CN106086886A - A kind of self-lubricating titanium diboride/diamond-like coating and its preparation method and application - Google Patents
A kind of self-lubricating titanium diboride/diamond-like coating and its preparation method and application Download PDFInfo
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- CN106086886A CN106086886A CN201610654843.2A CN201610654843A CN106086886A CN 106086886 A CN106086886 A CN 106086886A CN 201610654843 A CN201610654843 A CN 201610654843A CN 106086886 A CN106086886 A CN 106086886A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
- C23C28/046—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material with at least one amorphous inorganic material layer, e.g. DLC, a-C:H, a-C:Me, the layer being doped or not
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
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Abstract
The invention discloses a kind of self-lubricating titanium diboride (TiB2)/Diamond-like Carbon (DLC) hard coat and preparation method thereof.Described TiB2/ DLC hard coat is to use bipolar pulse magnetron sputtered deposition technology by TiB in substrate2Ceramic layer is periodically overlapped mutually with DLC layer and forms, TiB2The modulation period of/DLC hard coat is 15～60nm, and total coating thickness is 1.2～1.4 μm.TiB of the present invention2/ DLC hard coat combines TiB2Advantage respective with DLC, there is hardness and the lubrication property of excellence, and there is good electric conductivity, the pulsed magnetron sputtering deposition technique simultaneously used is easy to operate, technique is simple, and manufacturing cycle is short, low cost, it is easy to large-scale industrial production, can be widely applied to the fields such as cutter, mould, microelectronics, protection.
Description
Technical field
The invention belongs to surface protection technique and related coatings technical field, relate to the laminated coating of a kind of self-lubricating, more
In particular it relates to the titanium diboride (TiB of a kind of periodic multilayer structure with high rigidity, low-friction coefficient2)/diamond like carbon
(DLC) coating and its preparation method and application.
Background technology
Along with development and the progress of industrial technology of society, industrial circle proposes the highest wanting to the performance of material
Ask, there is at a lot of engineer applied application requirements materials the combination property of excellence；Do not require nothing more than it and there is high hardness, corrosion-resistant
Performance, also requires that it has low coefficient of friction, good high-temperature stability etc..For meeting the most complicated and diversified engineering need
Ask, coat one layer of hard coat at material surface, arise at the historic moment improving the protective coating of the combination property of material.Hard is coated with
Layer can improve the surface property of material, reduces the friction and wear with workpiece, the effective material surface hardness, toughness, resistance to of improving
Mill property and high-temperature stability, increase substantially the service life of coating product.Hard coat is improve material surface performance one
Plant economical and practical means, at present in machining, particularly occupy an important position in metal cutting.It develops adaptation
The modern manufacturing industry high-tech requirement to metal cutting tool, causes the great change of cutter material and performance, can be widely used
In fields such as machine-building, auto industry, textile industry, geological drilling, mould industry, Aero-Space.
Titanium diboride (TiB2) as magnesium-yttrium-transition metal boride, there is high rigidity, high-melting-point, high wearability and corrosion resistant
The physicochemical property of a series of excellences such as erosion property, good electrical conductivity and thermal conductivity, chemical stability are excellent, it is excellent to be that one has
Structural behaviour and the advanced ceramics material of functional performance.Diamond-like coating (DLC) is that one contains gold in microstructure
The coating of hard rock composition.The element constituting DLC is carbon, with sp between carbon atom and carbon atom3And sp2Strong form combines, due to
Containing diamond components, DLC has the most excellent characteristic, such as: high rigidity, low-friction coefficient, fabulous film layer compactness,
Good chemical stability and good optical property etc..The property that the DLC coating being applied on cutter is shown
Exceed well over other hard coat.
Titanium diboride is poor due to toughness, easily cracks and the inefficacy that comes off when being impacted, and causes it as protection
Service efficiency and the application of coating are restricted.The most conventional toughness reinforcing mode of hard coat has multiple structure toughness reinforcing and soft
Matter is mutually toughness reinforcing.Owing to being limited by structure and doping content, make coating performance unstable or tough in periodically change
Property improve while hardness decline the biggest.Therefore, exploration is capable of hard and tough coating becomes the skill that this area is urgently to be resolved hurrily
Art problem.
Summary of the invention
The invention aims to overcome the deficiencies in the prior art, it is provided that a kind of high rigidity, low stress, low friction system
Count and there is excellent toughness, can apply to the multilayer hard protective coating of the product surface such as component of machine, knife mold.I.e. adopt
Use TiB2With the combination of DLC, by TiB2What layer and DLC layer alternating deposit were formed on matrix has high rigidity and high friction resistance
The hard coat of the periodic multilayer structure of energy.
