CN106868500A - A kind of surface alloying coating, preparation method and mould electron beam alloyage method - Google Patents
A kind of surface alloying coating, preparation method and mould electron beam alloyage method Download PDFInfo
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- CN106868500A CN106868500A CN201710120483.2A CN201710120483A CN106868500A CN 106868500 A CN106868500 A CN 106868500A CN 201710120483 A CN201710120483 A CN 201710120483A CN 106868500 A CN106868500 A CN 106868500A
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Abstract
The invention discloses a kind of surface alloying coating, preparation method and mould electron beam alloyage method.The surface alloying coating includes the raw material of following mass parts：SiO220 ~ 30 parts, 20 ~ 25 parts of SiC, 20 ~ 25 parts of Nb, 20 ~ 25 parts of W, 20 25 parts of Hf, 20 ~ 25 parts of Al, 20 ~ 25 parts of Si, 20 ~ 25 parts of Be, 15 ~ 25 parts of bentonite, 6 ~ 10 parts of shellac, 300 ~ 400 parts of absolute ethyl alcohol.Can be prevented effectively from stomata, be mingled with, the generation of the defect such as crackle.Its preparation method is by SiO2, SiC, Nb, W, Hf, Al, Si, Be and bentonite be crushed to granularity respectively less than 3 microns, then it is well mixed and obtains alloy powder, by the shellac ethanol solution of a part of absolute ethyl alcohol melt into shellac, finally alloy powder, the ethanol solution of shellac and another part absolute ethyl alcohol mixer are stirred.Mould electron beam alloyage method is that mould is placed in into certain hour in above-mentioned electron beam alloy coating, then carries out beam bombardment treatment to the surface of mould with pulsed electron beam device in gas atmosphere is protected.
Description
Technical field
The invention belongs to material surface treatment and reinforcement technique field, and in particular to a kind of surface alloying coating, preparation method
With mould electron beam alloyage method.
Background technology
Hot-work die bears varying stress and impulsive force at high temperature, and Workpiece shaping temperature often more than 1000 DEG C, will also
Undergo high-temperature oxydation, scaling loss and undergo the cold and hot thermal shock effect for changing and causing under the conditions of strong water-cooled.Needed when under arms
The effect that high stress, thermal shock, defibrator process undermine the load such as corrosion is born, therefore die life is very low.To improve the life-span, adopt at present
Main method is surface peening.Conventional method has quenching, carburizing, nitriding etc., but the effect of these methods is very limited, because
For hot-work die is operated in hot environment, traditional quenching enters annealed condition again in high temperature environments.In addition, for carburizing
For this technique, penetrating into excessive carbon can reduce the toughness of hot-work die.
Using the method for electron beam alloyage, can be formed on the surface of hot die steel has good metallurgical junction with matrix
The alloying layer of conjunction, and wear-resisting, high temperature resistant, impact-resistant hot forged mould alloying layer are obtained under suitable parameter, make hot forging
The life-span of mould greatly improves.
Although the model of hot die steel, composition are more on the market, for the alloy powder of mould electron beam alloyage
It is few.Its reason is the particularity of electron beam alloyage, especially needs to consider the reasonable of its High-temperature-resandant andant wear-resistant and matrix
Transition and it is suitable for electron beam alloyage characteristic requirements etc., conventional alloying component proportioning is used in electron beam alloyage or has
Stomata, be mingled with, the defect such as crackle, or performance can not meet requirement.
The content of the invention
For deficiencies of the prior art, the present invention provides a kind of surface alloying coating, to solve existing alloy
Composition have stomata, be mingled with, the technical problem of the defect such as crackle, and correspondence provides its preparation method, while provide utilizing the electronics
Beam alloy coating carries out mould electron beam alloyage method, and the hot-work die being surface-treated with solving prior art uses the longevity
The short problem of life.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of surface alloying coating, including following mass parts raw material：SiO220 ~ 30 parts, 20 ~ 25 parts of SiC, 20 ~ 25 parts of Nb,
20 ~ 25 parts of W, Hf 20-25 parts, 20 ~ 25 parts of Al, 20 ~ 25 parts of Si, 20 ~ 25 parts of Be, 15 ~ 25 parts of bentonite, shellac 6 ~
10 parts, 300 ~ 400 parts of absolute ethyl alcohol.
