CN109666900A - A kind of electro beam physics vapour deposition micron multilayer complex films and preparation method thereof - Google Patents
A kind of electro beam physics vapour deposition micron multilayer complex films and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of electro beam physics vapour deposition micron multilayer complex films, including intermediate metal and ceramic layer, ceramic layer 9wt%Y2O3Stable ZrO2；Intermediate metal is nickel-base alloy.Preparation method is, firstly, to 20CrNi3A substrate is pre-processed, later cleaning experiment equipment, and substrate surface is polished, and ultrasonic cleaning in acetone, NiCoCrAl target and YSZ target are respectively placed in two crucibles, then substrate is heated to 500 DEG C, preheating time is 60min, while vacuum degree is adjusted to 10‑3~10‑ 2Pa, finally, using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron multilayer complex films.Even film layer using this method preparation is fine and close, has lower coefficient of friction and high wearability.
Description
Technical field
The invention belongs to membrane material preparation technical fields, and in particular to a kind of electro beam physics vapour deposition micron multilayer is multiple
Film is closed, the preparation method of this micron of multilayer complex films is further related to.
Background technique
The advantages of micron multilayer complex films can integrate ceramic material and metal material, intensity and toughness with higher,
Thermal expansion coefficient differs greatly between common metal/ceramic laminated material, very big heat can be introduced in these laminated materials and answered
Power causes material to be easy failure in use and destroy.Using electro beam physics vapour deposition equipment, pass through technique tune
It is whole, micron multilayer complex films are prepared, micro- pottery layer of micron multilayer complex films usually has columnar crystal structure, and strain tolerance is big, energy
The contraction and expansion of metal layer are followed, to a certain extent so as to greatly improve the impact of metal/ceramic laminated material
And service life, but metal layer columnar crystal structure can seriously damage the intensity of film layer.
Chinese patent " a kind of high-temperature alloy surface resistance to high temperature oxidation and the adhesive layer for preventing second of reaction zone from being formed and its
Preparation method " (application number: 201010034157.8, publication number: CN101746090A, publication date: 2010.06.23) it discloses
One layer of Ru is electroplated on metallic matrix using electric plating method, then using upper one layer of the method deposition of electron-beam vapor deposition
MCrAlYHf layers, the counterdiffusion of element between matrix and layer can be stopped, improve film performance, but institute's preparative layer contains column crystal knot
Structure can seriously damage the intensity of film layer, influence the comprehensive performance of film layer.
Summary of the invention
The object of the present invention is to provide a kind of electro beam physics vapour deposition micron multilayer complex films, prepared film layer is equal
Even densification has lower coefficient of friction and high wearability.
It is a further object of the present invention to provide the preparation methods of above-mentioned micron multilayer complex films.
The technical scheme adopted by the invention is that a kind of electro beam physics vapour deposition micron multilayer complex films, including gold
Belong to transition zone and ceramic layer, ceramic layer 9wt%Y2O3Stable ZrO2；Intermediate metal is nickel-base alloy, and wherein Co content is
14%~16%, Cr content are that 13%~15%, A1 content is 1%~5%, surplus Ni, the above constituent mass percentage it
Be 100%.
Another technical solution of the present invention is a kind of system of electro beam physics vapour deposition micron multilayer complex films
Preparation Method is specifically implemented according to the following steps:
Step 1, to 20CrNi3A substrate is pre-processed；
Step 2, the foreign matter for the fine sandpaper polishing stage surface for being 1200 with mesh number, later with the cotton for being moistened with dehydrated alcohol
Objective table table inner face, crucible and the groove for placing crucible in flower wiping vacuum chamber, until without obvious dirty trace, finally, using dipping in
There is cotton wiping four wall of vacuum chamber of dehydrated alcohol, removes pollutant；
Step 3, after step 2, substrate surface is polished to surface smoothness less than 0.35um, is surpassed later and in acetone
Sound wave cleans 10min~15min, is connected in the rotary shaft in operating room after drying, by NiCoCrAl target and YSZ target
Material is respectively placed in two crucibles, and the vacuum degree in operating room is finally adjusted to 10-3Pa~10-2Pa；
Step 4, after step 3, substrate is heated to 500 DEG C, preheating time 60min, is discharged adsorbed on substrate
Gas guarantees vacuum degree with higher in evaporation process, while vacuum degree is adjusted to 10-3~10-2Pa；
Step 5, more using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron after step 4
Layer composite membrane.