Another mesh of the present invention is to provide above-mentioned self-lubricating titanium diboride TiB2The system of/diamond like carbon DLC hard coat
Preparation Method, this preparation method has easy to operate, and technique is simple, and manufacturing cycle is short, low cost, it is simple to large-scale industrial production
Etc. advantage.
Still a further object of the present invention is to provide above-mentioned self-lubricating titanium diboride TiB2/ diamond like carbon DLC hard coat cutter,
Application in mould, microelectronics and protection field.
Above-mentioned purpose of the present invention is to be achieved by the following technical programs:
A kind of self-lubricating titanium diboride TiB2/ diamond like carbon DLC coating, described TiB2/ DLC coating is with TiB2Ceramic target
It is raw material with graphite target, on matrix, replaces sputtering sedimentation by multi-target magnetic control sputtering and formed by TiB2Nano-ceramic layer and DLC
Nanometer layer is periodically overlapped mutually and forms.
Preferably, described TiB2Ceramic target is flat target, and the atomic ratio of Ti and B is 1:2, and purity is 99.99%；Graphite target
For Style Columu Talget, purity is 99.99%.
Preferably, the one during described matrix is hard alloy, monocrystalline silicon piece, alumina wafer or glass.
Preferably, described matrix and TiB2Nanometer layer contacts, and described DLC nanometer layer is outermost layer, TiB2/ DLC hard coat
Gross thickness is 1.2～1.4 μm.
Preferably, the thickness of described DLC layer is 5～10nm/ layers, TiB2The thickness of layer is 10～50nm/ layers, described TiB2/
DLC and TiB in DLC hard coat2Total number of plies be 20～80 layers.
A kind of above-mentioned self-lubricating TiB2The preparation method of/DLC hard coat, comprises the following specific steps that:
S1. matrix is cleaned: the matrix after polished process is sent into ultrasonic washing unit, successively with acetone, dehydrated alcohol
Carry out ultrasonic cleaning 10～20min with 15～30kHz respectively, then clean with deionized water, then with the nitrogen of purity >=99.5%
Air-blowing is done；
S2. evacuation and ion beam etching clean plated film cavity: the matrix after ultrasonic cleaning is placed in the workpiece of vacuum chamber
On support, it is evacuated to vacuum 5.0 × 10-3Below Pa, later on ion source, it is passed through 80～100sccm argon to ion source, if
Putting ionogenic power is 0.9kW, and the bias arranging work support is-300～-500V, etch cleaner process continue 20～
30min；
S3. ion beam etching matrix: by matrix as ion source front, arranging bias is-300～-500V, the working time
It is 15～20min；
S4.TiB2The preparation of/DLC hard coat: the method using bipolar pulse magnetron sputtering, arranges matrix and support ginseng
Number, target and the distance of matrix, be passed through argon 80～100sccm, control gas pressure in vacuum 0.5～0.6Pa, open and arrange electricity
Source dates, wherein TiB2Ceramic target is A target, and graphite target is B target, by sample baffle plate transposition in TiB2Before ceramic target and graphite target, rise
Brightness, after pre-sputtering 10～15min, opens sample baffle plate, starts sputtering sedimentation TiB2/ DLC hard coat, sputtering time is 3h.
S5. deposition terminates, and closes power supply, treats that vacuum chamber temperature is down to room temperature, fills air toward vacuum chamber, opens vacuum chamber and take
Go out sample, form TiB at matrix surface2/ DLC hard coat.
Preferably, matrix described in step S4 and support parameter are: substrate bias-100～-300V, support rotation 3rpm/
Min, revolution 2～5rpm/min, depositing temperature 300 DEG C is set.
Preferably, power parameter described in step S4 is: frequency 40kHz, power 3～4kW, A target pulse power account for
Empty ratio is 25～75%.
Preferably, target described in step S4 is 6～10cm with the distance of matrix.
Above-mentioned self-lubricating titanium diboride/diamond like carbon hard coat is in cutter, mould and microelectronic surfacecti proteon field
In application the most within the scope of the present invention.
