CN106637062A - Method for preparing surface plasma nitrided layer of high-entropy alloy - Google Patents
Method for preparing surface plasma nitrided layer of high-entropy alloy Download PDFInfo
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- CN106637062A CN106637062A CN201610857904.5A CN201610857904A CN106637062A CN 106637062 A CN106637062 A CN 106637062A CN 201610857904 A CN201610857904 A CN 201610857904A CN 106637062 A CN106637062 A CN 106637062A
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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
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- Organic Chemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The invention provides a method for preparing a surface plasma nitrided layer of a high-entropy alloy. The method comprises the steps that a high-entropy alloy base material is cleaned, a part is dried in a plasma nitriding furnace; and after the inner pressure and the outer pressure of the plasma nitriding furnace are identical, the part is placed on a cathode disk, vacuumizing is conducted on a furnace body, high-purity ammonia gas is fed into the furnace body, the temperature is raised and then kept, feeding of the ammonia gas is cut off, vacuumizing continues to be conducted, and the surface plasma nitrided layer of the high-entropy alloy is obtained after furnace cooling. According to the method for preparing the surface plasma nitrided layer of the high-entropy alloy, the LDMC-100A type pulse plasma nitriding furnace and the double glow plasma nitriding technology are utilized to conduct nitriding on the surface of the high-entropy alloy for the first time; the method for preparing the surface plasma nitrided layer of the high-entropy alloy has the advantages that the plasma nitrided layer is thick, high in combination strength and hardness and resistant to wear and corrosion; besides, the method for preparing the surface plasma nitrided layer of the high-entropy alloy has the advantages that the nitriding speed is high, the nitrided layer has good performance, technological deformation is small, and gas consumption and electricity consumption are small; and the method for preparing the surface plasma nitrided layer of the high-entropy alloy is a non-pollution nuisance-free ideal technology, and the surface plasma nitrided layer of the high-entropy alloy can be widely applied to the working conditions having a high wear resistance requirement and a high corrosion-resistance requirement.
Description
Technical field
The present invention relates to a kind of method of high-entropy alloy surface ion nitriding layer, specifically a kind of high-entropy alloy surface
The preparation method of ion-nitriding layer.
Background technology
Glow discharge nitriding is the important component part of field of metal material surface treatment, it can give piece surface high rigidity,
Various specific functions such as wear-resisting, high temperature resistant, corrosion-resistant, anti-oxidant, antifatigue, radiation proof, are improve product quality, energy saving
With resource, a kind of surface reinforcing method of acquisition distinct economic, in many fields increasing extensively application is obtained.
High-entropy alloy is the luxuriant reason that equimolar ratio, the high entropy of mixing are based in last century the nineties of China's Taiwan's scholars leaf
A kind of novel alloy material of design is read, it has been broken and traditional is carried out alloyage this design reason based on a kind of metallic element
Read.Thus make high-entropy alloy that there are a series of excellent performances, such as high intensity, high rigidity, high-wear resistance, excellent anti-oxidant
Performance and corrosion resistance etc..
Used as novel alloy material, high-entropy alloy has many performances excellent compared with conventional alloys material, and application is got over
Come wider, therefore cause the great attention of increasing engineers and technicians.In many fields, in order to further explore and
Improve the surface property of conventional alloys material, many scholars with high entropy alloy material by developing kinds of processes technology to it
Surface property is studied, for example high-entropy alloy coating.But these methods come with some shortcomings to some extent, have impact on them
Range of application.Therefore, how to improve the surface property of high-entropy alloy, prepare high rigidity modified layer, improving its anti-wear performance is
One of focus of Chinese scholars concern and research.
Up to the present, for the research of high-entropy alloy, China Taiwan is in the leading level in the world, particularly Taiwan
Tsing-Hua University and the Industrial Technology Research Institute of Taiwan.That high-entropy alloy is studied earliest on ground in China is the Jiang Qing professors of Jilin University, what he studied
Problem is mainly lightweight high-entropy alloy.
