CN106282939B - A kind of mold coating and its preparation method and application - Google Patents
A kind of mold coating and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of mold coating, ingredient is expressed as (V1‑a‑bAlaMeb)1‑xNx, the Me is Hf, Nb, Zr, Y or Ta；A, b, x are atom ratio, wherein 0.18≤a≤0.57,0.03≤b≤0.68,0.4≤x≤0.6.The present invention provides a kind of VAlMeN mold coatings for adding metallic element Me, and the mold coating with high rigidity, low-friction coefficient and high tenacity is prepared by ingredient, structure regulating.When the mold coating is used for aluminium alloy processing mold, frictional resistance when die casting is mutually moved with mold, the degree of engagement for improving die casting and mold on the one hand can be significantly reduced, casting accuracy is high；On the other hand, coating has preferable toughness, in repeatedly extrusion process, it is possible to reduce the generation of crackle improves the surface quality of aluminium alloy castings.
Description
Technical field
The invention belongs to field of ceramic coatings, be specifically related to a kind of quaternary nitride mold coating and preparation method thereof and
Using.
The measure of precision of background die casting is to influence the key factor of die casting precision and surface quality.With aluminium alloy pressure
Illustrate the importance of mold coating for casting.The fusion temperature of aluminium is 680 DEG C, and temperature when due to die casting is high, is added
Pressure when filling type is big so that aluminum alloy die-casting die often with cracking, cracking, form erosion, sticking, deform and fail, mould
It is very low to have service life.
Ti-Al-N coating { Li C, Paulitsch, et al.Thermal stability and oxidation
Resistance of Ti-Al-N coatings [J] .Surf.Coat.Technol., 2012,206:2954-2960 }, because of tool
Have higher hardness (about 35GPa), (500 DEG C~800 DEG C) oxidisability resistant to high temperatures and low thermal coefficient.It is commonly used for aluminium at present
The protective coating of alloy die cast mold acts on the erosion of cavity when can effectively mitigate molten aluminum high speed packed type chamber, reduces pressure
The problems such as casting the cracking of mold brought by thermal stress, cracking in cyclic process.
As the Chinese patent literature of Publication No. CN103567374A discloses a kind of coating material for aluminium die casting
The method expected and prepare the coating material.The coating material includes forming CrN binder course on the surface of the substrate, being arranged in
It TiAlN/CrN nanometer multilayer on the surface of CrN binder course and is arranged on the surface of TiAlN/CrN nanometer multilayer
TiAlN/CrSi (C) N nanometer multilayer.Preparation method includes: to form nitrogen in response to the gas access input nitrogen through chamber
Atmosphere, using Cr target, on the surface of the substrate by CrN binder course deposition；Using TiAl target and Cr target, by TiAlN/
CrN nano multilayer is deposited on the surface of deposited CrN binder course；TiAl target and CrSi target are reused by TiAlN/
CrSiN nanometer multilayer is deposited on the surface of TiAlN/CrN nanometer multilayer.
Although such coating material has excellent heat resistance and high-temperature stability, because of the higher { friction of its coefficient of friction
Coefficient > 0.5 }, pressure when filling type in addition is big, so that frictional resistance when aluminum alloy die casting is mutually moved with mold is big, into
And the degree of engagement of die casting and mold is influenced, the die casting precision of preparation is low.Secondly, the hardness of Ti-Al-N coating is high, it is tough
Property is low, and in aluminium alloy extruded forming process, inevitable coating can be poor due to deformability, and cracked.These crackles go out
It is existing, it will affect the surface quality of aluminum alloy die casting, the especially demanding deep-cavity thin-wall die casting of Surface Quality influences more
It is prominent.
Therefore, the novel die coating that inventing one kind can solve the above problems is one of the direction studied at present.