Compared with prior art, the method have the advantages that
1. the TiB of the present invention2/ DLC hard coat has periodic multiple structure, not only has high rigidity but also have good
Toughness, friction resistant, polishing machine, electric conductivity and resistance to chemical corrosion all show good TiB simultaneously2/ DLC hard is coated with
Layer.Wherein, TiB2There is hexagonal crystallographic texture and (001) preferred orientation；DLC layer contains a number of SP3Key.Owing to adding
DLC layer makes TiB2/ DLC coating has high rigidity and relatively low coefficient of friction, and it is less than with the coefficient of friction of GCr15 steel ball
0.30, thus show excellence crocking resistance, can as protective coating for have high friction resistance can and high rigidity
Engineering applications, can be used for cutter, mould, microelectronic surfacecti proteon field.
2. present invention preparation has the TiB of nanometer laminated structure2/ DLC hard coat, easy to operate, technique is simple, preparation
Cycle is short, low cost, it is simple to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the TiB of embodiment 1 preparation2/ DLC coating structure schematic diagram.
Fig. 2 is the TiB of embodiment 1 preparation2/ DLC coating XRD figure.
Fig. 3 is the TiB of embodiment 1 preparation2The surface SEM figure of/DLC coating.
Fig. 4 is the TiB of embodiment 1 preparation2The cut shape appearance figure of/DLC coating.
Detailed description of the invention
Further illustrate present disclosure below in conjunction with Figure of description and specific embodiment, but should not be construed as this
The restriction of invention.If not specializing, the conventional hands that technological means used in embodiment is well known to those skilled in the art
Section.Unless stated otherwise, the present invention uses reagent, method and apparatus are the art conventional reagent, method and apparatus.
Embodiment 1
1. preparation:
S1. matrix is cleaned: the WC-Co hard alloy matrix after polished process is sent into ultrasonic washing unit, uses successively
Acetone, dehydrated alcohol carry out ultrasonic cleaning 10min respectively with 30kHz, then clean with deionized water, then with purity >=99.5%
Nitrogen dry up.
S2. evacuation and ion beam etching cleaning chamber and matrix: TiB installed by ion plating equipment2Flat target and graphite column
Shape target, cleans coating chamber with high power vacuum cleaner.Matrix after ultrasonic cleaning is placed on the work support of vacuum chamber, is evacuated to true
Reciprocal of duty cycle 5.0 × 10-3Below Pa, later on ion source, it is passed through 80sccm argon to ion source, ion source power 0.9kW is set,
Arranging work support bias-300V, this etching cleaning process continues 20min.
S3. ion beam etching matrix: rotate pivoted frame, by matrix as ion source front, bias-500V is set, during work
Between be 20min.
S4. it is passed through argon 80sccm, controls gas pressure in vacuum 0.56Pa, the method using bipolar pulse magnetron sputtering,
TiB2Ceramic target is A target, and graphite target is B target, and target is 10cm with the distance of matrix, arranges matrix and support parameter is: matrix
Bias-100V, support rotation 3rpm/min, revolve round the sun 2rpm/min, arranges depositing temperature 300 DEG C.Open and power parameter is set
For: frequency 40kHz, power 4kW, A target pulse power dutycycle be 75%.By sample baffle plate transposition in two sputtering targets
Before, build-up of luminance, after carrying out pre-sputtering 10min, open sample baffle plate, start formal sputtering depositing Ti B2/ DLC laminated coating, deposition
Time is 3h.
S5. deposition terminates, and closes power supply, treats that vacuum chamber temperature is down to room temperature, fills air toward vacuum chamber, opens vacuum chamber and take
Go out sample, form the TiB of periodic multilayer structure at WC-Co hard alloy matrix surface2/ DLC coating.
2. performance test:
Fig. 1 is TiB2/ DLC coating structure schematic diagram.Wherein, the thickness of DLC layer is 5～10nm/ layers, TiB2The thickness of layer
It is 10～50nm/ layers, TiB2DLC and TiB in/DLC hard coat2Total number of plies be 20～80 layers.Fig. 2 is TiB2/ DLC coating
XRD figure, it can be seen that TiB2Well-crystallized, has 001 preferred orientation, and DLC is amorphous state.Fig. 3 is TiB2/ DLC coating
Surface SEM schemes, it can be seen that coating surface is smooth, does not has obvious particle agglomeration, and result shows that coating surface growth is good
Good, dense uniform.