At present existing technology prepares high-entropy alloy using technologies such as magnetron sputtering deposition, electrochemical deposition and laser melting coatings
Coating and to high-entropy alloy surface coating, but the coating and plated film that are obtained using these methods are all very thin, and and base
The adhesion of body is not strong, easily comes off, it is difficult to play the advantage of high-entropy alloy aspect of performance.
In existing technology, some alloys are also adopted by plasma nitriding, ion implanting, PCVD/CVD technologies in alloy table
Face prepares modified layer, significantly improves hardness, wearability and the corrosion resistance of matrix, but strengthening layer than relatively thin, Performance comparision
Single, workpiece is susceptible to deformation, and to the application of correlation technique many restrictions are brought.
It is, with other alloys as base material, by preparing high-entropy alloy coating and coating base to be improved based on prior art
The performance of material.In order to expand the application of high-entropy alloy, inventor develops with high-entropy alloy as base material to obtain table
The preparation method of face nitriding layer.Therefore, the present invention utilizes LDMC-100A type pulse ion nitriding furnaces, double brightness plasma nitridations
Technology in high-entropy alloy surface carburization, prepares the high-entropy alloy with surface ion nitriding layer so that high-entropy alloy can first
To be used widely in increasing field.
The content of the invention
The invention solves the problems that concrete technical problems be that invention has that infiltration layer is thick, bond strength is high, hardness is high, and extensively
The high-entropy alloy surface carburization layer being applied under the working condition that anti-wear performance and decay resistance have high demands, it is therefore an objective to provide one
Plant the method for preparing high-entropy alloy surface ion nitriding layer.
The technical scheme taken to solve above-mentioned technical problem is as follows.
A kind of method for preparing high-entropy alloy surface ion nitriding layer, the composition of the high-entropy alloy base material that methods described is adopted
For Al1.3CoCuFeNi2, configure according to mol ratio, wherein, subscript represents the molar fraction shared by the composition, does not mark lower target
I.e. mol ratio is 1；Or
The composition of the high-entropy alloy base material is AlCoCrFeNi, according to equimolar than configuring；Or
Al, Co, Cu, Fe, Ni and Cr raw materials for metallurgy mass concentration that the high entropy alloy material is adopted is not less than 99.9 %；
The method for preparing high-entropy alloy surface ion nitriding layer is as follows：
（1）Alloy smelting raw material A l, Co of employing, Cu, Fe, Ni and Cr element are carried out into accurate weighing proportioning simultaneously according to mol ratio
Purification oxidation on metal surface thing；
In the groove that the raw material for preparing is placed in the water cooled copper mould melting pond of WK type vacuum arc furnace ignitions ,-applying argon gas, melting are vacuumized
At 250 amperes, the time is the 30-60 seconds to electric current, after alloy is sufficiently mixed, alloy block is overturn, after alloy pig is put into water-cooled
In the groove of copper mold, melting electric current is adjusted, after alloy melting is uniform, opens and inhale casting inlet valve, using vacuum in pump suction casting is carried out,
Take out after alloy mold cooling, that is, obtain the high-entropy alloy base material；
（2）High-entropy alloy base material after polishing, polishing is cleaned by supersonic wave cleaning machine, then by ion nitriding furnace zero
Part is dried, vacuum in purifying furnace；
（3）Manual air-release valves are opened, into stove air is filled with, after stove external and internal pressure is consistent, furnace tube is sling, part is placed in
The enterprising luggage stove of cathode disc, closes afterwards Manual air-release valves sealing；
（4）Furnace tube is covered, is switched on power, 5 Pa are evacuated to body of heater, high purity ammonia gas, gas are passed through into ion nitriding furnace
Pressure is maintained at 500 Pa, slowly rises high voltage, and temperature rises to 550 DEG C, is incubated 9 h, is then shut off ammonia, continues to vacuumize, with
Stove is cooled down, and when workpiece temperature is down to room temperature, closes cooling water, opens body of heater, takes out sample.
