CN206828625U - TiCN/CrCN nano-multilayer films - Google Patents
TiCN/CrCN nano-multilayer films Download PDFInfo
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- CN206828625U CN206828625U CN201720512825.0U CN201720512825U CN206828625U CN 206828625 U CN206828625 U CN 206828625U CN 201720512825 U CN201720512825 U CN 201720512825U CN 206828625 U CN206828625 U CN 206828625U
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Abstract
The utility model discloses a kind of TiCN/CrCN nano-multilayer films, belong to thin film materials art.The utility model uses multi sphere ion plating technology, deposited metal transition zone Ti first and ceramic interlayer TiN, last alternating deposit TiCN and CrCN films on hard alloy substrate, is in modulation period：TiCN is 15 20nm, when CrCN is 5 10nm, realizes superlattice structure.At 1.5 4 μm, hardness can be coated on the surface of cutting tool, improve its service behaviour, extend cutting-tool's used life the overall film thickness up to 39.03GPa, adhesive force up to 45.32N, friction factor minimum 0.137, and excellent corrosion resistance.
Description
Technical field
The utility model belongs to thin film materials art, is related to a kind of ceramic-like film and preparation method thereof, particularly one kind
TiCN/CrCN nano-multilayer films with high rigidity, high-wearing feature and excellent corrosion resistance, it is possible to achieve the surface of cutting tool
It is modified.
Background technology
With the high speed development of modern mechanical processing industry, difficult-to-machine material is more and more, therefore Cutting Process is particularly high
The techniques such as fast cutting, dry cutting propose more stringent requirement to cutting tool, such as high cutting speed, high reliability, length
Life-span, high-precision and good cutting controlling.As tool surface is coated on, the protectiveness of significant surfaces modifying function is played
The film such as thin-film material, traditional single group member TiN, CrN is difficult in adapt to the requirement of modern industrial technology, comprehensive in order to improve its
Can, ganoine thin film develops towards multiple stratification, diversification direction.
21 century is referred to as the century of nanosecond science and technology, size nanometer scale nanometer multilayer membrane material due to only
Special physicochemical characteristics, causes the more and more extensive concern of people.Research shows that nano-multilayer film has bigger than monofilm
Hardness much, and its inoxidizability, excellent wear-resisting property, therefore be a kind of preferable novel film material.Exist from Koehler
《Physical Review Letters》On deliver " Attempt to design a strong solid " (《Physical comment is fast
Report》, " attempt design firm solid "), after the super-hardness effect for proposing hetero-junctions super crystal lattice material, novel nano multi-layer film material
Quick development is obtained.
Nano-multilayer film is formed by the different monolayer material alternating deposit of two kinds or two or more structures or composition
Multilayer material, in nanometer scale, the interface of interlayer can prevent column crystal and coarse grain for the thickness of each individual layer
Growth, crystal grain thinning, plastic deformation ability is improved, there is inhibition to dislocation movement by slip, suppress the formation and extension of crackle, carry
The high intensity and impact resistance of film layer, referring to Dahotre N B et al. " application of the nano coating in automotive engine system "《Table
Face and coating technology》2005,194(1):58-67(Dahotre N B,Nayak S.Nanocoatings for engine
application[J].Surface&Coatings Technology,2005,194(1):58-67)。
In addition, although multi sphere ion plating technology is one of conventional film plating process of nanometer multilayer film preparation, but use at present
The technology prepares nano-multilayer film generally using the method for alternately continually opening and stopping multiple arc target, not only power-consuming, also makes whole
Individual coating process stability and security are poor, it is most important that, the big amount of molten drops that the moment that each target is opened ejects compared with
It is more so that bulky grain increase in film, serious has influence on film quality.
The content of the invention
In order to solve deficiency of the prior art, it is resistance to that the utility model aims to provide a kind of high rigidity, low friction coefficient, height
New TiCN/CrCN nanometer multilayers membrane material of mill property and corrosion resistance and preparation method thereof, preferably to lift cutting tool
Service behaviour, extend its service life.
