CN1074489A - The method of nitriding nickel alloy - Google Patents

The method of nitriding nickel alloy Download PDF

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Publication number
CN1074489A
CN1074489A CN92102171A CN92102171A CN1074489A CN 1074489 A CN1074489 A CN 1074489A CN 92102171 A CN92102171 A CN 92102171A CN 92102171 A CN92102171 A CN 92102171A CN 1074489 A CN1074489 A CN 1074489A
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gas
nickelalloy
nitriding
nickel alloy
fluorine
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CN92102171A
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CN1032264C (en
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田原正昭
仙北谷春男
北野宪三
林田忠司
湊辉男
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Air Water Inc
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Daido Sanso Co Ltd
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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
    • 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
    • C23C8/34—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 more than one element being applied in more than one step

Abstract

A kind of method of nitriding nickel alloy, comprise following operation: make nickelalloy under heating condition, remain in the gas atmosphere of fluorine-containing or fluoride, the fluorizated nickelalloy is remained in the nitriding atmosphere under heating condition, and uniform nitride layer is to provide the nickelalloy with improved surface hardness by forming dark on nickel alloy surfaces.

Description

The method of nitriding nickel alloy
The present invention relates on nickel alloy surfaces, form the method for nitride layer with the nitriding nickel alloy of enhancement surface hardness and other performances.
Contain nickelic alloy such as having obtained widespread use with its good heat-resisting and corrosion resisting property because of Cornell nickelalloy (Ni-Cr), Hastelloy (Ni-Cr-Mo) and Incoloy.Recently constantly increase about wear resistance and other performances of improving nickel-containing alloys and the demand of expanding its range of application.But above-mentioned nickelalloy for example because of the nickelalloy of Cornell, is promoted the method for its surface hardness and established as yet so far, only studied and be extrapolation method for curing that improves body material intensity and the application of using the superplasticity goods of powdered material.Yet because the extrapolation hardening process improves whole hardness of alloy, so the processability of alloy just suffers damage.Use the superplasticity goods of powdered material because the cost costliness also is difficult to be put to practical application.
Subsidiary mentioning, the case hardening process of common metal material mainly contains: (1) electrochemical plating, (2) coating such as PVD, (3) diffusion process is as nitrogenize and boronation.But, for nickelalloy, have only some coating, for example pure hard chrome plating and be coated with aluminum oxide and just partly drop into practical application above-mentioned.Those methods particularly have difficulty concerning coating aspect quality control, and because coating is too thin range of application is restricted.In addition, the expensive of processing also is a problem.As case-hardened method of diffusion, also the plasma nitrided method by using glow discharge partly to carrying out overtesting because of Cornell nickelalloy and Hastelloy.But so plasma nitrided hardened nitride layer that is difficult on above-mentioned nickelalloy, form.Even form, also can be the superthin layer that part forms, its thickness has only several microns.So in the present circumstance, almost abandon the test of the above-mentioned nickelalloy of nitrogenize, be far from making it to forward practical application to.
Therefore, the purpose of this invention is to provide a kind of method that can on nickel alloy surfaces, form uniform thick nitride layer with the nitriding nickel alloy that improves its surface hardness.
According to the present invention, above-mentioned purpose can realize by the method that following nitriding nickel alloy is provided, and this method comprises nickelalloy is remained in the gas atmosphere of fluorine-containing or fluoride heating and will heat the upper layer formation nitride layer that makes nickelalloy with the nickelalloy that fluorine was handled in nitriding atmosphere.
Of the present invention to liking nickelalloy, after it is fluoridized, in nitriding atmosphere, carry out nitrogenize in the gas atmosphere of fluorine-containing or fluoride.