The features of the present invention also characterized in that
In step 1, to 20CrNi3A substrate is pre-processed, specifically:
Step 1.1, by 20CrNi3A substrate is handled through carburizing-grinding, obtains the 20CrNi that size is Ф 15mm × 5mm3A
Substrate；
Step 1.2, after step 1.1, using the bulky grain pollutant of washes of absolute alcohol substrate surface, later will
20CrNi3A substrate is successively immersed in acetone soln, ethanol solution, is cleaned by ultrasonic in deionized water, finally with inflation
Ball removes 20CrNi3The remaining solution of A substrate surface.
In step 1.1, the coefficient of friction of carburizing layer surface is 0.4~0.7, layer depth 2mm, surface hardness be HRC60~
62。
In step 1.2, scavenging period is 20min~25min.
In step 5, using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron MULTILAYER COMPOSITE
Film, the specific steps are as follows:
Step 5.1, using NiCoCrAl target as metal targets, using electron beam on substrate deposited metal transition zone, electricity
Beamlet stream is 1A~3A, and electron-beam voltage is 5KV~15KV, the average sedimentation rate 0.028um/min of intermediate metal~
0.035um/min, when deposition, ask that 120min~150min, deposition thickness are 1.85um~2.33um；
Step 5.2, after step 5.1, using YSZ target as ceramic target, using electron beam on substrate deposited ceramic layer,
Electronic beam current is 1A~4A, and electron-beam voltage is 3KV~20KV, the average sedimentation rate 0.018um/min of ceramic layer~
0.025um/min, when deposition, ask that 30min~150min, deposition thickness are 1.12um~2.45um；
Step 5.3, after step 5.2, substrate temperature is risen to 1000 DEG C, after keeping the temperature 3h, and continues to keep vacuum state,
80 DEG C~120 DEG C are naturally cooled to substrate, a micron multilayer complex films can be obtained.
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and the temperature of substrate is 500 DEG C.
The invention has the advantages that
This micron of multilayer complex films metal layer is Ni based alloy, after Overheating Treatment, main oxidation product be NiO,
Cr2O3And NiCr2O4, crystal grain is twin and dislocation, increases the plasticity of metal, reduces film layer internal stress, prepared film layer
Even compact has lower coefficient of friction and high wearability, prepares in roller surface and meet diesel engine performance requirement
Wear-resisting micron multilayer complex films solve the problems, such as that idler wheel premature wear fails.
Detailed description of the invention
Fig. 1 is the original micron layer surface topography of electro beam physics vapour deposition during the present invention is implemented；
Fig. 2 is the surface topography of the micron layer for preparing the present embodiment method after heat treatment；
Fig. 3 is the original micron layer Cross Section Morphology of electro beam physics vapour deposition during the present invention is implemented；
Fig. 4 is the Cross Section Morphology of the micron layer for preparing the present embodiment method after heat treatment；
Fig. 5 is the wear rate of the original micron layer of electro beam physics vapour deposition during the present invention is implemented；
Fig. 6 is the wear rate of the micron layer for preparing the present embodiment method after heat treatment；
Fig. 7 is the coefficient of friction of the original micron layer surface of electro beam physics vapour deposition during the present invention is implemented；
Fig. 8 is the micron layer coefficient of friction after heat treatment using the preparation of the present embodiment method.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of electro beam physics vapour deposition micron multilayer complex films of the present invention, including intermediate metal and ceramic layer, pottery
Enamel coating is 9wt%Y2O3Stable ZrO2；Intermediate metal is nickel-base alloy (Ni-15Co-13Cr-3A1), and wherein Co content is
14%~16%, Cr content are that 13%~15%, A1 content is 1%~5%, surplus Ni, the above constituent mass percentage it
Be 100%.
