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CNB2004800137403A
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CN1842508A (en
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W·伦高尔
K·德赖尔
K·勒迪格
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Kennametal Widia GmbH and Co KG
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Kennametal Widia GmbH and Co KG
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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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/241—Chemical after-treatment on the surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention relates to a sintered part consisting of a hard metal, in particular WC with Co, Ni and/or Fe binders-based hard metal, or cermet, in particular on the base of composition consisting of (Ti, W) (C, N) or (Ti, Mo) (C, N) with Co, Ni and/or Fe binders and to a method for producing such a sintered part. The inventive method consists in exposing a sintered part totally or partially to an active plasma gaseous phase at a maximum pressure of 3x10<4> Pa during heating, sintering or after sintering, at least during a certain time preferably during a time period ranging from 10 to 100 min.

Description

Sintered compact and preparation method thereof
The present invention relates to a kind of by hard metal form, particularly by a kind of be the sintered compact that the hard metal of base is formed with the WC that contains Co, Ni and/or Fe binding agent, or the sintered compact of forming by sintering metal, particularly by a kind of (Ti that constitutes binding agent by Co, Ni and/or Fe that contains, W) (C, N) or (Ti, Mo) (C, N) sintering metal of Zu Chenging.
In addition, the invention still further relates to a kind of method for preparing this sintered compact.
The sintered compact of described kind can be used for machining as cutting insert especially to be handled.
Task of the present invention is to provide a kind of sintered compact with better cutting ability.The present invention also provides a kind of method for preparing such sintered compact in addition, and this method can make process period shorter and in dark as far as possible infiltration area tissue is exerted an influence.
This task can solve by sintered compact as claimed in claim 1 or by method as claimed in claim 6.
Further scheme record of the present invention in the dependent claims.
In principle, particularly the plasma diffusion treating processes of carrying out with nitrogenize nitriding or nitrated nitriding or nitro carburizing form is a kind of oneself method in order to modified improvement steel surface of a specified duration of using, and it is in order to improve the anti-heat sealability and the erosion resistance of steel.Recently, also have pair titanium alloy and stellite to carry out the method that diffusion of plasma is handled, change the tissue of this alloy body fringe region by seeping, method is to constitute a spreading area, perhaps one or more key coats.The material that is infiltrated can be such as nitrogen or carbon, and except the spacing that may change lattice, they can not change the crystallographic structure of substrate material.On this diffusion layer or nearly surf zone, can form single or multiple key coat, they for example constituted the element of substrate material and the material of infiltration are bondd another mutually.
Publication number is to disclose a kind of sintering metal in the literature summary of JP05302140A, its by hard mutually as TiCN and matrix metal such as Co and Ni forms and the nitrogen plasma atmosphere that will place a gas phase, plasma body wherein passes through high frequency or microwave discharge generation.Here, can form the thick nitride region of 10 to 500 μ m, in this zone, contain the TiN particle of uniform distribution and light≤0.1 μ m.In contrast, in sintered compact of the present invention, contain other structural constituents that the gas phase by plasma exciatiaon forms at nearly surf zone, its size is the scale parameter magnitude of this structural constituent, and has the hard composition of hard metal and sintering metal composition in this structural constituent usually.Contained in the plasma body activated gas phase, to penetrate into the material that goes in the surface can be nitrogen, carbon, boron, the metal that can be provoked into to plasmoid.With pure different with the gas phase of thermal excitation, the sintered compact that carries out the gas phase treatment of excitation of plasma have one in addition in darker scope affected surf zone.The gas phase of excitation of plasma can also can realize purifying and/or reductive action at nearly surf zone according to the difference of the gas composition of plasma body, improves surfaceness and form brand-new structural constituent (phase) and arrange aspect planeness.According to the present invention, the composition of nearly Surface Edge battery limit (BL) also can improve the cohesiveness of the coating that is made of carbide, nitride, oxide compound, boride or carbon or these substance mixture that applies thereafter.The treating processes of plasma exciatiaon also can exert an influence mutually to binding agent, and for example the nitrogen of plasma exciatiaon can cause forming cobalt-nickel-or the nitride of iron, and utilizes the nitrogen of thermal excitation can't realize this point.