Summary of the invention
The present invention provides a kind of VAlMeN mold coatings for adding metallic element Me, pass through ingredient, structure regulating, preparation
Obtain the mold coating with high rigidity, low-friction coefficient and high tenacity.The mold coating is used for aluminium alloy processing mold
When, frictional resistance when die casting is mutually moved with mold on the one hand can be significantly reduced, raising die casting is engaged with mold
Degree, casting accuracy are high；On the other hand, coating has preferable toughness, in repeatedly extrusion process, it is possible to reduce crackle
Generation, improve the surface quality of aluminium alloy castings.
A kind of mold coating, ingredient are expressed as (V1-a-bAla Meb)1-xNx, the Me is Hf (hafnium), Nb (niobium), Zr
(zirconium), Y (yttrium) or Ta (tantalum)；
A, b, x are atom ratio, wherein 0.18≤a≤0.57,0.03≤b≤0.68,0.4≤x≤0.6.
These elements such as Hf, Nb, Zr, Y, Ta, atomic radius is larger, and to be formed in view of these elements are reacted with nitrogen
The lattice constant of nitride (such as TaN, ZrN etc.) is greater than c-AlN, when part Ta substitutes Al, can cause AlN distortion of lattice, from
And the potential barrier that c-AlN changes to buergerite AlN is increased, so that still being kept higher after the annealing of V-Al-Me-N mold coating high-temp
Hardness.
Preferably, in the mold coating, 0.2≤a≤0.35,0.5≤b≤0.65,0.45≤x≤0.55.
Preferably, the Me is Ta, Hf or Zr；Further preferably Ta or Zr.
Most preferably, the mold coating, Me Ta, a=0.24, b=0.57, x=0.48；Me is Zr, a=0.25, b
=0.57, x=0.49.
From growth structure, i.e., from Cross Section Morphology, the mold coating structure is fine and close.Preferably, described
Mold coating be in the form of a column crystal structure, column crystal die width is 70~100nm, and average grain diameter is 80~100nm, and each column
The length of shape crystalline substance is more than 400nm, draw ratio >=5 of column crystal, and micro chink or existing is not present between two neighboring column crystal
Micro chink width is in 2~3nm.
It is tested within the scope of 2 θ=35 °~45 ° of the angle of diffraction using X-ray diffraction method, preferably, the mold
Coating is NaCl type crystal structure, and V-Al-Me-N exists in a manner of being dissolved, at 2 θ=41.6 °~42.8 ° of the angle of diffraction, out
Existing (200) diffraction maximum, and/or at 2 θ=36.8 °~37.8 ° of the angle of diffraction, there is (111) diffraction maximum.Further preferably, spreading out
When 2 θ=35 °~45 ° of firing angle, only there is (200) diffraction maximum in the mold coating, diffraction maximum appearance position be 2 θ=
42.4°。
The structure feature of prepares coating of the present invention determine its as mold coating in high temperature extrusion aluminium alloy castings still
It is able to maintain higher hardness and low coefficient of friction, and the anti-crack effect of coating is preferable when repeating to squeeze.In VAlN coating
On the basis of by addition relatively large radius element Hf, Nb, Zr, Y, Ta, by taking Ta element as an example, the VAlN coating high-temp without Ta
Hardness only has 14~20GPa after (700 DEG C) annealing.After Ta is added, when high temperature, can form the higher TaN of Composite hardness
(~32GPa), and when causing VAlTaN coating high-temp integral hardness raising.Secondly, in coating contain suitable Ta, compared with
Under high sputtering power, V, Al, N nuclear energy that the Ta atomic ratio sputtered sputters are higher by about 20eV, these are a small amount of high
The Ta atom of energy and the Ar atom of rebound increase the dynamics bombarded when film forming film surface together, so that surface atom moves
Shifting rate, diffusion increase, conducive to the densification of coating.Experiment discovery, coating densification, mechanical behavior under high temperature (such as coating hardness,
Fretting wear etc.) have and significantly improves.Secondly, the toughness of coating is improved after addition metal Ta.So that coating has
Can also draw up the generation of crackle while certain degree of hardness in repeating extrusion process, improve the surface matter of extruding aluminium alloy casting
Amount.