A kind of preparation method of electro beam physics vapour deposition micron multilayer complex films of the present invention, specifically according to the following steps
Implement:
Step 1, to 20CrNi3A substrate is pre-processed；Specifically:
Step 1.1, by 20CrNi3A substrate is handled through carburizing-grinding, obtains the 20CrNi that size is Ф 15mm × 5mm3A
Substrate；
Wherein, the coefficient of friction of carburizing layer surface is 0.4~0.7, layer depth 2mm, and surface hardness is HRC60~62；
Step 1.2, after step 1.1, using the bulky grain pollutant of washes of absolute alcohol substrate surface, later will
20CrNi3A substrate is successively immersed in acetone soln, ethanol solution, is cleaned by ultrasonic in deionized water, finally with inflation
Ball removes 20CrNi3The remaining solution of A substrate surface, the main purpose being cleaned by ultrasonic are to remove organic dirt of substrate surface
Object is contaminated, improves the surface cleanliness of substrate to improve the adhesive force between film and substrate；
Scavenging period is 20min~25min；
Step 2, the foreign matter for the fine sandpaper polishing stage surface for being 1200 with mesh number, later with the cotton for being moistened with dehydrated alcohol
Objective table table inner face, crucible and the groove for placing crucible in flower wiping vacuum chamber, until without obvious dirty trace, finally, using dipping in
There is cotton wiping four wall of vacuum chamber of dehydrated alcohol, removes pollutant；
Vacuum chamber is the key components of electro beam physics vapour deposition equipment, and all processes of plated film are all in vacuum chamber
Middle completion, and substrate is placed on objective table, the cleannes of objective table influence whether the quality of plated film, it is therefore necessary to vacuum chamber
Stringent cleaning is carried out with objective table；
Step 3, after step 2, substrate surface is polished to surface smoothness less than 0.35um, is surpassed later and in acetone
Sound wave cleans 10min~15min, is connected in the rotary shaft in operating room after drying, by NiCoCrAl target (metallic target
Material) and YSZ target (ceramic target) be respectively placed in two crucibles, the vacuum degree in operating room is finally adjusted to 10-3Pa~
10-2Pa；
Step 4, after step 3, substrate is heated to 500 DEG C, preheating time 60min, is discharged adsorbed on substrate
Gas guarantees vacuum degree with higher in evaporation process, while vacuum degree is adjusted to 10-3~10-2Pa；
Step 5, more using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron after step 4
Layer composite membrane, the specific steps are as follows:
Step 5.1, using NiCoCrAl target as metal targets, using electron beam on substrate deposited metal transition zone, electricity
Beamlet stream is 1A~3A, and electron-beam voltage is 5KV~15KV, the average sedimentation rate 0.028um/min of intermediate metal~
0.035um/min, when deposition, ask that 120min~150min, deposition thickness are 1.85um~2.33um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.2, after step 5.1, using YSZ target as ceramic target, using electron beam on substrate deposited ceramic layer,
Electronic beam current is 1A~4A, and electron-beam voltage is 3KV~20KV, the average sedimentation rate 0.018um/min of ceramic layer~
0.025um/min, when deposition, ask that 30min~150min, deposition thickness are 1.12um~2.45um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.3, after step 5.2, substrate temperature is risen to 1000 DEG C, after keeping the temperature 3h, and continues to keep vacuum state,