TiB by preparation2/ DLC coating sample is analyzed test, with Anton Paar NHT2 type nano-hardness tester testing coating
Consistency and elasticity modulus, result shows, TiB2/ DLC coating shows good toughness, and elastic resilience reaches 50%；Record
Coating hardness reaches 35Gpa；Recording coefficient of friction with HSR-2M coating friction wear testing machine is 0.19, after sample abrasion 1h,
Have no inefficacy, it is seen that TiB2/ DLC coating has good wear Characteristics.Coating is recorded residual with fast general membrane stress instrument
Overbottom pressure stress 0.5Gpa；By Anton Paar MST type nanometer scratching instrument test result as shown in Figure 4, Fig. 4 is TiB2Drawing of/DLC coating
Trace shape appearance figure.There it can be seen that cut with load increase, cut gradually broadens, load increase the degree of depth increase, around cut
Without film layer obscission, and crackle does not occur in scoring groove, more smooth groove occurs, result shows Hardness loss
TiB in the case of Bu great2/ DLC coating shows preferable toughness.Coated film base junction is closed critical load and is reached 10GPa, and coating is adhered to
Excellent performance；Finally by obtained TiB2/ DLC coating carries out acid-fast alkali-proof corrosion test at normal temperatures, and result shows, TiB2/
DLC coating has good chemical stability.
Embodiment 2
S1. matrix is cleaned: the single crystal silicon substrate being orientated (100) after polished process sends into ultrasonic washing unit, depends on
Secondary acetone, dehydrated alcohol carry out ultrasonic cleaning 10min respectively with 30kHz, then rinse with deionized water, then with purity >=
The nitrogen of 99.5% dries up.
S2. evacuation and ion beam etching cleaning chamber and matrix: TiB installed by ion plating equipment2Flat target and graphite column
Shape target, cleans coating chamber with high power vacuum cleaner.Matrix after ultrasonic cleaning is placed on the work support of vacuum chamber, vacuum chamber
Evacuation, to vacuum 5.0 × 10-3Below Pa, later on ion source, it is passed through 80sccm argon to ion source, ion source is set
Power 0.9kW, arranges work support bias 300V, and this etching cleaning process continues 20min.
S3. ion beam etching matrix: rotate pivoted frame, by matrix as ion source front, bias-500V is set, during work
Between be 20min.
S4. it is passed through argon 80sccm, controls gas pressure in vacuum 0.56Pa, the method using bipolar pulse magnetron sputtering,
TiB2Ceramic target is A target, and graphite target is B target, and target is 6cm with the distance of matrix, arranges matrix and support parameter is: matrix is inclined
Pressure-300V, support rotation 3rpm/min, revolve round the sun 5rpm/min, arranges depositing temperature 300 DEG C.Opening and arrange power parameter is:
Frequency 40kHz, power 4kW, A target pulse power dutycycle be 25%.By sample baffle plate transposition before two sputtering targets, rise
Brightness, after carrying out pre-sputtering 15min, opens sample baffle plate, starts formal sputtering depositing Ti B2/ DLC laminated coating, sedimentation time
3h。
S5. deposition terminates, and closes power supply, treats that vacuum chamber temperature is down to room temperature, inflates toward vacuum chamber, opens vacuum chamber and takes out
Sample, at the TiB of the single crystal silicon substrate surface formation periodic multilayer structure that (100) are orientated2/ DLC coating.
The above embodiment of the present invention only clearly demonstrates example of the present invention, and is not the reality to the present invention
Execute the restriction of mode.For those of ordinary skill in the field, can also be made other on the basis of the above description
The variation of multi-form.Here without also cannot all of embodiment be given exhaustive.All in the spirit and principles in the present invention
Within any amendment, equivalent and the improvement etc. made, within should be included in the protection domain of the claims in the present invention.
Claims (10)
1. a self-lubricating titanium diboride TiB2/ diamond like carbon DLC hard coat, it is characterised in that described TiB2/ DLC coating is
With TiB2Ceramic target and graphite target are raw material, replace sputtering sedimentation by multi-target magnetic control sputtering and formed by TiB on matrix2Nanometer
Ceramic layer is periodically overlapped mutually with DLC nanometer layer and forms.
Self-lubricating titanium diboride/diamond like carbon hard coat the most according to claim 1, it is characterised in that described TiB2Pottery
Porcelain target is flat target, and the atomic ratio of Ti and B is 1:2, and purity is 99.99%；Graphite target is Style Columu Talget, and purity is 99.99%.
Self-lubricating titanium diboride/diamond like carbon hard coat the most according to claim 1, it is characterised in that described matrix is
One in hard alloy, monocrystalline silicon piece, alumina wafer or glass.
Self-lubricating titanium diboride/diamond like carbon hard coat the most according to claim 1, it is characterised in that described matrix with
TiB2Nanometer layer contacts, and described DLC nanometer layer is outermost layer, TiB2/ DLC hard coat gross thickness is 1.2～1.4 μm.