The present invention also provides the preparation method of the mold coating, the preparation method that can be used includes magnetron sputtering
Method, vacuum evaporation, ion beam assisted depositing etc.；
Preferably, magnetron sputtering method is used in the present invention, by using radio frequency and DC power supply collective effect in Me
The mode of target, which makes the Me atom energy with higher sputtered, and (energy is about 100eV, than sputter gas Ar atom
It is higher by 20eV).On the one hand the Me atom of these high energy is easy to react to form Me nitride with nitrogen, then mutual with VAlN again
Solid solution forms the solid solution with NaCl type crystal structure.On the other hand, the Me atom of high energy and the Ar atom of rebound increase together
The dynamics that film surface is bombarded when having added film forming, so that the mobility of surface atom, diffusion increase, conducive to the densification of coating
Change.To which to prepare high-temperature oxidation resistance, low-friction coefficient, the preferable specific structure of VAlMeN mold coating institute of toughness is provided
Basis；And this method is easy to operate, production cost is low, is convenient for industrialization large-scale production.
Specific step is as follows:
(1) target and substrate are installed；
The target is Me target and VAl alloys target；
(2) coating deposits: in vacuum chamber, Me target is connected with the DC power supply of RF assistance, VAl alloys target and DC power supply
Be connected, in the presence of working gas nitrogen and argon gas, by reactive magnetron sputtering method on heating the substrate at least one
It is deposited in a main surface, obtains the wear-resistant coating；
Rf frequency >=60MHz, Me target power density are 3.2~5.1W/cm2；Vananum target power supply power density is
1.5~3.1W/cm2。
The present invention uses VAl alloys target and Me target for target, and two targets are jointly and N2Reactive sputtering and form mold coating.
Preferably, the baseplate material is selected from step (1): hard alloy, ceramics, due to substrate material pair
The Effect on Mechanical Properties very little of VAlMeN coating, as long as therefore the substrate can be suitable as with the binding force of the coating greater than 20N
The substrate of the VAlMeN coating.
The substrate is cleaned by chemical cleaning and/or plasma glow；
The chemical cleaning are as follows: by substrate or die workpiece be sequentially placed into concentration be 30%~60% cleanser solution,
It is saturated Na2CO3Solution, dehydrated alcohol, is respectively cleaned by ultrasonic 10~20min in deionized water at acetone, then temperature be 80 DEG C~
1~2h of forced air drying in 100 DEG C of drying box, or use purity for 99.99% high-purity N2Drying.
The plasma glow cleaning are as follows: the substrate after chemical cleaning is put into rotatable rack in vacuum chamber
On, 10~20min is etched to substrate using the plasma that argon gas generates, so that the hydrone of substrate surface attachment, gas point
Son or dust particale are fallen by complete bombardment.
Preferably, in vacuum chamber, back end vacuum is evacuated to lower than 4.5 × 10 in advance in step (2)-5Pa；Substrate heating
Temperature is 300~550 DEG C.
Preferably, in step (2), the flow-rate ratio of nitrogen and argon gas is 1/5~1/2, keep deposition pressure be 0.2~
1Pa；Further preferably, deposition pressure is 0.2~0.8Pa.
Preferably, in step (2), in deposition process, substrate can not biasing, directly hanging setting can also be in base
Application -20V~-30V back bias voltage on plate.
Preferably, the deposition rate of coating is 7~25nm/min, further preferably 15~20nm/ in step (2)
min。
The invention also discloses a kind of aluminium alloy processing mold, major face has the mold coating, coating layer thickness 2
~10 μm, Coating Surface Roughness Ra is 2.6~7.7nm；The surface of the degree of roughness be conducive to the coating have at high temperature compared with
Low coefficient of friction.
Preferably, the V-Al-Ta-N mold conductivity is in 600~3000 μ Ω .cm, further preferably
1000~1800 μ Ω .cm.