In order to realize above-mentioned function, the utility model will use following technical scheme：
A kind of TiCN/CrCN nano-multilayer films, it is characterised in that deposit compound transition zone first, compound transition zone includes Ti
The TiCN/CrCN films of intermediate metal and TiN ceramic interlayers, then alternating deposit nanoscale, it is 15- in TiCN
Film realizes superlattice structure under the conditions of the modulation period that 20nm, CrCN are 5-10nm, and nano-multilayer film, which produces, causes hard phenomenon.This
Kind of overall film thickness is at 1.5-4 μm, and hardness is up to 39.03GPa, and adhesive force is up to 45.32N, friction factor minimum 0.137,
And 72h salt spray tests examine its excellent corrosion resistance.
The utility model uses multi-arc ion coating embrane method, and the multi-Arc Ion Plating used during plated film is by coating chamber, first
Arc source, the second arc source, rotating unit, air admission unit, heating source, vavuum pump, striking power supply and pulsed bias power supply composition, its
In, inside cavities wall is provided with the first arc source and the second arc source being arranged oppositely, and is provided with rotating unit in the middle part of cavity, is set on cavity
There is the tracheae being connected respectively with vavuum pump, air admission unit, wherein, air admission unit includes outside gas cylinder and is connected with outside gas cylinder
Logical tracheae.Rotating unit includes the first arc and the second arc, rotating base, and the first arc and the second arc are consolidated
Dingan County forms nearly cylindrical structure on rotating base.
First arc source described in the utility model is provided with Ti targets, and the second arc source is provided with Cr targets, and matrix is separately fixed at
One arc lateral wall and the second arc lateral wall, can weld on the first arc and the second arc some small columns with
It is easy to the suspension and fixation of matrix.First arc and the second arc board size are determined by coating chamber space size, it is ensured that plating
When matrix is turned to towards the position of the target of wherein side in membrane process, the first arc and the second arc can block another
The arc light of side target, matrix are rotated successively by the area of the arc light of Ti targets and Cr targets covering with outside the first arc with the second arc
Domain, to realize TiCN and CrCN alternating deposit.
A kind of preparation method of TiCN/CrCN nano-multilayer films, it is characterised in that prepared, wrapped using multi-arc ion coating method
Include following steps：
(1) use purity for 99.99% each two pieces of Ti targets and Cr targets, to placement in the coating chamber of plated film.
(2) the first arc and the second arc are fixedly mounted on rotating base and form nearly cylindrical structure.
(3) matrix selects hard alloy steel, is cleaned by ultrasonic through deionized water, acetone and each 10min of alcoholic solution, removes table
Face greasy dirt, coating chamber is put into after drying, be fixed on the first arc and the second arc lateral wall.
(4) coating chamber air pressure is evacuated to 1.5 × 10-2Below Pa, opens heating tube, and temperature is 280-350 DEG C.Biased in height
Under -700V (40%) fill Ar gas, flow 160-200sccm, Ar is carried out to matrix surface+Aura cleans, and coating chamber air pressure is
1.7-2.2Pa。
(5) sample stage rotating switch, speed 5-50HZ are opened.Open Ti targets, arc current 60-80A, deposition
Transition zone Ti, Ar gas continues to be passed through as protective gas, flow 30-60sccm, enters first under high bias -450V (40%)
Row Ti+5-10min is bombarded, then depositing Ti transition zone 10-15mi, coating chamber air pressure are under normal bias -200V (40%)
0.2-0.4Pa。
(6) ceramic interlayer TiN is deposited：It is filled with N2As reacting gas, flow 120-150sccm, Ti targets are kept to open
Open, the depositing TiN transition zone under bias -200V (dutycycle 40%), time 10-15min.
(7) depositing Ti CN/CrCN nano-multilayer films：Ti targets and Cr targets are opened simultaneously, arc current scope is：Ti targets 60-
80A, Cr target 55-70A.It is filled with reacting gas N2And C2H2, flow controlled in 80-100sccm, the first arc and the second arc
Shape plate speed is 5-50HZ, and matrix towards Ti targets and Cr targets and circulates successively and carries out this process, realizes TiCN/CrCN nanometers
The preparation of multilayer film, time 2-3h.
