CN106835131A - A kind of preparation of plural layers and its method for Combined with Performance Evaluation - Google Patents
A kind of preparation of plural layers and its method for Combined with Performance Evaluation Download PDFInfo
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- CN106835131A CN106835131A CN201710160656.3A CN201710160656A CN106835131A CN 106835131 A CN106835131 A CN 106835131A CN 201710160656 A CN201710160656 A CN 201710160656A CN 106835131 A CN106835131 A CN 106835131A
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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Abstract
Prepared the invention discloses a kind of plural layers and Combined with Performance Evaluation method, depositing Cr binder courses, CrN transition zones and CrMoAlN functional layers respectively by non-equilibrium ion sputtering film coating technique by H13 matrixes is obtained Cr CrN CrMoAlN plural layers；Cr target currents 4A, Al target current 6A, Mo target current is set and is set in 0 ~ 6A, bias 75V, Cr binder courses deposition 360s, CrN transition zones deposition 600s, CrMoAlN functional layers deposition 3600s；Scratch experiment is carried out by multi-functional scratching instrument；Light confocal scanning microscope obtains film surface cut pattern and assesses its binding ability.Prepared plural layers structure in gradient, Cr layers of bottoming improves the associativity of film；CrN strengthens the bearing capacity of film as transition zone；CrMoAlN can improve the high temperature resistant and crocking resistance of film as functional layer.The present invention characterizes the difference caused due to Mo content differences in the binding ability of film using scarification simultaneously.
Description
Technical field
Prepared and its associativity the invention belongs to field of membrane material, more particularly to a kind of Cr-CrN-CrMoAlN plural layers
The method that can be evaluated.
Background technology
Mould is widely used in plastic part, diecast parts, sheet metal part, the big rule of formation of parts and forging product
Mould is produced.Mold machining technology occupies an important position in modern industry production.Wherein, H13 steel is as a kind of hot-work die
Steel, is widely used in hot forging, hot extruding die and non-ferrous metal compression mod.But because working condition is severe, H13 steel is easily in table
Failed at face.In order to improve life-span and the quality of mould, reduces cost, development kinds of surface modified technique skill
Art carrys out comprehensive hardness, wearability, intensity, toughness and the corrosion resistance for improving its surface.Wherein PVD coating technologies are to apply at present most
It is also simultaneously extensively a class sufacing of most worthy, what is obtained over nearly twenty or thirty year develops rapidly.
At present, most widely used PVD hard coats are mainly the binary coating that CrN and TiN is representative.But, due to
The complexity of operating mode, these binary coatings can not fully meet use demand.And ternary, quaternary for occurring in the prior art etc.
Polynary hard coat, by adding some metallic elements（Such as Al, W, Zr, V, Mo）Increase coating in nitride coatings
Can, but the market demand can not be met.
The content of the invention
In order to solve the above problems, first purpose of the invention is to provide a kind of preparation method of plural layers, so that
Further increase the species of plural layers, optimize market.
Adopted the following technical scheme that for this：
A kind of preparation method of plural layers, it is characterised in that：The plural layers with H13 as matrix, by non-on matrix
Ion balance sputter coating process deposited in sequential Cr binder courses, CrN transition zones and CrMoAlN functional layers；Specific preparation process is such as
Under：
Step（1）Non-equilibrium plasma sputter coating apparatus are opened, start preheating cools down water flowing, successively opens mechanical pump and molecular pump,
It is evacuated to 1.0 × 10-4Pa;
Step（2）Argon gas is passed through, gas cylinder valve and flowmeter is adjusted, vacuum intracavity gas are adjusted, makes magnetic control target electric discharge build-up of luminance；
Step（3）Matrix surface plasma cleaning：Substrate bias are adjusted to -450V, with Ar Ions Bombardment matrix surfaces, remove base
Body surface impurity, cleans 20min;
Step（4）Substrate bias are adjusted to -100V, while opening two Cr targets, target current is set to 4A, deposits one layer of simple metal
Cr layers of bottoming；
Step（5）Substrate bias are adjusted to -75V, are passed through nitrogen, deposit CrN transition zones, and nitrogen flow is controlled by OEM systems,
Gradually decrease the Cr atom numbers of target as sputter, the N content in coating gradually increases；
Step（6）Al targets and Mo targets are opened, Al target currents are gradually increased to 6A, and Mo target currents increase to specified numerical value, and four targets are complete
Portion is in opening, starts deposition CrMoAlN functional layers 60min, you can obtain Cr-CrN-CrMoAlN plural layers；
Step（7）After coating is completed and cooled down, coating chamber is deflated, and is sampled and is vacuumized；
Cr-CrN-CrMoAlN plural layers are finally obtained, the Cr joint thickness is 0.2 ~ 0.4 μm；The CrN transition zones
Thickness is 1.0 ~ 1.2 μm；The CrMoAlN functional layers thickness is 2.2 ~ 2.4 μm；The total coating thickness is 3.4 ~ 4 μm.