The main use nickeliferously is abbreviated as % below being higher than 25 weight %() nickelalloy, for example Ni-Cr, Ni-Cr-Mo and Ni-Cr-Fe are as the nickelalloy of the invention described above object.More particularly, they are to contain nickelic alloy, for example because of Cornell nickelalloy, Hastelloy and Incoloy.Nickeliferous 25% the nickelalloy of not being higher than also can be used as material of the present invention.So in the present invention, " nickelalloy " this term had both comprised and nickeliferously has been higher than 25% and also comprises nickeliferous 25% the alloy that is no more than.But, it is more suitable to contain the alloy of 25% above nickel.Method therefor had not both been stipulated the shape of nickelalloy, did not stipulate the degree of processing yet.Useful nickelalloy material, intermediate and the finished product made include in nickelalloy scope of the present invention.
The atmosphere that above-mentioned nickelalloy reacts therein be fluorine-containing or the fluoride gas atmosphere in gas fluorine-containing or fluoride be fluorine compound gas, such as NF 3, BF 3, CF 4, HF, SF 6, C 2F 6, WF 6, CHF 3Or SiF 4The use of can using individually or combine of these gases.In addition, can be used in the fluorine compound gas that contains F in its molecule and make above-mentioned fluorine-containing or fluoride gas.Can also use the F that in thermal decomposer, forms by the cracking fluorine compound gas 2Gas and previously prepared F 2Gas is as the gas of above-mentioned fluorine-containing or fluoride.According to circumstances, with such fluorine compound gas and F 2Gas mixes use.Gas such as the fluorine compound gas and the F of above-mentioned fluorine-containing or fluoride 2Gas can use independently, but generally all uses rare gas element such as N 2After being diluted, gas is used for handling.The concentration of the gas of fluorine-containing or fluoride itself for example should reach 10 in the gas of like this dilution, 000-100, and 000ppm better is 20,000-70,000ppm, and preferably 30,000-50,000ppm.
In the present invention, above-mentioned nickelalloy is fluoridized under heated condition in the gas atmosphere of the fluorine-containing or fluoride of such concentration.This is characteristic of the present invention.In this case, nickelalloy heating is remained on for example under the 350-500 ℃ of temperature.The hold-time of above-mentioned nickelalloy in the gas atmosphere of fluorine-containing or fluoride can be looked the geometrical shape of nickelalloy kind, alloy and size, Heating temperature or the like and suitably be selected, generally at more than ten minutes to dozens of minutes.Nickelalloy is handled in the gas atmosphere of so fluorine-containing or fluoride " N " atom is infiltrated in the nickelalloy, and this is impossible in the past.
Though the mechanism of infiltrating also is not verified now, can do following understanding substantially, promptly formed NiO zone of oxidation stops " N " atom of using for nitrogenize to infiltrate on nickel alloy surfaces.When the nickelalloy of band zone of oxidation being remained in the gas atmosphere of fluorine-containing or fluoride by above-mentioned heating, the NiO zone of oxidation just changes into and NiF 2Fluorinated layer." N " atom that is used for nitrogenize infiltrates NiF 2Fluorinated layer is more more or less freely than infiltrating the NiO zone of oxidation, that is to say that by above-mentioned fluoridation nickel alloy surfaces having been formed is suitable for the condition that " N " atom infiltrates.Therefore, can think that when nickelalloy remained in the nitriding atmosphere with the suitable condition of surface that absorbs " N " atom, " N " atom in the nitriding gas just penetrated into equably and reaches certain depth in the nickelalloy, the result forms dark and uniform nitride layer.
Then, as mentioned above, by having the nickelalloy of suitable condition of surface to remain on heating generation nitride in the nitriding atmosphere to absorbing " N " atom after the fluoridation.In the case, the nitriding gas of formation nitriding atmosphere is only by NH 3The pure gas of forming, or by NH 3With a kind of carbon source gas mixed gas of being formed of RX gas for example.Also can use the mixture of two kinds of gases.Usually use above-mentioned pure gas to mix with picture N 2Such rare gas element.According to circumstances, with H 2Gas is added in these gases.
In such nitriding atmosphere, make above-mentioned fluorizated nickelalloy keep heating, heating condition is set in 500-700 ℃ usually, and the treatment time is set in 3-6 hour scope.By this nitriding treatment, on above-mentioned nickel alloy surfaces, form dark and uniform fine and close nitride layer (forming) by complete simple layer, make nickel alloy surfaces hardness reach Hv=800～1100 whereby, by contrast the Hv=280 of body material～380.The thickness of hardened layer depends on nitriding temperature and time basically.But temperature surpasses 650 ℃ making nitride layer form the generation difficulty below 500 ℃ and work as temperature, and fluorinated layer is damaged, and nickel is easy to oxidation simultaneously, thereby causes forming inhomogeneous nitride layer.