Compared with prior art, the present invention has the advantage that
(1) present invention develops a kind of VAlMeN mold coating, and coating hardness after 700 DEG C of ambient anneals is 30GPa,
To the Al of diameter 6mm2O3Under the active force of mill ball 2N, the wear rate of coating is~10-15m3/ Nm the order of magnitude, coefficient of friction
It is 0.3~0.5, frictional resistance when aluminium alloy and mold extruding can be significantly reduced.
(2) mold coating prepared by the present invention, moulding index are 0.52, coating can be reduced in repeating extrusion process and split
The generation of line improves the surface quality of aluminium alloy castings.
Detailed description of the invention
Fig. 1 is the Cross Section Morphology photo of VAlTaN coating prepared by embodiment 3, wherein (a), (b) is SEM photograph, (c)
It is (d) TEM high-resolution photo, the scale of pattern successively reduces from (a)~(d) for TEM photo；
Fig. 2 is the surface A FM pattern photo of VAlTaN coating prepared by embodiment 3；
The XRD spectrum for the VAlTaN coating that Fig. 3 is prepared respectively for embodiment 1,3,6, (a) embodiment 1, embodiment 3 (b),
(c) embodiment 6；
Fig. 4 is the coefficient of friction figure for the VAlTaN coating that embodiment 1,3,6 is prepared respectively, and (a) embodiment 1 (b) is implemented
Example 3, (c) embodiment 6；
Fig. 5 is the frictional wear experiment figure of VAlTaN coating prepared by embodiment 3；
The vickers indentation figure for the V-Al-Ta-N coating that Fig. 6 is prepared respectively for embodiment 1,2,3 and 6, (a) embodiment 1,
(b) embodiment 2, (c) embodiment 6, (d) embodiment 3.
Specific embodiment
Below in conjunction with Figure of description and embodiment, the invention will be further described:
Examples 1 to 6
Select VAl alloys target and metal Ta target be target source by with N2React double target co-sputtering shape on tungsten carbide substrate
At VAlTaN coating.
Implement 7~10
Select VAl alloys target and metal Zr target be target source by with N2React double target co-sputtering shape on tungsten carbide substrate
At VAlZrN coating.
The following are specific steps:
(1) target is installed, substrate is installed again after first passing through chemical cleaning and plasma glow cleaning in advance.
(2) VAlTaN or VAlZrN coating is deposited using magnetic control sputtering system, VAl target is connected with DC power supply, Ta target
Or Zr target is connected with the DC power supply of RF assistance.When back end vacuum is lower than 4.5 × 10-5After Pa, it is passed through N2With Ar gas and adjust
The flow-rate ratio of the two is 1/3, and holding deposition pressure is that 0.5Pa is deposited to obtain VAlTaN by deposition parameter shown in table 1
Or VAlZrN coating.
See Table 1 for details for magnetron sputtering deposition parameter in Examples 1 to 10.
Table 1
After deposition, sample is taken out, the structure of the mold coating of embodiment preparation is assessed using following test method
Feature and mechanical property.
Coating structure and mechanical property characterization:
The detailed mark for having carried out ingredient, pattern and mechanical property to the VAlTaN coating being prepared below is levied, to preparation
ValZrN only carried out the characterization of mechanical property.
Composition measurement:
The VAlTaN coating of preparation uses EDAX energy matched with Hitachi S4800 field emission scanning electron microscope
Spectrometer carries out composition measurement, and configuration EDAX Si (Li) probe is calibrated by ZAF, and each sample is selected an area and is not less than
40mm2Region measures the average value of its ingredient.
Morphology observation:
Using Hitachi S4800 type field emission scanning electron microscope (ejecting gun voltage 4kV) to the VAlTaN of preparation
The surface of coating, section are characterized, and are rubbed using FEI QUANTA 250FEG type field emission scanning electron microscope to it
Pattern after abrasion is characterized.