80 DEG C~120 DEG C are naturally cooled to substrate, a micron multilayer complex films can be obtained.
Embodiment 1
A kind of preparation method of electro beam physics vapour deposition micron multilayer complex films of the present invention, specifically according to the following steps
Implement:
Step 1, to 20CrNi3A substrate is pre-processed；Specifically:
Step 1.1, by 20CrNi3A substrate is handled through carburizing-grinding, obtains the 20CrNi that size is Ф 15mm × 5mm3A
Substrate；
Wherein, the coefficient of friction of carburizing layer surface is 0.4, layer depth 2mm, surface hardness HRC60；
Step 1.2, after step 1.1, using the bulky grain pollutant of washes of absolute alcohol substrate surface, later will
20CrNi3A substrate is successively immersed in acetone soln, ethanol solution, is cleaned by ultrasonic in deionized water, finally with inflation
Ball removes 20CrNi3The remaining solution of A substrate surface, the main purpose being cleaned by ultrasonic are to remove organic dirt of substrate surface
Object is contaminated, improves the surface cleanliness of substrate to improve the adhesive force between film and substrate；
Scavenging period is 20min；
Step 2, the foreign matter for the fine sandpaper polishing stage surface for being 1200 with mesh number, later with the cotton for being moistened with dehydrated alcohol
Objective table table inner face, crucible and the groove for placing crucible in flower wiping vacuum chamber, until without obvious dirty trace, finally, using dipping in
There is cotton wiping four wall of vacuum chamber of dehydrated alcohol, removes pollutant；
Step 3, after step 2, substrate surface is polished to surface smoothness less than 0.35um, is surpassed later and in acetone
Sound wave cleans 10min, is connected in the rotary shaft in operating room after drying, by NiCoCrAl target (metal targets) and
YSZ target (ceramic target) is respectively placed in two crucibles, and the vacuum degree in operating room is finally adjusted to 10-3Pa；
Step 4, after step 3, substrate is heated to 500 DEG C, preheating time 60min, is discharged adsorbed on substrate
Gas guarantees vacuum degree with higher in evaporation process, while vacuum degree is adjusted to 10-3；
Step 5, more using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron after step 4
Layer composite membrane, the specific steps are as follows:
Step 5.1, using NiCoCrAl target as metal targets, using electron beam on substrate deposited metal transition zone, electricity
Beamlet stream is 1A, electron-beam voltage 5KV, the average sedimentation rate 0.028um/min of intermediate metal, and when deposition asks
120min, deposition thickness 1.85um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.2, after step 5.1, using YSZ target as ceramic target, using electron beam on substrate deposited ceramic layer,
Electronic beam current is 1A, electron-beam voltage 3KV, the average sedimentation rate 0.018um/min of ceramic layer, and when deposition asks 30min, is sunk
Product is with a thickness of 1.12um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.3, after step 5.2, substrate temperature is risen to 1000 DEG C, after keeping the temperature 3h, and continues to keep vacuum state,
80 DEG C are naturally cooled to substrate, a micron multilayer complex films can be obtained.
In the present embodiment, the original micron layer surface topography of electro beam physics vapour deposition, as shown in Figure 1, its composite membrane table
There is cavity in face, influences film layer comprehensive performance, using the present embodiment method preparation micron layer after heat treatment, composite film table
Face is fine and close, as shown in Fig. 2, the wear-resisting property of film layer can be significantly improved；The original micron layer cross section of electro beam physics vapour deposition
Pattern, as shown in figure 3, intermediate metal is layer columnar crystal structure, column crystal width should be several hundred nanometers, serious damage film layer
The porosity of intensity, column intergranular is usually larger, and the combination of intergranular is also poor, and uses the micron layer of the present embodiment method preparation
After heat treatment, in metal layer biggish crystal grain cluster gap oneself through disappearing, as shown in figure 4, its main oxidation product is
NiO、Cr2O3And NiCr2O4, crystal grain is twin and dislocation, increases the plasticity of metal, reduces film layer internal stress.
In the present embodiment, the original micron layer wear rate of electro beam physics vapour deposition, as shown in figure 5, its original micron layer
Wear rate is 4.45 × 10-17, using the present embodiment method preparation micron layer after heat treatment, as shown in fig. 6, its wear rate
It is 1.02 × 10-17；The original micron layer coefficient of friction of electro beam physics vapour deposition, as shown in fig. 7, original micron layer friction system
Number is 0.29；Using the present embodiment method preparation micron layer after heat treatment, as shown in figure 8, its coefficient of friction be 0.18, this
Illustrate that the coefficient of friction of micron layer can be effectively reduced in this method.