It is a further object of the invention to provide a kind of method of plural layers Combined with Performance Evaluation, so that accurate high
Judge the film binding ability of target product in effect ground.
Adopted the following technical scheme that for this：
A kind of method of plural layers Combined with Performance Evaluation, it is characterised in that methods described is carried out as follows：
Step A）By H13 matrixes by non-equilibrium ion sputtering film coating technique deposit respectively Cr binder courses, CrN transition zones and
CrMoAlN functional layers are obtained Cr-CrN-CrMoAlN plural layers；
Setting device parameter is：Cr target currents 4A, Al target current 6A, Mo target current is set in 0 ~ 6A, bias -75V, Cr combination
Layer deposition 360s, CrN transition zones deposition 600s, CrMoAlN functional layers deposition 3600s；
Cr-CrN-CrMoAlN plural layers are obtained, the Cr joint thickness is 0.2 ~ 0.4 μm；The CrN transition region thicknesses
It is 1.0 ~ 1.2 μm；The CrMoAlN functional layers thickness is 2.2 ~ 2.4 μm；The total coating thickness is 3.4 ~ 4 μm；
Step B）Take step A）Prepared Cr-CrN-CrMoAlN plural layers carry out scratch experiment by multi-functional scratching instrument；
Wherein：Maximum load is 30N, and loading speed is 30mN/s, and cut length is 1mm；
Step C）Take step A）Prepared Cr-CrN-CrMoAlN plural layers are obtained by laser confocal scanning microscope
Film surface cut pattern assesses its binding ability.
By technical scheme, a kind of Cr-CrN-CrMoAlN gradient functions ganoine thin film, this hair are obtained in that
The bright two kinds of elements of Al, Mo that be with the addition of on the basis of CrN form quaternary hard nitride coatings, and provide a kind of film associativity
The method that can be evaluated, is directed to the institutional framework and binding ability of the CrMoAlN coatings of different Mo target currents.Wherein, associativity
Can be characterized using scarification.This method principle is simple, and more directly perceived, therefore can be widely used.
Compared with prior art, the beneficial effects are mainly as follows：
Prepared Cr-CrN-CrMoAlN plural layers structure in gradient, wherein Cr layers of bottoming improves the associativity of film；CrN
Strengthen the bearing capacity of film as transition zone；CrMoAlN can improve the high temperature resistant and crocking resistance of film as functional layer.
Meanwhile, the present invention causes the difference in the binding ability of film using scarification further characterization due to Mo content differences, clearly
Requirement of the film to Mo contents, further optimization Cr-CrN-CrMoAlN plural layers performances.
Brief description of the drawings
Fig. 1 is Cr-CrN-CrMoAlN multi-layer film structure schematic diagrames.
Fig. 2 A ~ D is respectively the surface topography map of the film of embodiment one to four.
Fig. 3 is the cut shape appearance figure of embodiment one.
Fig. 4 is the cut shape appearance figure of embodiment two.
Fig. 5 is the cut shape appearance figure of embodiment three.