The sight of light field high-resolution pattern has been carried out to sample segment using FEI Tecnai F20 type transmission electron microscope
It examines, acceleration voltage 200kV.
Using contact mode, VAlTaN coating surface profile is carried out using CETR AIST-NT type atomic force microscope
Characterization.
Coating cross sections pattern prepared by embodiment 3 is as shown in Figure 1, can be seen that coating is in the form of a column crystals growth structure from SEM
{ shown in Fig. 1 (a) }, amplifying its shape appearance figure can be seen that { shown in Fig. 1 (b) }, not deposit on SEM scale between adjacent two column crystal
In micro chink.It is observed under TEM bright field image, column crystal width is about 70~100nm, and the length of each column crystal is more than 400nm,
There is no slight gap { shown in Fig. 1 (c) } between adjacent column crystalline substance, coating is fine and close.Further applied by TEM High Resolution Observations
Layer { shown in Fig. 1 (d) }, can significantly see that lattice fringe, grain boundaries be not defective.
The embodiment 3 preparation coating surface AFM pattern photo it is as shown in Figure 2, it can be seen that its grain size be 70~
100nm { shown in Fig. 2 (a) }, surface roughness Ra are the nm of 2.6nm~7.7, coating surface smoother { shown in Fig. 2 (b) }.
Crystal Structure:
Using use the D8Advance type polycrystal X ray diffractometer of German Brooker company production to VAlTaN coating into
The characterization of row crystal structure, using Cu-K alpha ray, 30 ° -50 ° of scanning range, 0.02 ° of step-length.
Coating mechanical property characterization:
The hardness of VAlTaN or VAlZrN coating is measured using the NANO G200 type nano-hardness tester of MTS company, is moulded
Shape and elastic deformation, wherein pressure head is Berkovich, and compression distance is the 10% of coating layer thickness, certain using compression distance,
The mode of varying load obtains load-displacement curves.Plasticity and elastic deformation are obtained according to load-displacement curves, utilizes formula
(1) computational plasticity index:
Wherein δHFor plasticity index, εpFor plastic deformation, εeFor elastic deformation, ε=εp+εe.Attached drawing 6 is embodiment 1, real
Apply example 2, embodiment 6, the main part pattern of the Vickers indentation of coating prepared by embodiment 3 in the secure execution mode (sem.It can be seen that implementing
There is " returning " font crackle in the impression of example 1 and embodiment 2, and annular crack extends to outside impression, and oriented in impression quadrangle
Radial crackle, coating poor toughness, in conjunction with table 2 it can be seen that its moulding index point is than being 0.28 He is presented in external radiation
0.35.The toughness of embodiment 6 makes moderate progress compared with Examples 1 and 2, but impression quadrangle, still with the presence of radial crackle, moulding refers to
Number is 0.45.Coating toughness prepared by embodiment 3 is preferable, and impression underbead crack quantity is obviously less, and quadrangle radial crack is more
Refinement is small, and crack length is also shorter, and moulding index is 0.52.
The friction and wear behavior test of VAlTaN or VAlZrN coating is tested in CETR UMT-3 type multifunction friction wear
It is carried out on machine.Antithesis ball is the Al of diameter 6mm2O3Ball, load 2N, friction velocity 5cm/s.
The structure composition and Mechanical Characteristics for the mold coating that Examples 1 to 10 is prepared respectively are as shown in table 2.
Table 2
From the results shown in Table 2, the VAlTaN coating that prepared by embodiment 3 still has height after 700 DEG C of high temperature annealing
Hardness 30GPa, when as mold coating, coefficient of friction 0.3, compare currently used TiAlN mold coating frictional resistance
Reduce 2~3 times, wear rate is down to 1.6 × 10-15m3/ N.m, the toughness of coating also improve 2.5 times compared with TiAlN.Similarly,
VAlZrN coating also shows preferable mechanical property.As coating hardness is 28GPa, friction system after 9,700 DEG C of embodiment annealing
Number is 0.3, and plasticity index 0.46, wear rate is down to 4.6 × 10-15m3/N.m。
Fig. 3 is embodiment 1, embodiment 3, the XRD spectra for the VAlTaN coating that embodiment 6 is prepared respectively.In conjunction with table 2
The mechanical property of test can be seen that when preparation coating mainly along (111) high preferred orientation growth when, coating hardness it is lower (H≤
20GPa).When the coating of preparation is mainly grown along (200) high preferred orientation, coating hardness is relatively high (H=25~30GPa).Together
Relationship between the structure feature and performance of sample, still has in VAlZrN coating.