SiO2Effect in coating：Auxiliary rheological agents, because the solvent volatilization of coating edge is very fast, are led in work progress
Cause surface tension uneven, coating is moved to edge, and network of silica can effectively prevent the movement of coating
And webbing is formed, while also preventing coating sagging phenomenon in the curing process, make coating uniform.2nd, anti-settling agent, SiO2It is one
Kind preferable anti-settling agent, for preventing the precipitation of pigment in coating system highly effective, especially for the system of mill base, suitably
Addition will greatly improve the stability of mill base, and the amount of wetting dispersing agent can be reduced, to improve the applicability of mill base,
And reduce influence of the mill base to coating system, SiO2Anti-settling effect highly beneficial, particularly some pigment are deposited to coating,
Such as metal powder, all easily precipitate and can not suspend completely, use SiO2Can ensure that its dispersion is not precipitated.3rd, auxiliary agent is dispersed in powder
In last coating system, due to SiO2Small particle and high surface energy, they can be adsorbed on the surface of fine paint powders, and in powder
Surface forms a top layer, improves powder and obtains dispersed, therefore can use in same coating system as dispersant, adds
SiO2Jitter time can substantially be shortened, improve production efficiency is mono- it is noted that first by SiO2Complete effect is disperseed more preferably may be used
It is used together with other rheology main frame auxiliary agents of arranging in pairs or groups simultaneously, and SiO is adjusted using alcohols solvent2Rheological property.4、SiO2May be used also
To improve weather resisteant, the resistance to marring of coating, the bond strength between coating and base material is improved.
SiC is ceramic phase, improves coating hardness.The species of ceramic phase, content and matched with metal wetability, be all base
Drawn in many experiments.
Nb, W, Hf, Al, Si, Be are prepared into alloy powder together, collectively form high-entropy alloy.High-entropy alloy has：Heating power
" cocktail " in the distortion of lattice effect on entropic effect high, structures, sluggish diffusion effect kinetically, performance on
Effect.Using these characteristics, and binding isotherm calculates the high-entropy alloy designed with many experiments with SiC with preferably compatible
Property, after electron beam irradiation, coating structure can be refined, strengthen toughness, the alloy-layer of formation is without empty crackle, alloy-layer and matrix
Metallurgical binding, bond strength is high.With SiC collective effects, can improve high temperature abrasion resistance, impact resistance, hot-cracking resistance, so as to improve
Die life.
Wherein, described SiO2, SiC, Nb, W, Hf, Al, Si, Be and bentonitic powder and the granularity of being it is micro- less than 3
Rice.
A kind of preparation method of above-mentioned surface alloying coating, comprises the following steps：
1）By SiO2, SiC, Nb, W, Hf, Al, Si, Be and bentonite be crushed to granularity respectively less than 3 microns, then mix equal
It is even, alloy powder is obtained, it is standby.Micron powder can farthest avoid existing alloying component stomata, be mingled with,
The generation of the defects such as crackle.
2）By a part of anhydrous alcohol solution of shellac, the ethanol solution of shellac is obtained, it is standby.Shellac can provide coating
Caking property, but to form uniform coating, because commercially available shellac is solid, it is necessary to be first made solution and just advantageously form
The coating of suspended liquid status, and why make solvent using absolute ethyl alcohol, then it is the solubility due to shellac in absolute ethyl alcohol
It is higher, while absolute ethyl alcohol is easy to volatilize and substantially harmless to human body.
3）Alloy powder, the ethanol solution of shellac and another part absolute ethyl alcohol are stirred with mixer, that is, is obtained
Surface alloying coating.