Fig. 6 is the cut shape appearance figure of example IV.
Specific embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This：
Embodiment one：
Step（1）The closed field unbalanced plasma sputter coating apparatus preheating of Teer-UDP650/4 types is opened, water flowing is cooled down, successively beaten
Mechanical pump and molecular pump are driven, 1.0 × 10 are evacuated to-4Pa;
Step（2）Argon gas is passed through, gas cylinder valve and flowmeter is adjusted, vacuum intracavity gas are adjusted, makes magnetic control target electric discharge build-up of luminance；
Step（3）Matrix surface plasma cleaning：Substrate bias are adjusted to -450V, with Ar Ions Bombardment matrix surfaces, remove base
Body surface impurity, cleans 20min;
Step（4）Substrate bias are adjusted to -100V, while opening two Cr targets, target current is set to 4A, deposits one layer of simple metal
Cr layers of bottoming, deposits 360s.
Step（5）Substrate bias are adjusted to -75V, are passed through nitrogen, deposit CrN transition zones, and nitrogen is controlled by OEM systems
Flow, gradually decreases the Cr atom numbers of target as sputter, and the N content in coating gradually increases, and deposits 600s；
Step（6）Al targets are opened, Al target currents are gradually increased to 6A, and three targets are in opening, and Mo targets are closed（I.e.
Mo target currents are 0A）.Start to deposit CrMoAlN functional layer 60min, obtain Cr-CrN-CrAlN plural layers.
Step（7）After coating is completed and cooled down, coating chamber is deflated, and is sampled and is vacuumized.
Finally as shown in figure 1, plural layers be matrix 1 with H13, the Cr is tied prepared Cr-CrN-CrMoAlN plural layers
It is 0.2 ~ 0.4 μm to close the thickness of layer 2；The thickness of CrN transition zones 3 is 1.0 ~ 1.2 μm；The thickness of CrMoAlN functional layers 4 is
2.2~2.4μm；The total coating thickness is 3.4 ~ 4 μm.
According to step（1）~（7）It is the Cr-CrN-CrAlN plural layers of 0A, its surface topography such as Fig. 2 to obtain Mo target currents
Shown in middle A.The film surface appearance is in thicker graininess as seen from the figure.Tissue is more smoothed out, with certain mechanical property
Energy.Fig. 3 is the surface scratch shape appearance figure of the film.It can thus be appreciated that in the case of without Mo elements, film crack cracking is early simultaneously
And have a large amount of obscissions.It can thus be appreciated that the film binding ability is poor.
Embodiment two：
Step（1）The closed field unbalanced plasma sputter coating apparatus preheating of Teer-UDP650/4 types is opened, water flowing is cooled down, successively beaten
Mechanical pump and molecular pump are driven, 1.0 × 10 are evacuated to-4Pa;
Step（2）Argon gas is passed through, gas cylinder valve and flowmeter is adjusted, vacuum intracavity gas are adjusted, makes magnetic control target electric discharge build-up of luminance；
Step（3）Matrix surface plasma cleaning：Substrate bias are adjusted to -450V, with Ar Ions Bombardment matrix surfaces, remove base
Body surface impurity, cleans 20min;
Step（4）Substrate bias are adjusted to -100V, while opening two Cr targets, target current is set to 4A, deposits one layer of simple metal
Cr layers of bottoming, deposits 360s.
Step（5）Substrate bias are adjusted to -75V, are passed through nitrogen, deposit CrN transition zones, and nitrogen is controlled by OEM systems
Flow, gradually decreases the Cr atom numbers of target as sputter, and the N content in coating gradually increases, and deposits 600s；
Step（6）Al targets and Mo targets are opened, Al target currents are gradually increased to 6A, and Mo target currents are gradually increased to 2A, and four targets are in
Opening.Start to deposit CrMoAlN functional layer 60min, obtain Cr-CrN-CrMoAlN plural layers.
Step（7）After coating is completed and cooled down, coating chamber is deflated, and is sampled and is vacuumized.