Fig. 5 and Fig. 6 is the frictional wear experiment result that VAlTaN coating carries out after 700 DEG C of annealing.It can from Fig. 5
The lower coating coefficient of friction that out prepared by embodiment 3 is 0.3, when coating Ta too high levels or too low, all higher (reality of coefficient of friction
Apply example 6 and embodiment 1).Further from coating polishing scratch prepared by embodiment 3, find its polishing scratch smoother, mill road compared with
Narrow { Fig. 6 (a) and 6 (b) }, coating is more wear-resisting, and wear rate is low { Fig. 6 (c) }.What VAlZrN coating carried out after 700 DEG C of annealing
Fretting wear also has similar as a result, specific be shown in Table 2.
All references mentioned in the present invention is incorporated herein by reference, independent just as each document
It is incorporated as with reference to such.In addition, it should also be understood that, after having read the above content of description of the invention, those skilled in the art
The present invention can be made various changes or modifications, these equivalent technical solutions equally fall within the application the appended claims institute
The range of restriction.
Claims (5)
1. a kind of aluminium alloy processing mold mold coating, which is characterized in that ingredient is expressed as (V1-a-bAlaMeb)1-xNx, described
Me be Hf, Nb, Zr, Y or Ta；
A, b, x are atom ratio, wherein 0.2≤a≤0.35,0.5≤b≤0.65,0.45≤x≤0.55；
The mold coating is in the form of a column crystal structure, and column crystal die width is 70~100nm, and average grain diameter is 80~100nm,
And the length of each column crystal is more than 400nm, draw ratio >=5 of column crystal, and micro chink is not present between two neighboring column crystal
Or existing micro chink width, in 2~3nm, coating structure is fine and close；
The mold coating is NaCl type crystal structure, and V-Al-Me-N exists in a manner of being dissolved；
At 2 θ=35 °~45 ° of the angle of diffraction, only there is (200) diffraction maximum in the mold coating.
2. a kind of preparation method of mold coating according to claim 1, which is characterized in that steps are as follows:
(1) target and substrate are installed；
The target is Me target and VAl alloys target；
(2) coating deposits: in vacuum chamber, Me target is connected with the DC power supply of RF assistance, VAl alloys target and DC power supply phase
Even, in the presence of working gas nitrogen and argon gas, pass through at least one of reactive magnetron sputtering method on heating the substrate
It is deposited in main surface, obtains the mold coating；
Rf frequency >=60MHz, Me target power density are 3.2~5.1W/cm2；Vananum target power supply power density be 1.5~
3.1W/cm2。
3. the preparation method of mold coating according to claim 2, which is characterized in that in step (2), in vacuum chamber, back
Bottom vacuum is lower than 4.5 × 10-5Pa；Substrate heating temperature is 300~550 DEG C.
4. the preparation method of mold coating according to claim 2, which is characterized in that in step (2), nitrogen and argon gas
Flow-rate ratio is 1/5~1/2, and holding deposition pressure is 0.2~1Pa.
5. a kind of aluminium alloy processing mold, the with good grounds mold coating described in claim 1 of major face, feature exist
In coating layer thickness is 2~10 μm, and Coating Surface Roughness Ra is 2.6~7.7nm.
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| CN103567374A (en) * | 2012-08-07 | 2014-02-12 | 现代自动车株式会社 | Coating material for aluminum die casting mold and method of manufacturing the coating material |
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