Further it is technically characterized in that：The purity that high purity ammonia gas are passed through into ion nitriding furnace be 99.99 %,
The flow velocity for being passed through high purity ammonia gas is 0.4 m3/h；The ion nitriding furnace is existed using LDMC-100A type pulse ion nitriding furnaces
High-entropy alloy surface carburization.
Above-mentioned a kind of the provided method for preparing high-entropy alloy surface ion nitriding layer of the present invention is realized, with prior art
Compare, its advantage is with good effect：The high-entropy alloy surface ion nitriding layer being prepared by the method for the present invention has infiltration layer
Thick, bond strength is high, high, the wear-resistant and corrosion resistant advantage of hardness, and the preparation method possesses, and infiltration rate is fast, penetrated layer property
The features such as good, little process distortions and gas consumption, little power consumption, be pollution-free, non-harmful ideal technology, be can be widely applied to wear-resisting
Damage the working condition having high demands with decay resistance.
Description of the drawings
Fig. 1 is the preparation technology flow chart of high-entropy alloy surface ion nitriding layer of the present invention.
Fig. 2 is the surface scan picture of high-entropy alloy surface ion nitriding layer sample 1 of the present invention.
Fig. 3 is the surface scan picture of high-entropy alloy surface ion nitriding layer sample 2 of the present invention.
Fig. 4 is the profile scanning picture of high-entropy alloy surface ion nitriding layer sample 1 of the present invention.
Fig. 5 is the profile scanning picture of high-entropy alloy surface ion nitriding layer sample 2 of the present invention.
Fig. 6 is coefficient of friction of the high-entropy alloy surface ion nitriding layer sample 1 of the present invention in varying environment under 3 N load
Curve map.
Fig. 7 is coefficient of friction of the high-entropy alloy surface ion nitriding layer sample 2 of the present invention in varying environment under 3 N load
Curve map.
Fig. 8 is the mill after high-entropy alloy surface ion nitriding layer sample 1 of the present invention weares and teares in varying environment under 3 N load
Trace cross section profile figure.
Fig. 9 is the mill after high-entropy alloy surface ion nitriding layer sample 2 of the present invention weares and teares in varying environment under 3 N load
Trace cross section profile figure.
Figure 10 is the nitriding layer cross section component distributing curve map of high-entropy alloy surface ion nitriding layer sample of the present invention 1.
Figure 11 is the nitriding layer cross section component distributing curve map of high-entropy alloy surface ion nitriding layer sample of the present invention 2.
Figure 12 is the key property table of high-entropy alloy surface ion nitriding layer sample 1 of the present invention.
Figure 13 is the key property table of high-entropy alloy surface ion nitriding layer sample 2 of the present invention.
Specific embodiment
The specific embodiment of the present invention is further illustrated below.
Embodiment 1
One kind prepares high-entropy alloy Al1.3CoCuFeNi2The method of surface ion nitriding layer, the method is comprised the following steps that：
The preparation of sample
（1）Processing Al1.3CoCuFeNi2Sample.Adopt wire cutting machine processing dimension for 10 mm × 10 mm × 1.5 mm sample
Product.
（2）Cleaning Al1.3CoCuFeNi2Specimen surface.It is different with 2500# with 300#, 800#, 1000#, 1500# successively
The SiC sand paper grinding alloy sample of granularity, is then mechanically polished to 100 times with the diamond polishing cream that granularity is 0.5 μm
Light microscope lower surface no marking.It is last cleaned with supersonic wave cleaning machine in alcohol dry up it is stand-by.
Double brightness plasma nitridations
（1）Shove charge：Manual air-release valves are opened, toward in stove air is filled with, furnace tube is sling after stove external and internal pressure is consistent, by zero
Part is placed in the enterprising luggage stove of cathode disc.After shove charge is finished, Manual air-release valves are closed, make ion nitriding furnace be in good sealing
State.
（2）Vacuumize：Furnace tube is covered, power supply is connected, " master control " switch is opened, " vavuum pump is pressedOpen " button
" vavuum pumpOpen " button, start vavuum pumpAnd vavuum pump, butterfly valve is opened, body of heater is vacuumized.