On the other hand, fluoridize temperature and just can not generate a kind of enough fluorinated layers below 400 ℃ usually.The temperature that surpasses 600 ℃ in addition is unfavorable to production process, because the burner hearth material of retort furnace is owing to fierce fluoridation can be damaged.From forming the viewpoint of nitride layer, had better make the difference of fluoridizing between temperature and the nitriding temperature as much as possible little.For example, in case fluoridize and cool off after just carry out nitrogenize, just can not form suitable nitride layer.
Above-mentionedly fluoridize operation and the nitrogenize operation for example can be carried out in metal retort furnace as shown in Figure 1, promptly at first carry out fluoridation, within retort furnace, implement nitriding treatment then.In Fig. 1, reference number 1 is a retort furnace, the 2nd, and the shell of retort furnace, the 3rd, well heater, the 4th, inner vessels, the 5th, inlet pipe, the 6th, vapor pipe, the 7th, motor, the 8th, fan, the 11st, metal vessel, the 13rd, vacuum pump, the 14th, the toxic substance eliminator, 15 and 16 is gas cylinders, the 17th, under meter, the 18th, valve.Nikel alloy products 10 is placed in the stove 1, and the gas atmosphere by introducing fluorine-containing or fluoride is NF for example 3And fluoridation is carried out in heating.Effect by vacuum pump 13 is introduced gas in the vapor pipe 6, discharges behind the detoxification in toxic substance eliminator 14.Then, gas cylinder 15 is connected with conduit, nitriding gas is introduced carried out nitrogenize in the stove 1.After the nitrogenize, gas is discharged through vapor pipe 6 and toxic substance eliminator 14.Through this a series of operation, make to fluoridize and put into practice with nitrogenize.Also can use the device of the device replacement Fig. 1 among Fig. 2 in addition.This device is made up of the nitrogenize chamber of fluoridizing chamber and the right on the left side.In the figure, reference number 2 ' be metal vessel, 3 ' be well heater, 5 ' be vapor pipe, 6 ' and 7 ' for opening Yi Guangai, 11 ' be pedestal, 21 is the bodies of heater of being with diathermic wall, 22 is dividing plate moving up and down.Dividing plate 22 is divided into two cells 23 and 24 with the internal space of body of heater 21.Cell 23 designs are used as fluoridizes the chamber, and the 24th, as the nitrogenize chamber.Reference number 25 is the stands that comprise two tracks, and the metal vessel 2 of Nikel alloy products ' can slidably reciprocate in orbit is equipped with in inside between cell 23 and 24.Reference number 10 ' be the supporting of stand 25.Reference number 26 is gas introduction tubes, and it is introduced the gas of fluorine-containing or fluoride and fluoridizes chamber 23,27th, temperature sensor, the 28th, nitriding gas ingress pipe.As the material that meets the requirements of above-mentioned metal retort furnace 1 is high Refractoloy but not stainless material.
This device is a kind of continous processing system, and the heating of the internal temperature of wherein fluoridizing chamber 23 when carrying out nitrogenize in nitrogenize chamber 24 improves, and Nikel alloy products is fluoridized chamber 23 carrying out introducing under the fluorizated condition.After gas in the chamber 23 is fluoridized in discharge, Nikel alloy products is transplanted on nitrogenize chamber 24 together with metal vessel by opening and closing dividing plate 22.After this, under this condition, carry out nitrogenize, fluoridize continuously in this way and nitrogenize.
Select NF for use 3As the gas of fluorine-containing or fluoride for above-mentioned fluoridize especially suitable.That is to say NF 3Be a kind of gaseous substance easy to use, it is anergy at normal temperatures, is easy to operation and to the detoxification of vent gas.
Fig. 1 generally illustrates the structure of carrying out the processing stove of nitrogenize according to the present invention,
Fig. 2 generally illustrates the structure of another kind of stove,
Fig. 3 is the amplification sectional view of the nickelalloy plate (because of Cornell 600) of nitrogenize,
Fig. 4 is the amplification sectional view of the nickelalloy plate (because of Cornell 751) of nitrogenize,
Fig. 5 is the amplification sectional view of the nickelalloy plate (haas troy nickel-base alloy C) of nitrogenize.
Below the present invention is illustrated with implementing several modes of the present invention.
Example 1