According to step（1）~（7）Cr-CrN-CrMoAlN plural layers when the Mo target currents that will be obtained are 2A, its surface
Pattern is as shown in B in Fig. 2.As seen from the figure, the film surface crystal grain has diminution compared with Fig. 2A, and surface is tightr, with preferable
Mechanical property.Fig. 4 is the surface scratch shape appearance figure of the film.Thus know, when Mo target currents are 2A, due to lacking for Mo elements
Amount adds the crackle and obscission that cause film surface to alleviate, but still obvious.Therefore Mo elements are combined for film
The improvement of performance has certain effect.
Embodiment three：
Step（1）The closed field unbalanced plasma sputter coating apparatus preheating of Teer-UDP650/4 types is opened, water flowing is cooled down, successively beaten
Mechanical pump and molecular pump are driven, 1.0 × 10 are evacuated to-4Pa;
Step（2）Argon gas is passed through, gas cylinder valve and flowmeter is adjusted, vacuum intracavity gas are adjusted, makes magnetic control target electric discharge build-up of luminance；
Step（3）Matrix surface plasma cleaning：Substrate bias are adjusted to -450V, with Ar Ions Bombardment matrix surfaces, remove base
Body surface impurity, cleans 20min;
Step（4）Substrate bias are adjusted to -100V, while opening two Cr targets, target current is set to 4A, deposits one layer of simple metal
Cr layers of bottoming, deposits 360s.
Step（5）Substrate bias are adjusted to -75V, are passed through nitrogen, deposit CrN transition zones, and nitrogen is controlled by OEM systems
Flow, gradually decreases the Cr atom numbers of target as sputter, and the N content in coating gradually increases, and deposits 600s；
Step（6）Al targets and Mo targets are opened, Al target currents are gradually increased to 6A, and Mo target currents are gradually increased to 4A, and four targets are in
Opening.Start to deposit CrMoAlN functional layer 60min, obtain Cr-CrN-CrMoAlN plural layers.
Step（7）After coating is completed and cooled down, coating chamber is deflated, and is sampled and is vacuumized.
According to step（1）~（7）Obtain Cr-CrN-CrMoAlN plural layers when Mo target currents are 4A, its surface topography
As shown in C in Fig. 2.Now, with the increase of Mo contents, film surface crystal grain more compacts, smaller, with good power
Learn performance.Fig. 5 is Cr-CrN-CrMoAlN plural layers surface scratch patterns when Mo target currents are 4A.Now, crackle and de-
The phenomenon that falls is significantly reduced, and the diaphragm failure time is also delayed significantly.The raising of this explanation Mo content considerably increases film
Binding ability.
Example IV：
Step（1）The closed field unbalanced plasma sputter coating apparatus preheating of Teer-UDP650/4 types is opened, water flowing is cooled down, successively beaten
Mechanical pump and molecular pump are driven, 1.0 × 10 are evacuated to-4Pa;
Step（2）Argon gas is passed through, gas cylinder valve and flowmeter is adjusted, vacuum intracavity gas are adjusted, makes magnetic control target electric discharge build-up of luminance；
Step（3）Matrix surface plasma cleaning：Substrate bias are adjusted to -450V, with Ar Ions Bombardment matrix surfaces, remove base
Body surface impurity, cleans 20min;
Step（4）Substrate bias are adjusted to -100V, while opening two Cr targets, target current is set to 4A, deposits one layer of simple metal
Cr layers of bottoming, deposits 360s.
Step（5）Substrate bias are adjusted to -75V, are passed through nitrogen, deposit CrN transition zones, and nitrogen is controlled by OEM systems
Flow, gradually decreases the Cr atom numbers of target as sputter, and the N content in coating gradually increases, and deposits 600s；
Step（6）Al targets and Mo targets are opened, Al target currents are gradually increased to 6A, and Mo target currents are gradually increased to 6A, and four targets are in
Opening.Start to deposit CrMoAlN functional layer 60min, obtain Cr-CrN-CrMoAlN plural layers.