Embodiment 2
A kind of preparation method of electro beam physics vapour deposition micron multilayer complex films of the present invention, specifically according to the following steps
Implement:
Step 1, to 20CrNi3A substrate is pre-processed；Specifically:
Step 1.1, by 20CrNi3A substrate is handled through carburizing-grinding, obtains the 20CrNi that size is Ф 15mm × 5mm3A
Substrate；
Wherein, the coefficient of friction of carburizing layer surface is 0.5, layer depth 2mm, surface hardness HRC60；
Step 1.2, after step 1.1, using the bulky grain pollutant of washes of absolute alcohol substrate surface, later will
20CrNi3A substrate is successively immersed in acetone soln, ethanol solution, is cleaned by ultrasonic in deionized water, finally with inflation
Ball removes 20CrNi3The remaining solution of A substrate surface；
Scavenging period is 20min；
Step 2, the foreign matter for the fine sandpaper polishing stage surface for being 1200 with mesh number, later with the cotton for being moistened with dehydrated alcohol
Objective table table inner face, crucible and the groove for placing crucible in flower wiping vacuum chamber, until without obvious dirty trace, finally, using dipping in
There is cotton wiping four wall of vacuum chamber of dehydrated alcohol, removes pollutant；
Step 3, after step 2, substrate surface is polished to surface smoothness less than 0.35um, is surpassed later and in acetone
Sound wave cleans 10min, is connected in the rotary shaft in operating room after drying, by NiCoCrAl target (metal targets) and
YSZ target (ceramic target) is respectively placed in two crucibles, and the vacuum degree in operating room is finally adjusted to 10-3Pa；
Step 4, after step 3, substrate is heated to 500 DEG C, preheating time 60min, is discharged adsorbed on substrate
Gas guarantees vacuum degree with higher in evaporation process, while vacuum degree is adjusted to 10-3；
Step 5, more using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron after step 4
Layer composite membrane, the specific steps are as follows:
Step 5.1, using NiCoCrAl target as metal targets, using electron beam on substrate deposited metal transition zone, electricity
Beamlet stream is 1.5A, electron-beam voltage 6KV, the average sedimentation rate 0.03um/min of intermediate metal, and when deposition asks
125min, deposition thickness 2um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.2, after step 5.1, using YSZ target as ceramic target, using electron beam on substrate deposited ceramic layer,
Electronic beam current is 3A, electron-beam voltage 5KV, the average sedimentation rate 0.02um/min of ceramic layer, and when deposition asks 50min, is sunk
Product is with a thickness of 1.8um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.3, after step 5.2, substrate temperature is risen to 1000 DEG C, after keeping the temperature 3h, and continues to keep vacuum state,