The utility model uses above-mentioned technical method, has the following advantages that：
(1) the utility model using high rigidity TiCN and have high-wearing feature concurrently and the CrCN of excellent anticorrosive is two kinds thin
Membrane material, nano-multilayer film is prepared, propose more suitable scope modulation period of two kinds of materials：TiCN is 15-20nm, and CrCN is
5-10nm, i.e., using TiCN as modulating layer main component, ensure nanometer multilayer film hardness, while TiCN hardened layers and frictional behaviour
Excellent CrCN film alternating deposits, to reduce interfacial shearing stress, lift wearability and corrosion resistance.
(2) the utility model TiCN/CrCN nano-multilayer films obtained under the conditions of above-mentioned modulation period, combine two
The advantages of kind thin-film material, microhardness belongs to superhard thin film, and film base junction up to 39.03GPa, adhesive force up to 45.32N
With joint efforts preferably, friction factor minimum 0.137, friction and wear behavior is excellent, and in 72h salt spray tests, film performance is stable, shows
Excellent corrosion resistance is shown.Compared with preparing the single TiCN or CrCN films of same thickness, TiCN/CrCN nano-multilayer films
Combination property more preferably, the properties test result such as following table of three kinds of thin-film materials.
(3) multi sphere ion plating technology used by the utility model, compared with other PVD film plating process, there is ionization level
High (more than 90%), the advantages that film forming speed is fast, and cost is relatively low, and intermembranous adhesion is good and easily operated, be most suitable application
In the PVD film plating process of high-volume actual production, and the utility model be under nanoscale alternating deposit TiCN with
CrCN, it is not easy to form during traditional plating films of multi-arc ion plating the bulk column crystal occurred so that membrane structure is finer and close, ensures
Film has preferable mechanical property and a friction and wear behavior.
(4) the utility model is improved to existing multi-arc ion plating equipment, with the first arc of two pieces of semi-cylindricals
Substitute original sample hanger with the second arc, matrix is as the first arc and the second arc rotate and circulate through Ti
The arc light scope of target and Cr targets, semicircular arc plate use stainless steel, and diameter is approximately equal to central rotating disk, ensure target-substrate distance with using
Target-substrate distance during hanger fixing base is identical, and semicircular arc plate is highly about the top arc target height, ensures its screening to arc light
Keep off effect.During TiCN/CrCN nano-multilayer films are prepared, the first arc and the second arc when depositing wherein thin film
Shape plate can block the arc light of opposite target completely.The document of nano-multilayer film is being prepared using multi-arc ion coating method at present
In, most common method is that control different materials target is alternately opened and stopped realizing the deposition of nano-multilayer film, this practicality
New the first arc and the second arc plate structure as a result of semi-cylindrical so that all targets can be beaten simultaneously for a long time
Open, avoid Ti targets and the alternately continually start and stop of Cr targets.The not only more power saving of this method, also makes whole coating process more steady
Fixed, safety, it is most important that the big amount of molten drops that the moment that each target is opened ejects can be substantially reduced so that big in film
Particle is reduced, and high-quality thin film is prepared to ensure.
(5) it is very convenient to the modulation period of TiCN/CrCN nano thin-films and the adjustment of modulation ratio in the utility model：Adjust
The frequency that cycle (i.e. monolayer film thickness) processed is only rotated by changing matrix with the first arc and the second arc can be real
Existing, rotational frequency scope be 5-50HZ in the utility model, and rotational frequency is bigger, matrix pass through each target arc light region when
Between it is shorter, individual layer TiCN and CrCN film thickness is smaller, i.e. modulation period is smaller.Modulation ratio (i.e. individual layer TiCN and CrCN films
Thickness ratio) it can be adjusted by changing Ti targets or Cr targets arc current, if for example, Cr target arc currents are constant, Ti target arc currents
Bigger, TiCN sedimentation rates are faster, and TiCN is bigger than the modulation ratio of CrCN film thickness within a modulation period, and this practicality is new
Arc current scope is in type：Ti targets 60-80A, Cr target 55-70A.And if replacing start and stop using different targets in many documents
Film plating process, if wanting to adjust modulation period and modulation ratio, need to take considerable time that film is carried out from level to level to plated film flow
Time sets.