Step（7）After coating is completed and cooled down, coating chamber is deflated, and is sampled and is vacuumized.
According to step（1）~（7）Obtain Cr-CrN-CrMoAlN plural layers when Mo target currents are 6A, its surface topography
As shown in D in Fig. 2.Now, most closely careful defect is less for film surface crystal grain, with good mechanical property.Fig. 6 is Mo targets
Cr-CrN-CrMoAlN plural layers surface scratch patterns when electric current is 6A.Now, crackle is largely suppressed, and it is existing to come off
As being substantially not present.This explanation film is in the case where Mo content compositions are larger, and the performance of its binding ability is the most excellent.
Claims (2)
1. a kind of preparation method of plural layers, it is characterised in that：The plural layers pass through with H13 as matrix on matrix
Non-equilibrium ion sputtering film coating technique deposited in sequential Cr binder courses, CrN transition zones and CrMoAlN functional layers；Specific preparation process
It is as follows：
Step（1）Non-equilibrium plasma sputter coating apparatus are opened, start preheating cools down water flowing, successively opens mechanical pump and molecular pump,
It is evacuated to 1.0 × 10-4Pa;
Step（2）Argon gas is passed through, gas cylinder valve and flowmeter is adjusted, vacuum intracavity gas are adjusted, makes magnetic control target electric discharge build-up of luminance；
Step（3）Matrix surface plasma cleaning：Substrate bias are adjusted to -450V, with Ar Ions Bombardment matrix surfaces, remove base
Body surface impurity, cleans 20min;
Step（4）Substrate bias are adjusted to -100V, while opening two Cr targets, target current is set to 4A, deposits one layer of simple metal
Cr layers of bottoming；
Step（5）Substrate bias are adjusted to -75V, are passed through nitrogen, deposit CrN transition zones, and nitrogen stream is controlled by OEM systems
Amount, gradually decreases the Cr atom numbers of target as sputter, and the N content in coating gradually increases；
Step（6）Al targets and Mo targets are opened, Al target currents are gradually increased to 6A, and Mo target currents increase to specified numerical value, and four targets are complete
Portion is in opening, starts deposition CrMoAlN functional layers 60min, you can obtain Cr-CrN-CrMoAlN plural layers；
Step（7）After coating is completed and cooled down, coating chamber is deflated, and is sampled and is vacuumized；
Cr-CrN-CrMoAlN plural layers are finally obtained, the Cr joint thickness is 0.2 ~ 0.4 μm；The CrN transition zones
Thickness is 1.0 ~ 1.2 μm；The CrMoAlN functional layers thickness is 2.2 ~ 2.4 μm；The total coating thickness is 3.4 ~ 4 μm.
2. a kind of method of plural layers Combined with Performance Evaluation, it is characterised in that methods described is carried out as follows：
Step A）By H13 matrixes by non-equilibrium ion sputtering film coating technique deposit respectively Cr binder courses, CrN transition zones and
CrMoAlN functional layers are obtained Cr-CrN-CrMoAlN plural layers；
Setting device parameter is：Cr target currents 4A, Al target current 6A, Mo target current is set in 0 ~ 6A, bias -75V, Cr combination
Layer deposition 360s, CrN transition zones deposition 600s, CrMoAlN functional layers deposition 3600s；
Cr-CrN-CrMoAlN plural layers are obtained, the Cr joint thickness is 0.2 ~ 0.4 μm；The CrN transition region thicknesses
It is 1.0 ~ 1.2 μm；The CrMoAlN functional layers thickness is 2.2 ~ 2.4 μm；The total coating thickness is 3.4 ~ 4 μm；
Step B）Take step A）Prepared Cr-CrN-CrMoAlN plural layers carry out scratch experiment by multi-functional scratching instrument；
Wherein：Maximum load is 30N, and loading speed is 30mN/s, and cut length is 1mm；
Step C）Take step A）Prepared Cr-CrN-CrMoAlN plural layers are obtained by laser confocal scanning microscope
Film surface cut pattern assesses its binding ability.
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