（3）Heat up：Furnace tube is covered, power supply is connected, 5 Pa are evacuated to body of heater, be passed through high purity ammonia gas, gas
Pressure is maintained at 500 Pa, slowly rises high-temperature, and furnace body temperature is higher than 35 DEG C, it is necessary to open the cooling water of body of heater.
（4）Insulation：Temperature rises to 550 DEG C, is incubated 9 h.
（5）Cooling：After workpiece insulation terminates, stopping is passed through ammonia, continues to vacuumize, along with the furnace cooling.
（6）Come out of the stove：When workpiece temperature is down to room temperature, cooling water is closed, to body of heater air is filled with, treat stove external and internal pressure
When consistent, body of heater is opened, take out sample.
Its surface scan picture as shown in Figure 2, profile scanning picture as shown in Figure 4, friction coefficient curve such as accompanying drawing 6
It is shown, sample abrasion after polishing scratch cross section profile figure as shown in Figure 8, the nitriding layer cross section component distributing curve map such as institute of accompanying drawing 10
Show, alloying layer thickness is 6 μm, and the key property of surface ion nitriding layer is as shown in Figure 12.
Embodiment 2
Difference from Example 1 carries out nitriding by base material of AlCoCrFeNi, and other steps are identical.
Its surface scan picture as shown in Figure 3, profile scanning picture as shown in Figure 5, friction coefficient curve such as accompanying drawing 7
It is shown, sample abrasion after polishing scratch cross section profile figure as shown in Figure 9, the nitriding layer cross section component distributing curve map such as institute of accompanying drawing 11
Show, alloying layer thickness is 7 μm, and the key property of surface ion nitriding layer is as shown in Figure 13.
Claims (3)
1. a kind of method for preparing high-entropy alloy surface ion nitriding layer, the composition of the high-entropy alloy base material that methods described is adopted for
Al1.3CoCuFeNi2, configure according to mol ratio, wherein, subscript represents the molar fraction shared by the composition, does not mark lower target i.e.
Mol ratio is 1；Or
The composition of the high-entropy alloy base material is AlCoCrFeNi, according to equimolar than configuring；Or
Al, Co, Cu, Fe, Ni and Cr raw materials for metallurgy mass concentration that the high entropy alloy material is adopted is not less than 99.9 %；
The method for preparing high-entropy alloy surface ion nitriding layer is as follows：
（1）Alloy smelting raw material A l, Co of employing, Cu, Fe, Ni and Cr element are carried out into accurate weighing proportioning simultaneously according to mol ratio
Purification oxidation on metal surface thing；
In the groove that the raw material for preparing is placed in the water cooled copper mould melting pond of WK type vacuum arc furnace ignitions ,-applying argon gas, melting are vacuumized
At 250 amperes, the time is the 30-60 seconds to electric current, after alloy is sufficiently mixed, alloy block is overturn, after alloy pig is put into water-cooled
In the groove of copper mold, melting electric current is adjusted, after alloy melting is uniform, opens and inhale casting inlet valve, using vacuum in pump suction casting is carried out,
Take out after alloy mold cooling, that is, obtain the high-entropy alloy base material；
（2）High-entropy alloy base material after polishing, polishing is cleaned by supersonic wave cleaning machine, then by ion nitriding furnace zero
Part is dried, vacuum in purifying furnace；
（3）Manual air-release valves are opened, into stove air is filled with, after stove external and internal pressure is consistent, furnace tube is sling, part is placed in
The enterprising luggage stove of cathode disc, closes afterwards Manual air-release valves sealing；
（4）Furnace tube is covered, is switched on power, 5 Pa are evacuated to body of heater, high purity ammonia gas, gas are passed through into ion nitriding furnace
Pressure is maintained at 500 Pa, slowly rises high voltage, and temperature rises to 550 DEG C, is incubated 9 h, is then shut off ammonia, continues to vacuumize, with
Stove is cooled down, and when workpiece temperature is down to room temperature, closes cooling water, opens body of heater, takes out sample.