TiCN and CrCN is the Typical Representative of polynary superhard thin film.In appropriate amount incorporation C element can improve binary TiN and
The performance of CrN films.In TiCN, C atomic components substitute the N atoms of Ti-N keys, the stronger Ti-C keys of generation bond energy, and cause
TiCN produces distortion of lattice so that its hardness is obviously improved；C element in CrCN is mainly with sp2C-C key-shapeds formula is present, in rotten
Pureed structure, this plays highly important lubrication in process of friction and wear, it is possible to reduce adhesive surface phenomenon, reduces boundary
The shear stress in face, therefore CrCN anti-wear performance is excellent, in addition, CrCN excellent anti-corrosion performance, extensively using Yu Haiyang
Under environment in the corrosion resistance research of component of machine.
TiN systems and the lattice constant and similar thermal expansion coefficient of CrN systems coating, and there is high rigidity and high-wearing feature respectively
Advantage, in cutter or TiCN and the CrCN film of metal surface alternating deposit nanoscale, in suitable modulation period and tune
Under the conditions of system ratio, the combination of two kinds of thin-film material advantages will be realized, the splendid TiCN/CrCN nanometers of combination property can be prepared
Multilayer film.
Brief description of the drawings
Accompanying drawing 1 is TiCN/CrCN nano-multilayer film structural representations.
Accompanying drawing 2 is the structural representation of plating films of multi-arc ion plating equipment.
Accompanying drawing 3 is the microscopic cross figure of embodiment one.
Accompanying drawing 4 is the micro-hardness testing interface in embodiment one.
The friction factor curve for sample in embodiment one, five, six that accompanying drawing 5 represents.
Wherein, 1 is matrix, and 2 be Ti transition zones, and 3 be TiN transition zones, and 4 be TiCN layer, and 5 be CrCN layers.Wherein, 6 be plating
Film room, 7 be Ti targets, and 8 be Cr targets, and 9 be rotating unit, and 10 be heating source, and 11 be vavuum pump, and 12 be striking power supply, and 13 be pulse
Grid bias power supply, 14 be air admission unit.
Embodiment
Below in conjunction with the accompanying drawings and embodiment the utility model is described in further detail：
As shown in figure 1, a kind of TiCN/CrCN nano-multilayer films, deposit compound transition zone, including Ti intermediate metals first
The TiCN/CrCN films of 2 and TiN ceramic interlayers 3, then alternating deposit nanoscale, it is 15-20nm, CrCN in TiCN layer 4
Layer 5 realizes superlattice structure for film under the conditions of 5-10nm modulation period, and nano-multilayer film, which produces, causes hard phenomenon.This film
Gross thickness is at 1.5-4 μm, and hardness is up to 39.03GPa, and adhesive force is up to 45.32N, friction factor minimum 0.137, and 72h salt
Its excellent corrosion resistance of mist experimental examination.
As shown in Figure 2, in coating chamber 6, to placing two pure Ti targets 7 and two pure Cr targets 8；Cavity center is with partly
The cylindrical arc of stainless steel first and the second arc substitute pivoted frame, are fixed on the rotating disk of bottom, form rotating unit 9,
First arc and the second arc plate surface fix hard alloy substrate, matrix concomitant rotation and circulate through Ti targets and Cr targets；
Before deposition film, heating source 10 is opened, heating source can be heating tube, as required by cavity is evacuated to plated film by vavuum pump 11
Vacuum；During plated film, open striking power supply 12, form arc current, pulsed bias power supply 13 provides substrate negative voltage, gas by
Tracheae in gas cell 14 is passed through, in substrate deposit into film.