90 DEG C are naturally cooled to substrate, a micron multilayer complex films can be obtained.
Embodiment 3
A kind of preparation method of electro beam physics vapour deposition micron multilayer complex films of the present invention, specifically according to the following steps
Implement:
Step 1, to 20CrNi3A substrate is pre-processed；Specifically:
Step 1.1, by 20CrNi3A substrate is handled through carburizing-grinding, obtains the 20CrNi that size is Ф 15mm × 5mm3A
Substrate；
Wherein, the coefficient of friction of carburizing layer surface is 0.7, layer depth 2mm, surface hardness HRC62；
Step 1.2, after step 1.1, using the bulky grain pollutant of washes of absolute alcohol substrate surface, later will
20CrNi3A substrate is successively immersed in acetone soln, ethanol solution, is cleaned by ultrasonic in deionized water, finally with inflation
Ball removes 20CrNi3The remaining solution of A substrate surface；
Scavenging period is 25min；
Step 2, the foreign matter for the fine sandpaper polishing stage surface for being 1200 with mesh number, later with the cotton for being moistened with dehydrated alcohol
Objective table table inner face, crucible and the groove for placing crucible in flower wiping vacuum chamber, until without obvious dirty trace, finally, using dipping in
There is cotton wiping four wall of vacuum chamber of dehydrated alcohol, removes pollutant；
Step 3, after step 2, substrate surface is polished to surface smoothness less than 0.35um, is surpassed later and in acetone
Sound wave cleans 14min, is connected in the rotary shaft in operating room after drying, by NiCoCrAl target (metal targets) and
YSZ target (ceramic target) is respectively placed in two crucibles, and the vacuum degree in operating room is finally adjusted to 10-2Pa；
Step 4, after step 3, substrate is heated to 500 DEG C, preheating time 60min, is discharged adsorbed on substrate
Gas guarantees vacuum degree with higher in evaporation process, while vacuum degree is adjusted to 10-2Pa；
Step 5, more using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron after step 4
Layer composite membrane, the specific steps are as follows:
Step 5.1, using NiCoCrAl target as metal targets, using electron beam on substrate deposited metal transition zone, electricity
Beamlet stream is 2A, electron-beam voltage 10KV, the average sedimentation rate 0.032um/min of intermediate metal, and when deposition asks
140min, deposition thickness 2.10um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.2, after step 5.1, using YSZ target as ceramic target, using electron beam on substrate deposited ceramic layer,
Electronic beam current is 3A, electron-beam voltage 6KV, the average sedimentation rate 0.025um/min of ceramic layer, when deposition ask 30min~
150min, deposition thickness 2.15um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.3, after step 5.2, substrate temperature is risen to 1000 DEG C, after keeping the temperature 3h, and continues to keep vacuum state,
100 DEG C are naturally cooled to substrate, a micron multilayer complex films can be obtained.
Embodiment 4
A kind of preparation method of electro beam physics vapour deposition micron multilayer complex films of the present invention, specifically according to the following steps
Implement:
Step 1, to 20CrNi3A substrate is pre-processed；Specifically:
Step 1.1, by 20CrNi3A substrate is handled through carburizing-grinding, obtains the 20CrNi that size is Ф 15mm × 5mm3A
Substrate；
Wherein, the coefficient of friction of carburizing layer surface is 0.7, layer depth 2mm, surface hardness HRC62；
Step 1.2, after step 1.1, using the bulky grain pollutant of washes of absolute alcohol substrate surface, later will
20CrNi3A substrate is successively immersed in acetone soln, ethanol solution, is cleaned by ultrasonic in deionized water, finally with inflation
Ball removes 20CrNi3The remaining solution of A substrate surface；
Scavenging period is 25min；
Step 2, the foreign matter for the fine sandpaper polishing stage surface for being 1200 with mesh number, later with the cotton for being moistened with dehydrated alcohol
Objective table table inner face, crucible and the groove for placing crucible in flower wiping vacuum chamber, until without obvious dirty trace, finally, using dipping in
There is cotton wiping four wall of vacuum chamber of dehydrated alcohol, removes pollutant；
Step 3, after step 2, substrate surface is polished to surface smoothness less than 0.35um, is surpassed later and in acetone
Sound wave cleans 10min, is connected in the rotary shaft in operating room after drying, by NiCoCrAl target (metal targets) and
YSZ target (ceramic target) is respectively placed in two crucibles, and the vacuum degree in operating room is finally adjusted to 10-3Pa~10- 2Pa；
Step 4, after step 3, substrate is heated to 500 DEG C, preheating time 60min, is discharged adsorbed on substrate
Gas guarantees vacuum degree with higher in evaporation process, while vacuum degree is adjusted to 10-3Pa；
Step 5, more using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron after step 4
Layer composite membrane, the specific steps are as follows:
Step 5.1, using NiCoCrAl target as metal targets, using electron beam on substrate deposited metal transition zone, electricity
Beamlet stream is 3A, electron-beam voltage 12KV, the average sedimentation rate 0.032um/min of intermediate metal, and when deposition asks
145min, deposition thickness 2.25um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.2, after step 5.1, using YSZ target as ceramic target, using electron beam on substrate deposited ceramic layer,
Electronic beam current is 2A, electron-beam voltage 16KV, the average sedimentation rate 0.018um/min of ceramic layer, and when deposition asks 60min,
Deposition thickness is 2.2um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.3, after step 5.2, substrate temperature is risen to 1000 DEG C, after keeping the temperature 3h, and continues to keep vacuum state,