A kind of mould electron beam alloyage method, the method is that mould is placed in into certain hour in above-mentioned surface alloying coating,
Mould is then taken out, and beam bombardment treatment is carried out to the surface of mould with pulsed electron beam device in gas atmosphere is protected,
Die surface is formed alloying coating, that is, complete the electron beam alloyage of die surface.Specifically include following steps：
（1）Mould is first heated to 70 ~ 110 DEG C, then the mould is immersed in 1 ~ 3s in surface alloying coating, then take out the mould
Stand to constant weight, obtain to surface and be bonded with the mould of powder bed.Due to mould be heated, in electron beam alloy coating the time compared with
It is short, still keep hot during taking-up, therefore under heat effect, the absolute ethyl alcohol of die surface can volatilize rapidly, and remaining composition is then
One layer of mixed-powder being firmly bonded can be formed on its surface, to facilitate lower step remelting.
（2）The mould that surface is bonded with powder bed is placed in vacuum less than 6 × 10-3 In the vacuum chamber of Pa, then pass to
Inert gas carries out beam bombardment treatment with pulsed electron beam device as protective gas to die surface, that is, complete mould
The electron beam alloyage on surface.
Wherein, the parameter of pulsed electron beam device is：Energy density 6-8J/cm2, pulse width 9-11 μ s, pulse number
200 ~ 300 times.
Fine and close, bond strength coating higher can be obtained after being processed through beam bombardment, the coating can improve mould
Service life.Such surface adds with hardness is high at high temperature, finish is good, coefficient of friction is low with little need for follow-up machine
Work, can directly go up production line and use.
Hardness is high at high temperature, finish is good, coefficient of friction is low, several on the surface processed using electron beam alloyage of the present invention
Need not subsequently machine, can directly go up production line and use.
Described mould is hot-work die；Described protective gas is argon gas, helium or nitrogen.
Compared with prior art, the present invention has the advantages that：
1st, the present invention so after ethanol volatilization, can form fine and close, light using raw material based on micron powder in die surface
Clean powder bed, it is to avoid the stomata of existing alloying component, be mingled with, the generation of the defect such as crackle.
2nd, electron beam alloy coating of the invention can complete to prepare at room temperature, and simple production process is easy.
3rd, at present, hot-work die working face in hot environment continuously using a period of time after steel bonding problem often occurs, make
With the present invention after steel cylinder ring mould face surface forms new alloy-layer, the problem of steel bonding is significantly improved.
4th, using electron beam surface alloying, its surface roughness disclosure satisfy that use requirement.Except electron beam surface is closed
This process program of aurification, also someone improve the service life of hot-work die by cladding Wear-resistant, high-temperature resistant powder, but its
Cladding layer is coarse, it is necessary to can just reach the standard grade and uses after being machined by car, mill etc., and hardness cladding layer very high, and machine adds
Work is very difficult, and operability is low.And the present invention is processed by hot biofilm, beam bombardment, its surface is more smooth, it is not necessary to machine
Processing be can be used, and substantially increase operability, and cost is substantially reduced.
5th, relatively low to the production efficiency of hot-work die working face electron beam alloyage, cost using the present invention, step is few, just
In promoting the use of.
6th, the present invention through production testing more than 1 year, it was demonstrated that the hot-work die red hardness after processed by the invention can be very
It is good, rank of the roughness close to smart car.Using effect shows, can improve die life to original more than 2.5 times.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment.
Embodiment one
The raw material for preparing surface alloying coating is calculated using following mass parts：SiO221 parts, 25 parts of SiC, 25 parts of Nb, W 20
Part, 20 parts of Hf, 25 parts of Al, 24 parts of Si, 21 parts of Be, 23 parts of bentonite, 10 parts of shellac, 380 parts of absolute ethyl alcohol.Wherein
SiO2, SiC, Nb, W, Hf, Al, Si, Be and bentonite be powdery, its granularity is below 3 microns.