Embodiment one
Technological parameter is：300 DEG C of temperature, Ti target currents 75A, Cr target current 55A, matrix rotation frequencies 50HZ, during deposition
Between 120min.TiCN thickness is about that 19nmCrCN thickness is about 9nm in obtained TiCN/CrCN nano-multilayer films, total film thickness
About 2.6 μm of degree.Film hardness is 39.03GPa, adhesive force 45.32N, friction factor 0.214, the examination of salt fog corrosion resistance
Test 72h and have no hickie and rusty stain.
Embodiment two
Technological parameter is：300 DEG C of temperature, Ti target currents 75A, Cr target current 55A, matrix rotation frequencies 20HZ, during deposition
Between 120min.TiCN thickness is about that 38nm CrCN thickness is about 20nm in obtained TiCN/CrCN nano-multilayer films, and film is total
Thickness is about 2.4 μm.Film hardness is 36.12GPa, adhesive force 40.25N, friction factor 0.481, salt fog corrosion resistance
There is hickie after experiment 60h.
Embodiment three
Technological parameter is：280 DEG C of temperature, Ti target currents 65A, Cr target current 55A, matrix rotation frequencies 40HZ, during deposition
Between 120min.TiCN thickness is about 16nm in obtained TiCN/CrCN nano-multilayer films, and CrCN thickness is about 11nm, and film is total
Thickness is about 1.9 μm.Film hardness is 32.46GPa, adhesive force 43.84N, friction factor 0.137, salt fog corrosion resistance
Experiment 72h has no hickie and rusty stain.
Example IV
Technological parameter is：320 DEG C of temperature, Ti target currents 70A, Cr target current 65A, matrix rotation frequencies 50HZ, is obtained
TiCN thickness is about 23nm in TiCN/CrCN nano-multilayer films, and CrCN thickness about 15nm, overall film thickness is about 2.9 μm.Film
Hardness is 29.03GPa, adhesive force 38.61N, friction factor 0.183, and salt fog corrosion resistance test 72h has no hickie and rust
Mark.
The combination property of TiCN/CrCN nano-multilayer films is together decided on by modulation period and modulation ratio, in Examples 1 and 2
In, TiCN and CrCN modulation are bigger, i.e. film is based on TiCN strengthening layers, therefore hardness is higher than embodiment 3 and 4；But implement
CrCN compositions in example 1 and 2 are less, therefore friction and wear behavior is less than embodiment 3 and 4.In addition, mistake modulation period of embodiment 2
Greatly, only it is the superposition of multi-player super-hard film, fails to form superlattice structure, film is not fine and close enough, and intermembranous dislocation can not with sliding
Access effective suppression, therefore friction factor is apparently higher than other 3 groups of samples, and corrosion resistance is general.In general, embodiment
Multilayer film properties in 1 and 3 are optimal, i.e., TiCN/CrCN nano-multilayer films of the present utility model optimum modulation period and tune
Make than condition and be：TiCN is 15-20nm, CrCN 5-10nm.
Embodiment five
Ti targets are only opened, TiCN films is prepared, is compared research.Technological parameter is：300 DEG C of Ti target current 75A of temperature,
Bias as -200V (dutycycle 40%), N2Flow 100sccm, C2H2Flow 100sccm, sedimentation time 240min.Obtain
TiCN overall film thickness is about 3.1 μm.Film hardness is 32.56GPa, adhesive force 44.68N, friction factor 0.325, salt
There is hickie after mist corrosion resistance test 48h.
Embodiment six
Cr targets are only opened, CrCN films is prepared, is compared research.Technological parameter is：300 DEG C of temperature, Cr target currents
55A, bias as -200V (dutycycle 40%), N2Flow 100sccm, C2H2Flow 100sccm, sedimentation time 240min.Obtain
CrCN overall film thickness be about 2.4 μm.Film hardness is 25.63GPa, adhesive force 40.90N, friction factor 0.218,
Salt fog corrosion resistance test 72h has no hickie and rusty stain.
By taking embodiment 1 as an example, accompanying drawing 3 is that embodiment one is scanned using the Flied emissions of Nova NanoSEM 450 of FEI Co.