Preferred sintered compact of the present invention has wherein because migration and/or diffusion contain the material of the gas phase that comes from plasma exciatiaon or the fringe region of the compound of formation thus.The degree of depth of affected borderline region can by select processing parameter temperature, pressure and treatment time and for example the inhomogeneity of structure of this borderline region be controlled in the scope that is no more than 1200 μ m.
Especially, owing to the gas phase of plasma exciatiaon, in borderline region, also contain the nitride particles of particle diameter 〉=0.2 μ m in addition.
For preparing this sintered compact, adopt a kind of method, powder metallurgy ground hard metal of pre-treatment or sintering metal and be pressed into base substrate wherein, then in being heated to the sintering temperature process, during the sintering or after carrying out last sintering, at least will be by the timed interval, preferably through time period of at least 10 minutes to 100 minutes and be maximum 3 * 10 4The pressure of Pa is complete down or just these base substrates are in the gas phase of plasma exciatiaon.Plasma exciatiaon can generate electricity by microwave discharge or by aura and carry out, and wherein preferably utilizes impulse method to produce glow discharge again, is communicated with sintered compact in this method and is used as the negative electrode use, applies a pulsed dc voltage on negative electrode.Preferred volts DS is between 200 to 900V.In interpulse period, volts DS drops to 0V or remnant DC voltage, and wherein said remnant DC voltage is equal to or greater than the minimum ionization potential value that participates in gas, but is pulsed dc voltage peaked 50% to the maximum.If keep remnant DC voltage constant in interpulse period, then its ratio with the maximum impulse dc voltage value should be 0.02 to 0.5.The cycle of pulsed dc voltage is between the 20 μ s to 20ms.The ratio of pulse intermittent phase is 0.1 to 0.6 during pulse width.
Aforesaid, but the mixture of metal, compound or the aforementioned substances of nitrogen, carbon, boron or plasma exciatiaon in the gas phase of plasma exciatiaon, should be contained, or precursor.
According to an improvement project of the inventive method, be before feeding reactant gas or reactive gas mixture, the object that will handle places inert atmosphere, particularly by rare gas and/or chemical reducing agent, is preferably the inert atmosphere that hydrogen is formed.Reactive materials non-chemically, for example argon is used for the clean surface, feeds the gas phase of plasma exciatiaon then in the other method step, by migration and diffusion process targetedly and molten loosing in nearly upper layer.Contained hydrogen is used for the reduction process on the excitating surface in the gas phase, especially for the decomposing oxidation settling.
For in the gas phase of plasma exciatiaon, handling sintered compact, preferably temperature is chosen in and is higher than 900 ℃ to 1350 ℃.
Below will set forth some other advantage of the present invention according to embodiment that is inquired into and accompanying drawing.Accompanying drawing is:
Fig. 1 to 4 is respectively the microscope figure of sintered compact, wherein will be subjected to the sintered compact of the gas phase treatment of plasma exciatiaon (to be respectively a) and to do contrast with simultaneous test sample (being respectively b).
Embodiment 1:
At first, under 1350 ℃ hypereutectic temperature and under 300mbar pressure in nitrogen atmosphere, handle two WC-Ti (C, N)-the Co type, through agglomerating and hard metal (being W, 25.5 quality %Ti, 9 quality %Ta, 0.5 quality %Nb, 7 quality %C, 3 quality %N and the 15 quality %Co of 40 quality %) 20 minutes with identical chemical constitution, wherein, first hard metal is loaded plasma body, then needn't load second.In these two samples, can form so-called gradient layer, the carbonitride of enrichment titanium in this layer and the WC composition of sample inside is fallen in displacement simultaneously.But, can find out by the contrast of Fig. 1 a and Fig. 1 b, load the sample of nitrogen plasma (Fig. 1 a) in, be subjected to zone that nitrogen influences obviously greater than heating just and the same area of the sample that non-plasma activated gas phase is handled.
Embodiment 2:
(C N)-side and the top nitrogen plasma treatment that stands of Co-hard metal, does not then carry out this Cement Composite Treated by Plasma below it to make agglomerating WC-Ti under the pressure of 1350 ℃ temperature and 300mbar.Described hard metal consist of 60.5 quality %W, 16 quality %Ti, 5 quality %Ta, 0.3 quality %Nb, 7 quality %C and 1.2 quality %N and 10 quality %Co.From having shown above the hard metal Fig. 2 a of microscope figure as can be seen, formed the thick enrichment Ti (C of about 25 μ m, N) and not the layer that containing among the figure the bright WC particle that shows, the following microscope figure shown in Fig. 2 b then shows and is not subjected to any influence that just is subjected to nitrogen thermal excitation, infiltration in fact here simultaneously.
Embodiment 3:
Under 1250 ℃ hypereutectic temperature and at 150mbar N 2Condition under annealing (gl ü hen) two through agglomerating hard metal 60min, described hard metal consist of 40 quality %W, 25.5 quality %Ti, 9 quality %Ta, 0.5 quality %Nb, 7 quality %C, 3 quality %N and 15 quality %Co, wherein first hard metal is placed the nitrogen of plasma exciatiaon and makes second just to be subjected to just being subjected to the nitrogen of thermal excitation to handle in gas phase.Shown in Fig. 3 a, the metathesis of WC obviously is deep into until 1200 μ m in the sample of loading plasma body.Can see that in Fig. 3 a (C, enriched layer N) are deep to about 20 μ m to Ti.On the contrary, shown in Fig. 3 b, only the hard metal of warmed nitrogen atmosphere processing then demonstrates the edge effect district that only is deep to 5 μ m.
Embodiment 4:
Under 1250 ℃ hypereutectic temperature and at 150mbar N 2Condition under annealing two through agglomerating hard metal 60min, described hard metal consist of 60.5 quality %W, 16 quality %Ti, 5 quality %Ta, 0.3 quality %Nb, 7 quality %C and 1.2 quality %N and 10 quality %Co, wherein again first metallic object is annealed in the gas phase of plasma exciatiaon, and make second being to handle in the pure gas phase that is subjected to thermal excitation.The sample that loads plasma body has thickness to be the nitride layer of 50 μ m and to be positioned at the thick zone of containing less WC content of about 40 μ m under it (referring to Fig. 4 a), and in the metallic object that the nitrogen that just is subjected to thermal excitation is handled mutually, only have the thick nitride layer of 5 μ m and less than 5 μ m thick be positioned at zone under it.
Above embodiment shows, just can regulate the inhomogeneity of structure of being scheduled to and/or can produce a key coat by in the gas phase of plasma exciatiaon, sintered compact being handled, this key coat can improve the use properties of sintered compact, during as cutter life, durability and machining and miscellaneous part reactive little.Preferably produce the plasma exciatiaon effect by glow discharge, particularly will be by means of impulse method, it can avoid forming electric arc.In time period, needn't always keep plasma exciatiaon in entire treatment.Air pressure is remained in the scope that is no more than 300mbar, in this scope, can reach a kind of isoionic state, promptly can light and keep plasma body.Select treatment temp or its threshold value can realize further that the interior region of sintered compact is not subjected to tangible heat affecting yet, thereby the intravital structure of sintering is remained on original shape and just has influence on nearly surf zone.Hide the sintered compact surface or, do not have plasma body to invade or can not form so-called plasma limit there by part with regard to making with its reverse side placement or coating.In these positions, only need can influence contingent tissue modification, rather than can carry out at the plasma body that nearly Surface Edge battery limit (BL) obtains different tissue modification effects by it by some atmosphere and the processing parameter of being regulated.
If desired or requirement is arranged, also can before the treating processes in the gas phase of plasma exciatiaon, carry out an anneal process earlier, purify the surface with this.Another substitutes or additional scheme is also can carry out a treating processes of carrying out before the gas phase process of plasma exciatiaon in the gas phase of being made up of chemical reducing agent.
By the influence of plasma body, in the borderline region on nearly surface, can produce new phase, be impossible form if they do not have the excitation of plasma effect.Therefore, utilize method of the present invention both can obtain phase composite, also can obtain organizing affected darker infiltration district and by selecting processing parameter to regulate the ideal inhomogeneity of structure in the frontier district on nearly surface through changing.Than those comparable sintered compacies well known in the prior art, those also have much advantage with surface flatness or the roughness (latter is aspect the needed coating) that quadrat method obtains.