The specific preparation process of electron beam alloy coating is：
1）By SiO2, SiC, Nb, W, Hf, Al, Si, Be and bentonite be crushed to granularity respectively less than 3 microns, then mix equal
It is even, alloy powder is obtained, it is standby.
2）By a part of anhydrous alcohol solution of shellac, the ethanol solution of shellac is obtained, it is standby.
3）Alloy powder, the ethanol solution of shellac and another part absolute ethyl alcohol are stirred with mixer, that is, is obtained
Surface alloying coating.
The electron beam alloyage for carrying out die surface using above-mentioned electron beam alloy coating is processed：
1）Hot-work die is worked into the size of needs.
2 add surface alloying coating in the container more than mould.
3）Hot-work die chamber type electric resistance furnace is heated to 110 DEG C, is put into after taking-up in the container equipped with surface alloying coating,
Allow coating to flood mould, after 1 second, mould is taken out from coating, under heat effect, the ethanol of die surface can volatilize rapidly, stay
The next layer of firm mixed-powder of bonding.
4）Use electron beam irradiation die surface：Sample is put on the station of vacuum chamber on fixture, is vacuumized, until
The vacuum P ＜ 6 × 10 of vacuum chamber-3Pa, then to being filled with inert gas in vacuum chamber as protective gas, such as argon gas, helium
Deng；Starting impulse electron beam equipment, loads high pressure（20-25kv）, the surface to mould carries out beam bombardment treatment.Pulse electricity
The main parameters ranges of beamlet surface treatment：Energy density 8J/cm2, the μ s of pulse width 9, pulse number 220 times；Open vacuum chamber,
Take out through the part of E.B surface treatment.
The present embodiment processed after alloying surface at 900 DEG C hardness average value be HRC33, do not carry out surface conjunction
Aurification treatment has and is obviously improved, and does not carry out the working face of the surface alloying treatment hardness average value at 900 DEG C and is
HRC17.Through production testing, the present embodiment can improve die life to original 2.8 times.
Embodiment two
The raw material for preparing surface alloying coating is calculated using following mass parts：SiO225 parts, 22 parts of SiC, 21 parts of Nb, W 24
Part, 24 parts of Hf, 21 parts of Al, 20 parts of Si, 24 parts of Be, 23 parts of bentonite, 10 parts of shellac, 380 parts of absolute ethyl alcohol.Wherein：
SiO2, SiC, Nb, W, Hf, Al, Si, Be and bentonite be powdery, its granularity is below 3 microns.
The specific preparation process of electron beam alloy coating is：
1）By SiO2, SiC, Nb, W, Hf, Al, Si, Be and bentonite be crushed to granularity respectively less than 3 microns, then mix equal
It is even, alloy powder is obtained, it is standby.
2）By a part of anhydrous alcohol solution of shellac, the ethanol solution of shellac is obtained, it is standby.
3）Alloy powder, the ethanol solution of shellac and another part absolute ethyl alcohol are stirred with mixer, that is, is obtained
Electron beam alloy coating.
The electron beam alloyage for carrying out die surface using above-mentioned electron beam alloy coating is processed：
1）Hot-work die is worked into the size of needs.
2 add surface alloying coating in the container more than mould.
3）Hot-work die chamber type electric resistance furnace is heated to 85 DEG C, is put into after taking-up in the container equipped with surface alloying coating,
Allow coating to flood mould, after 3 seconds, mould is taken out from coating, under heat effect, the ethanol of die surface can volatilize rapidly, stay
The next layer of firm mixed-powder of bonding.
4）Use electron beam irradiation die surface：Sample is put on the station of vacuum chamber on fixture, is vacuumized, until
The vacuum P ＜ 6 × 10 of vacuum chamber-3Pa, then to being filled with inert gas in vacuum chamber as protective gas, such as argon gas, helium
Deng；Starting impulse electron beam equipment, loads high pressure（20-25kv）, the surface to mould carries out beam bombardment treatment.Pulse electricity
The main parameters ranges of beamlet surface treatment：Energy density 8J/cm2, the μ s of pulse width 9, pulse number 220 times；Open vacuum chamber,
Take out through the part of E.B surface treatment.