Self-lubricating titanium diboride/diamond like carbon hard coat the most according to claim 1, it is characterised in that described DLC layer
Thickness is 5～10nm/ layers, TiB2The thickness of layer is 10～50nm/ layers, described TiB2DLC and TiB in/DLC hard coat2Total
The number of plies is 20～80 layers.
6. one kind according to self-lubricating TiB described in any one of claim 1-52The preparation method of/DLC hard coat, its feature exists
In, comprise the following specific steps that:
S1. matrix is cleaned: the matrix after polished process is sent into ultrasonic washing unit, successively with acetone, dehydrated alcohol with 15
～30kHz carries out ultrasonic cleaning 10～20min respectively, then clean with deionized water, then blow with the nitrogen of purity >=99.5%
Dry；
S2. evacuation and ion beam etching clean plated film cavity: the matrix after ultrasonic cleaning is placed in the work support of vacuum chamber
On, it is evacuated to vacuum 5.0 × 10-3Below Pa, later on ion source, be passed through 80～100sccm argon to ion source, arrange from
The power of component is 0.9kW, and the bias arranging work support is-300～-500V, and etch cleaner process continues 20～30min；
S3. ion beam etching matrix: by matrix as ion source front, arranging bias is-300～-500V, and the working time is 15
～20min；
S4.TiB2The preparation of/DLC hard coat: the method using bipolar pulse magnetron sputtering, arranges matrix and support parameter, target
Material and the distance of matrix, be passed through argon 80～100sccm, control gas pressure in vacuum 0.5～0.6Pa, open and arrange power supply ginseng
Number, wherein TiB2Ceramic target is A target, and graphite target is B target, by sample baffle plate transposition in TiB2Before ceramic target and graphite target, build-up of luminance,
After pre-sputtering 10～15min, open sample baffle plate, start sputtering sedimentation TiB2/ DLC hard coat, sputtering time is 3h.
S5. deposition terminates, and closes power supply, treats that vacuum chamber temperature is down to room temperature, fills air toward vacuum chamber, opens vacuum chamber and takes out sample
Product, form TiB at matrix surface2/ DLC hard coat.
Preparation method the most according to claim 6, it is characterised in that matrix described in step S4 and support parameter be: base
Body-bias-100～-300V, support rotation 3rpm/min, revolution 2～5rpm/min, depositing temperature 300 DEG C is set.
Preparation method the most according to claim 6, it is characterised in that power parameter described in step S4 is: frequency
40kHz, power 3～4kW, A target pulse power dutycycle be 25～75%.
Preparation method the most according to claim 6, it is characterised in that target described in step S4 is 6 with the distance of matrix
～10cm.
10. the self-lubricating titanium diboride/diamond-like coating described in claim 1-6 is on cutter, mould and microelectronic surface
Application in protection field.
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Cited By (9)
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| CN106756820A (en) * | 2016-12-01 | 2017-05-31 | 深圳先进技术研究院 | Containing diamond-like composite coating and preparation method thereof |
| CN106835133A (en) * | 2016-12-21 | 2017-06-13 | 中国科学院深圳先进技术研究院 | A kind of workpiece with titanium diboride diamond composite coating and preparation method thereof |
| CN107937873A (en) * | 2017-12-22 | 2018-04-20 | 深圳先进技术研究院 | Transition metal boride coating, carbon transition metal boride composite coating, preparation method and application and the cutting element of carbon doping |
| CN108300967A (en) * | 2018-03-29 | 2018-07-20 | 武汉大学 | High temperature resistant low friction DLC/AlTiSiN multi-layer composite coatings and preparation method thereof |
| CN109136839A (en) * | 2017-06-28 | 2019-01-04 | 深圳先进技术研究院 | A kind of workpiece and preparation method thereof with aluminium doping titanium diboride coating |
| CN109750291A (en) * | 2017-11-07 | 2019-05-14 | 深圳先进技术研究院 | A kind of boron-doped diamond electrode and preparation method thereof |
| CN112458399A (en) * | 2020-11-24 | 2021-03-09 | 创隆实业(深圳)有限公司 | TiB2Preparation method of DLC coating |
| CN113529031A (en) * | 2020-04-13 | 2021-10-22 | 季华实验室 | Diamond-like carbon film and preparation method thereof |
| CN114033799A (en) * | 2021-11-29 | 2022-02-11 | 江苏科技大学 | Machining method of sliding bearing composite lubricating structure based on electron beam curing |
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