110 DEG C are naturally cooled to substrate, a micron multilayer complex films can be obtained.
Embodiment 5
A kind of preparation method of electro beam physics vapour deposition micron multilayer complex films of the present invention, specifically according to the following steps
Implement:
Step 1, to 20CrNi3A substrate is pre-processed；Specifically:
Step 1.1, by 20CrNi3A substrate is handled through carburizing-grinding, obtains the 20CrNi that size is Ф 15mm × 5mm3A
Substrate；
Wherein, the coefficient of friction of carburizing layer surface is 0.7, layer depth 2mm, surface hardness HRC62；
Step 1.2, after step 1.1, using the bulky grain pollutant of washes of absolute alcohol substrate surface, later will
20CrNi3A substrate is successively immersed in acetone soln, ethanol solution, is cleaned by ultrasonic in deionized water, finally with inflation
Ball removes 20CrNi3The remaining solution of A substrate surface；
Scavenging period is 25min；
Step 2, the foreign matter for the fine sandpaper polishing stage surface for being 1200 with mesh number, later with the cotton for being moistened with dehydrated alcohol
Objective table table inner face, crucible and the groove for placing crucible in flower wiping vacuum chamber, until without obvious dirty trace, finally, using dipping in
There is cotton wiping four wall of vacuum chamber of dehydrated alcohol, removes pollutant；
Step 3, after step 2, substrate surface is polished to surface smoothness less than 0.35um, is surpassed later and in acetone
Sound wave cleans 15min, is connected in the rotary shaft in operating room after drying, by NiCoCrAl target (metal targets) and
YSZ target (ceramic target) is respectively placed in two crucibles, and the vacuum degree in operating room is finally adjusted to 10-2Pa；
Step 4, after step 3, substrate is heated to 500 DEG C, preheating time 60min, is discharged adsorbed on substrate
Gas guarantees vacuum degree with higher in evaporation process, while vacuum degree is adjusted to 10-2Pa；
Step 5, more using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron after step 4
Layer composite membrane, the specific steps are as follows:
Step 5.1, using NiCoCrAl target as metal targets, using electron beam on substrate deposited metal transition zone, electricity
Beamlet stream is 3A, electron-beam voltage 15KV, the average sedimentation rate 0.035um/min of intermediate metal, and when deposition asks
150min, deposition thickness 2.33um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.2, after step 5.1, using YSZ target as ceramic target, using electron beam on substrate deposited ceramic layer,
Electronic beam current is 4A, electron-beam voltage 20KV, the average sedimentation rate 0.025um/min of ceramic layer, and when deposition asks 150min,
Deposition thickness is 2.45um；
In deposition process, substrate rotates 40 turns around rotary shaft per minute, and substrate temperature is 500 DEG C；
Step 5.3, after step 5.2, substrate temperature is risen to 1000 DEG C, after keeping the temperature 3h, and continues to keep vacuum state,
120 DEG C are naturally cooled to substrate, a micron multilayer complex films can be obtained.
The micron multilayer complex films of the method for the present invention preparation, metal layer is Ni based alloy, main after Overheating Treatment
Oxidation product is NiO, Cr2O3And NiCr2O4, crystal grain is twin and dislocation, increases the plasticity of metal, reduces in film layer and answer
Power, prepared even film layer is fine and close, has lower coefficient of friction and high wearability, prepares in roller surface and meet bavin
The wear-resisting micron multilayer complex films of oil machine performance requirement solve the problems, such as that idler wheel premature wear fails.
Claims (7)
1. a kind of electro beam physics vapour deposition micron multilayer complex films, which is characterized in that including intermediate metal and ceramic layer,
Ceramic layer is 9wt%Y2O3Stable ZrO2；Intermediate metal is nickel-base alloy, and wherein Co content is 14%~16%, Cr content
It is 1%~5% for 13%~15%, A1 content, surplus Ni, the sum of above constituent mass percentage is 100%.