To use because of Cornell 600 alloys (Ni76, Cr16, Fe8), (Ti2.5) and haas troy nickel-base alloy C(Ni56, Cr16, three kinds of nickelalloy sheet materials Mo7) making pack in as shown in Figure 1 the processing stove for Ni73, Cr16 because of Cornell 751 alloys.After carrying out vacuum purge in the stove, be heated to 550 ℃.Under this state, in stove, charge into the gas (NF of fluorine-containing or fluoride then 310 volume %+N 290 volume %), in stove, form barometric point and kept this operating mode 30 minutes.After the gas of above-mentioned fluorine-containing or fluoride discharged in the stove, feed nitriding gas (NH 350 volume %+N 225 volume %+H 225 volume %), with stove internal heating to 570 ℃.Under this operating mode, carry out 3 hours nitriding treatment.Through this nitrogenize operation, on using, just form a kind of cementation zone B of nitride layer respectively because of Cornell 600 alloys, three kinds of nickelalloy plate surfaces making because of Cornell 751 alloys and haas troy nickel-base alloy C, its thickness is respectively 15 microns, 12 microns and 10 microns, as Fig. 3, Fig. 4 and shown in Figure 5.In these figure, the body material of " A " expression nickel-base alloy.The surface hardness of these cementation zones B is Hv=800～1000 in all cases in addition.
Example 2
To pack in as shown in Figure 1 the processing stove with three kinds of nickelalloy sheet materials making because of Cornell 600 alloys, because of Cornell 751 alloys and haas troy nickel-base alloy C.After carrying out vacuum purge in the stove, be heated to 350 ℃.Under this operating mode, in stove, charge into the gas (NF of fluorine-containing or fluoride then 310 volume %+N 290 volume %), in stove, form barometric point and kept this operating mode 30 minutes.After then the gas of above-mentioned fluorine-containing or fluoride being discharged in the stove, feed nitriding gas (NH 350 volume %+RX50 volume %), and with stove internal heating to 530 ℃.Under this operating mode, carry out 5 hours nitriding treatment.Through this nitrogenize operation, just form a kind of cementation zone of nitride layer on using because of Cornell 600 alloys, three kinds of nickelalloy plate surfaces making because of Cornell 751 alloys and haas troy nickel-base alloy C respectively, its thickness is respectively 12 microns, 12 microns and 10 microns.The surface hardness of these cementation zones is Hv=650～1,050 in all cases.
Example 3
To using, similarly carry out fluoridation respectively as example 1 because of Cornell 600 alloys, because of three kinds of nickelalloy plates that Cornell 751 alloys and haas troy nickel-base alloy C make.In stove, feed NH then as nitriding gas 350 volume %+N 2The mixed gas that 50 volume % form meanwhile carries out 3 hours nitriding treatment under 620 ℃.After the nitrogenize, use with described in the embodiment 1 similarly gas fluorine-containing or fluoride under 620 ℃, they are carried out 3 hours fluoridation, use the nitrogenize 3 hours once more under 620 ℃ of above-mentioned nitriding gas then.Like this each of three kinds of nickelalloys is implemented twice and fluoridize and nitriding treatment, measure the thickness of the hardened layer of forming by nitride layer that on these surfaces, forms then.The result is respectively 25 microns, 20 microns and 18 microns because of Cornell 600 alloys, because of the thin hardened layer of Cornell 751 alloys and haas troy nickel-base alloy C.The surface hardness of finding them is identical with example 1.
Example 4
Use is by F 210 volume %+N 2The mixed gas that 90 volume % form is as the gas of fluorine-containing or fluoride.Except that this difference, three kinds of nickelalloy plates are carried out and example 1 identical fluoridizing and nitriding treatment.As a result, after the processing, on three kinds of nickelalloy plate surfaces, formed the hard nitride layer identical with example 1, and also identical with example 1 of surface hardness.
As indicated above, the method of nitriding nickel alloy of the present invention comprises makes nickelalloy remain in the gas atmosphere of fluorine-containing or fluoride and heating, thereby remove attached to the organic and inorganic pollutant on the nickelalloy, make the zone of oxidation on the nickel alloy surfaces be converted into fluorinated layer simultaneously, make alloy stand nitriding treatment afterwards.Because the zone of oxidation on the nickel alloy surfaces is converted into fluorinated layer in this mode, the existence of fluorinated layer just makes nickel alloy surfaces be protected.Therefore, even from fluoridizing behind nitrogenize experience certain hour, above-mentioned fluorinated layer still can play the effect of protection nickel alloy surfaces.The result can not form zone of oxidation again on nickel alloy surfaces.Because this fluorinated layer can transmit " N " atom, " N " atom just can infiltrate in the nickel alloy surfaces layer of certain depth equably during nitrogenize.The uniform infiltration that the result forms can cause only forming fine and close nitride layer uniformly in the degree of depth of nickel alloy surfaces layer, and improves surface hardness significantly and do not improve the rigidity of nickelalloy matrix material.