Claims (12)

1. the sintered compact of forming by hard metal, or the sintered compact of forming by sintering metal, it is characterized in that, in heat-processed, during the sintering or after carrying out last sintering, at least will be by through timed interval of at least 10 minutes to 100 minutes and be 1.5 * 10 4-3 * 10 4The pressure of Pa is complete down or just sintered compact is in the gas phase of plasma exciatiaon, wherein contain nitrogen, carbon, boron, metal, their compound or mixture or corresponding precursor in the gas phase that this plasma body excites, with in the borderline region on nearly surface, contain the material of the gas phase that comes from plasma exciatiaon or formed thus compound by migration and/or diffusion.
2. sintered compact as claimed in claim 1 is characterized in that, contains the nitride particles of particle diameter 〉=0.2 μ m at the nearly surf zone of sintered compact.
3. sintered compact as claimed in claim 1 or 2 is characterized in that, the gradient of organizing of sintered compact is to point to the inside of sintered compact from the surface.
4. sintered compact as claimed in claim 1, it is characterized in that, described hard metal be a kind of be the hard metal of base with the WC that contains Co, Ni and/or Fe binding agent, described sintering metal is a kind of containing by Co, Ni and/or Fe to constitute binding agent (Ti, W) (C, N) or (Ti, Mo) (C, N) sintering metal of Zu Chenging.
5. preparation is as the method for the described sintered compact that is made of hard metal or sintering metal of one of claim 1 to 4, it is characterized in that, in being heated to the sintering temperature process, during the sintering or after carrying out last sintering, at least will be by through timed interval of at least 10 minutes to 100 minutes and be 1.5 * 10 4-3 * 10 4The pressure of Pa descends fully or just partly makes through sintered compact pretreated with powder metallurgic method and that be pressed into base substrate to be in the gas phase of plasma exciatiaon.
6. method as claimed in claim 5 is characterized in that, during the sintering or after carrying out last sintering, fully or just sintered compact is in the gas phase of plasma exciatiaon under 900 ℃ to 1350 ℃ temperature.
7. method as claimed in claim 5 is characterized in that, produces plasma exciatiaon by microwave or by glow discharge.
8. method as claimed in claim 7 is characterized in that, utilizes impulse method to produce plasma exciatiaon by microwave or by glow discharge, is communicated with sintered compact and uses and apply pulsed dc voltage thereon as negative electrode in this impulse method.
9. as claim 5 or 6 described methods, it is characterized in that, contain nitrogen, carbon, boron, metal, their compound or mixture in the gas phase of plasma exciatiaon.
10. method as claimed in claim 5 is characterized in that, before input reactant gas or reactive gas mixture, gas phase is formed and/or contained chemical reducing agent by rare gas element.
11. method as claimed in claim 10 is characterized in that, described rare gas element is that rare gas and described chemical reducing agent are hydrogen.
12. method as claimed in claim 5 is characterized in that, hides the surface part of substrate body when handling in the gas phase of plasma exciatiaon.
CNB2004800137403A 2003-05-21 2004-04-29 Sintered part and the method for the production thereof Expired - Fee Related CN100398497C (en)

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CN101974713B (en) * 2010-10-25 2012-11-07 北京科技大学 Method for preparing gradient cemented carbide with beta removal layer
CN103357872A (en) * 2012-06-12 2013-10-23 北京京磁强磁材料有限公司 Sintering technology of NdFeB (neodymium iron boron) magnet
CN102825252B (en) * 2012-08-21 2015-07-29 沈阳化工大学 A kind of powder metallurgy manufactures the method for titanium base medical material
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CN103896635B (en) * 2014-03-07 2015-09-02 太原理工大学 The surface alloying process of powdered ceramic material
CN104174846B (en) * 2014-09-10 2017-02-01 太仓派欧技术咨询服务有限公司 Ceramic matrix composite niobium alloy skirt section 3D printing method
US20170067137A1 (en) * 2015-09-07 2017-03-09 Seiko Epson Corporation Titanium sintered body and ornament
JP6861235B2 (en) * 2019-04-04 2021-04-21 日本タングステン株式会社 A member for a plasma processing device and a plasma processing device including the member.

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WO2004108632A1 (en) 2004-12-16
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US20060280639A1 (en) 2006-12-14
DE10322871A1 (en) 2004-12-16
EP1625102A1 (en) 2006-02-15

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