2. method according to claim 1, the purity that high purity ammonia gas are passed through into ion nitriding furnace is 99.99
%, be passed through high purity ammonia gas flow velocity be 0.4 m3/h。
3. method according to claim 1, the ion nitriding furnace is using LDMC-100A type pulse ion nitriding furnaces in height
Entropy alloy surface nitriding.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107034410A (en) * | 2017-05-12 | 2017-08-11 | 南昌大学 | A kind of many pivot high-entropy alloys and preparation method thereof |
| CN107267843A (en) * | 2017-06-28 | 2017-10-20 | 吉林化工学院 | A kind of high strength and high hardness AlCoCrFeNi high-entropy alloys and preparation method thereof |
| CN107955928A (en) * | 2017-11-06 | 2018-04-24 | 中国人民解放军国防科技大学 | High-entropy alloy surface carburization modification method |
| CN108754463A (en) * | 2018-06-13 | 2018-11-06 | 太原理工大学 | A method of improving face-centred cubic structure high-entropy alloy tensile strength |
| CN109604611A (en) * | 2019-01-09 | 2019-04-12 | 苏州科技大学 | A kind of powder metallurgy prepares the forming method of wear-and corrosion-resistant high-entropy alloy gear |
| CN109797303A (en) * | 2019-01-28 | 2019-05-24 | 太原理工大学 | A kind of raising Al0.3The method of CoCrFeNi high-entropy alloy intensity |
| CN113025966A (en) * | 2021-02-26 | 2021-06-25 | 赵中里 | Zr-based high-entropy alloy coating for prolonging service life of hot forging die and preparation method thereof |
| CN113046585A (en) * | 2021-03-17 | 2021-06-29 | 江苏理工学院 | Preparation method and application of high-entropy alloy for extremely cold environment |
| CN113652659A (en) * | 2021-08-12 | 2021-11-16 | 南京航空航天大学 | Preparation method of high-entropy alloy nitride coating metallurgically bonded with substrate |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107034410A (en) * | 2017-05-12 | 2017-08-11 | 南昌大学 | A kind of many pivot high-entropy alloys and preparation method thereof |
| CN107267843A (en) * | 2017-06-28 | 2017-10-20 | 吉林化工学院 | A kind of high strength and high hardness AlCoCrFeNi high-entropy alloys and preparation method thereof |
| CN107955928A (en) * | 2017-11-06 | 2018-04-24 | 中国人民解放军国防科技大学 | High-entropy alloy surface carburization modification method |
| CN108754463A (en) * | 2018-06-13 | 2018-11-06 | 太原理工大学 | A method of improving face-centred cubic structure high-entropy alloy tensile strength |
| CN109604611A (en) * | 2019-01-09 | 2019-04-12 | 苏州科技大学 | A kind of powder metallurgy prepares the forming method of wear-and corrosion-resistant high-entropy alloy gear |
| CN109797303A (en) * | 2019-01-28 | 2019-05-24 | 太原理工大学 | A kind of raising Al0.3The method of CoCrFeNi high-entropy alloy intensity |
| CN113025966A (en) * | 2021-02-26 | 2021-06-25 | 赵中里 | Zr-based high-entropy alloy coating for prolonging service life of hot forging die and preparation method thereof |
| CN113025966B (en) * | 2021-02-26 | 2022-05-17 | 何阳轩 | Zr-based high-entropy alloy coating for prolonging service life of hot forging die and preparation method thereof |
| CN113046585A (en) * | 2021-03-17 | 2021-06-29 | 江苏理工学院 | Preparation method and application of high-entropy alloy for extremely cold environment |
| CN113046585B (en) * | 2021-03-17 | 2022-05-13 | 江苏理工学院 | Preparation method and application of high-entropy alloy for extremely cold environment |
| CN113652659A (en) * | 2021-08-12 | 2021-11-16 | 南京航空航天大学 | Preparation method of high-entropy alloy nitride coating metallurgically bonded with substrate |
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Application publication date: 20170510 |