Claims (5)

1, a kind of method of nitriding nickel alloy comprises following operation: nickelalloy is remained in the gas atmosphere of fluorine-containing or fluoride heat, the fluorizated nickelalloy is remained in the nitriding atmosphere heat, thereby form nitride layer in the nickel alloy surfaces layer.
2, at least a by following listed (a) and (b) or (c) of the method for nitriding nickel alloy according to claim 1, the gas in the gas atmosphere of wherein fluorine-containing or fluoride and form for the rare gas element of dilution usefulness,
(a) contain and be selected from NF 3, BF 3, CF 4, HF, SF 6, C 2F 6, WF 6, CHF 3And SiF 4In the fluorine compound gas of at least a component,
(b) by the formed F of the above-mentioned fluorine compound gas of cracking (a) 2Gas,
(c) previously prepared F 2Gas.
3, the method for nitriding nickel alloy according to claim 1, wherein nickelalloy maintenance in the gas atmosphere of fluorine-containing or fluoride under heating condition is carried out under 350 ℃ to 600 ℃ temperature.
4, the method for nitriding nickel alloy according to claim 1, wherein the gas of nitriding atmosphere only is by NH 3The pure gas of forming; By NH 3Mixed gas with the RX gas composition; With rare gas element and above-mentioned single NH 3Gas or and NH 3Mix the formed gas that is mixed with rare gas element with the mixed gas of RX gas; Or with H 2Gas mixes with the gas that is mixed with rare gas element and a kind of mixed gas of forming.
5, the method for nitriding nickel alloy according to claim 1, wherein nickelalloy maintenance in nitriding atmosphere under heating condition is carried out under 500 ℃ to 700 ℃ temperature.
CN92102171A 1992-01-14 1992-03-30 Method of nitriding nickel alloy Expired - Lifetime CN1032264C (en)

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JP4024763A JP2501062B2 (en) 1992-01-14 1992-01-14 Nitriding method of nickel alloy

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US8377234B2 (en) 2010-04-26 2013-02-19 King Fahd University Of Petroleum And Minerals Method of nitriding nickel-chromium-based superalloys
CN106884134A (en) * 2015-12-16 2017-06-23 中国科学院上海应用物理研究所 A kind of surface passivation treatment method of nickel-base alloy

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CN102330062A (en) * 2011-10-18 2012-01-25 沈阳大学 Preparation method of titanium/nickel nitride nano multilayer film
CN102330062B (en) * 2011-10-18 2013-01-02 沈阳大学 Preparation method of titanium/nickel nitride nano multilayer film
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CN106884134B (en) * 2015-12-16 2020-07-03 中国科学院上海应用物理研究所 Surface passivation treatment method of nickel-based alloy

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JP2501062B2 (en) 1996-05-29
KR930016559A (en) 1993-08-26
EP0551702A1 (en) 1993-07-21
TW198070B (en) 1993-01-11
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DE69225880T2 (en) 1998-12-17

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