The present embodiment processed after alloying surface at 900 DEG C hardness average value be HRC35, do not carry out surface conjunction
Aurification treatment has and is obviously improved, and does not carry out the working face of the surface alloying treatment hardness average value at 900 DEG C and is
HRC17.Through production testing, the present embodiment can improve die life to original 3.0 times.
The above embodiment of the present invention is only example to illustrate the invention, and is not to implementation of the invention
The restriction of mode.For those of ordinary skill in the field, other can also be made not on the basis of the above description
With the change and variation of form.Here all of implementation method cannot be exhaustive.It is every to belong to technical scheme
The obvious change amplified out changes row still in protection scope of the present invention.
Claims (7)
1. a kind of surface alloying coating, it is characterised in that the raw material including following mass parts：SiO220 ~ 30 parts, SiC 20 ~ 25
Part, 20 ~ 25 parts of Nb, 20 ~ 25 parts of W, Hf 20-25 parts, 20 ~ 25 parts of Al, 20 ~ 25 parts of Si, 20 ~ 25 parts of Be, bentonite 15
~ 25 parts, 6 ~ 10 parts of shellac, 300 ~ 400 parts of absolute ethyl alcohol.
2. the surface alloying coating according to right 1, it is characterised in that described SiO2, SiC, Nb, W, Hf, Al, Si, Be and swollen
The granularity for moistening soil is less than 3 microns.
3. a kind of preparation method of surface alloying coating as claimed in claim 1, it is characterised in that comprise the following steps：
1）By SiO2, SiC, Nb, W, Hf, Al, Si, Be and bentonite be crushed to granularity respectively less than 3 microns, then mix equal
It is even, alloy powder is obtained, it is standby；
2）By a part of anhydrous alcohol solution of shellac, the ethanol solution of shellac is obtained, it is standby；
3）Alloy powder, the ethanol solution of shellac and another part absolute ethyl alcohol are stirred with mixer, that is, obtains alloy
Change coating.
4. a kind of mould electron beam alloyage method, it is characterised in that be placed in mould one in the surface alloying coating of claim 1
Fix time, then take out mould, and carry out electron beam to the surface of mould with pulsed electron beam device in gas atmosphere is protected and bang
Treatment is hit, die surface is formed alloying coating, that is, complete the electron beam alloyage of die surface.
5. mould electron beam alloyage method according to claim 4, it is characterised in that comprise the following steps：
（1）Mould is first heated to 70 ~ 110 DEG C, then the mould is immersed in 1 ~ 3s in surface alloying coating, then take out the mould
Stand to constant weight, obtain to surface and be bonded with the mould of powder bed；
（2）The mould that surface is bonded with powder bed is placed in vacuum less than 6 × 10-3 In the vacuum chamber of Pa, inertia is then passed to
Gas carries out beam bombardment treatment with pulsed electron beam device as protective gas to die surface, that is, complete die surface
Electron beam alloyage；
Wherein, the parameter of pulsed electron beam device is：Energy density 6-8J/cm2, pulse width 9-11 μ s, pulse number 200-
300 times.
6. mould electron beam alloyage method according to claim 5, it is characterised in that described mould is Forming Die
Tool.
7. mould electron beam alloyage method according to claim 5, it is characterised in that described protective gas is argon
Gas, helium or nitrogen.
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| CN108641420A (en) * | 2018-05-14 | 2018-10-12 | 江苏久祥汽车电器集团有限公司 | A kind of method of surface of hot working die multicomponent alloy electron beam alloyage |
| CN108864779A (en) * | 2018-07-19 | 2018-11-23 | 江苏久祥汽车电器集团有限公司 | A kind of electron beam alloyage coating composition and its preparation, application method |
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| CN106868500B (en) | 2018-12-21 |
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