2. a kind of preparation method of electro beam physics vapour deposition micron multilayer complex films, which is characterized in that specifically according to following
Step is implemented:
Step 1, to 20CrNi3A substrate is pre-processed；
Step 2, the foreign matter for the fine sandpaper polishing stage surface for being 1200 with mesh number, is wiped with the cotton for being moistened with dehydrated alcohol later
Objective table table inner face in vacuum chamber, crucible and the groove for placing crucible are wiped, until without obvious dirty trace, finally, using nothing is moistened with
The cotton of water-ethanol wipes four wall of vacuum chamber, removes pollutant；
Step 3, after step 2, substrate surface is polished to surface smoothness less than 0.35um, later and in acetone ultrasonic wave
10min~15min is cleaned, is connected in the rotary shaft in operating room after drying, by NiCoCrAl target and YSZ target point
It is not placed in two crucibles, the vacuum degree in operating room is finally adjusted to 10-3Pa~10-2Pa；
Step 4, after step 3, substrate is heated to 500 DEG C, preheating time 60min, discharges adsorbed gas on substrate,
Guarantee vacuum degree with higher in evaporation process, while vacuum degree is adjusted to 10-3~10-2Pa；
Step 5, it after step 4, is answered using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron multilayer
Close film.
3. a kind of preparation method of electro beam physics vapour deposition micron multilayer complex films according to claim 2, special
Sign is, in the step 1, to 20CrNi3A substrate is pre-processed, specifically:
Step 1.1, by 20CrNi3A substrate is handled through carburizing-grinding, obtains the 20CrNi that size is Ф 15mm × 5mm3A base
Plate；
Step 1.2, after step 1.1, using the bulky grain pollutant of washes of absolute alcohol substrate surface, later by 20CrNi3A
Substrate is successively immersed in acetone soln, ethanol solution, is cleaned by ultrasonic in deionized water, is finally removed with inflatable ball
20CrNi3The remaining solution of A substrate surface.
4. a kind of preparation method of electro beam physics vapour deposition micron multilayer complex films according to claim 3, special
Sign is, in the step 1.1, the coefficient of friction of carburizing layer surface is 0.4~0.7, layer depth 2mm, surface hardness HRC60
~62.
5. a kind of preparation method of electro beam physics vapour deposition micron multilayer complex films according to claim 3, special
Sign is, in the step 1.2, scavenging period is 20min~25min.
6. a kind of preparation method of electro beam physics vapour deposition micron multilayer complex films according to claim 2, special
Sign is, in the step 5, is answered using two electron gun alternatively vaporised NiCoCrAl targets and YSZ target material deposition micron multilayer
Close film, the specific steps are as follows:
Step 5.1, using NiCoCrAl target as metal targets, using electron beam on substrate deposited metal transition zone, electron beam
Stream is 1A~3A, and electron-beam voltage is 5KV~15KV, the average sedimentation rate 0.028um/min of intermediate metal~
0.035um/min, when deposition, ask that 120min~150min, deposition thickness are 1.85um~2.33um；
Step 5.2, after step 5.1, using YSZ target as ceramic target, using electron beam on substrate deposited ceramic layer, electronics
Line is 1A~4A, and electron-beam voltage is 3KV~20KV, average sedimentation rate 0.018um/min~0.025um/ of ceramic layer
Min, when deposition, ask that 30min~150min, deposition thickness are 1.12um~2.45um；
Step 5.3, after step 5.2, substrate temperature is risen to 1000 DEG C, after keeping the temperature 3h, and continues to keep vacuum state, to base
Plate naturally cools to 80 DEG C~120 DEG C, and a micron multilayer complex films can be obtained.
7. a kind of preparation method of electro beam physics vapour deposition micron multilayer complex films according to claim 6, special
Sign is, in the deposition process, substrate rotates 40 turns around rotary shaft per minute, and the temperature of substrate is 500 DEG C.
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