Electron microscope (SEM), the microscopic cross figure that multiplication factor is 200000 times of shootings.Because two kinds of different thin-film materials are conductive
Property it is different, cause shooting effect under Electronic Speculum different, therefore the nano-multilayered structures of TiCN and CrCN alternating deposits show in figure
For light and dark lines, as seen from the figure, multilayer film interior solid is uniform, preferable with matrix associativity.Accompanying drawing 4 show implementation
Micro-hardness testing interface in example one, the TTX-NHT2 type nano-hardness testers produced using Anton Paar company of Switzerland are measured.By
Diamond penetrator carries 10s to depth (being pressed into 135nm in the present embodiment) of the film press-in not higher than film thickness 10%, guarantor,
Compression distance-loaded load curve is obtained, can be calculated by software, sample hardness is 39.03GPa.
As shown in figure 5, in embodiment one, five, six sample friction factor curve, material be respectively TiCN, CrCN with
TiCN/CrCN nano-multilayer films.Using MMW-1 type friction wear testing machines, sell disk and 45 steel test rings with 40Cr and mill, loading are carried
Lotus 50N, rotating speed 1000r/min, obtain average friction factor and its change curve.TiCN, CrCN and TiCN/CrCN nanometer multilayer
The average friction factor of film is followed successively by 0.325,0.218,0.137, and CrCN and the friction factor of TiCN/CrCN nano-multilayer films
Curve ratio TiCN is more stable.In general, the wearability of TiCN/CrCN nano-multilayer films is best.
In summary, due to the utility model under nanoscale alternating deposit TiCN and CrCN, be not easy to form tradition more
The bulk column crystal occurred in arc ion plating coating process so that membrane structure is finer and close, has ensured that film has preferable power
Performance and friction and wear behavior are learned, made nano-multilayer film has low interfacial shearing stress, wearability and corrosion resistance high
The advantages that.In addition, after being improved to existing multi-arc ion plating equipment, during TiCN/CrCN nano-multilayer films are prepared, when
The first arc and the second arc can block the arc light of opposite target completely when depositing wherein thin film, and all targets can
To open for a long time simultaneously, Ti targets and the alternately continually start and stop of Cr targets are avoided, the not only more power saving of this method, also makes entirely to plate
Membrane process is more stable, safety, can substantially reduce the big amount of molten drops that the moment that each target is opened ejects so that in film
Bulky grain is reduced, and high-quality thin film is prepared to ensure；Meanwhile this improvement also causes to TiCN/CrCN nano thin-film films
The adjustment of modulation period and modulation ratio is very convenient：Modulation period (i.e. monolayer film thickness) is only by changing matrix with the first arc
The frequency that shape plate and the second arc rotate be can be achieved, and modulation ratio can be adjusted by changing Ti targets or Cr targets arc current.
Claims (3)
1. a kind of TiCN/CrCN nano-multilayer films, it is characterised in that provided with Ti transition zones, TiN transition zones and nanoscale
TiCN/ CrCN films, wherein, TiCN and CrCN alternating deposits form TiCN/ CrCN films, Ti transition zones, TiN transition zones and
TiCN/ CrCN films are sequentially depositing to form superlattices nano-multilayer film from matrix to coating surface.
2. TiCN/CrCN nano-multilayer films according to claim 1, it is characterised in that TiCN/CrCN thin film modulates cycles
For：TiCN is 15-20nm, CrCN 5-10nm；Multilayer film gross thickness is 1.5-4 μm, and total cycle number of plies is 60-200 layers.
3. TiCN/CrCN nano-multilayer films according to claim 1, it is characterised in that Ti transition region thicknesses are 200-
500nm, TiN transition region thickness are 100-400nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110205584A (en) * | 2019-05-30 | 2019-09-06 | Oppo广东移动通信有限公司 | Casting of electronic device and preparation method thereof and electronic equipment |
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| CN110205584A (en) * | 2019-05-30 | 2019-09-06 | Oppo广东移动通信有限公司 | Casting of electronic device and preparation method thereof and electronic equipment |
| CN110205584B (en) * | 2019-05-30 | 2021-05-28 | Oppo广东移动通信有限公司 | Electronic equipment shell, preparation method thereof and electronic equipment |
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