CN103510046A - Metal-doped diamond-like carbon thick film and preparation method thereof - Google Patents
Metal-doped diamond-like carbon thick film and preparation method thereof Download PDFInfo
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- CN103510046A CN103510046A CN201310453284.5A CN201310453284A CN103510046A CN 103510046 A CN103510046 A CN 103510046A CN 201310453284 A CN201310453284 A CN 201310453284A CN 103510046 A CN103510046 A CN 103510046A
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Abstract
The invention discloses a metal-doped diamond-like carbon thick film which comprises a substrate, a combining layer, doping layers and functional layers, wherein the doping layers and the functional layers are combined to form composite layers, the combining layer is arranged on the upper surface of the substrate, the sequentially overlapped composite layers are arranged on the upper surface of the combining layer, the doping layers and the functional layers are arranged at intervals, the combining layer is combined with the doping layers in the composite layers, and the thickness of the diamond-like carbon thick film is more than 4 micron. The metal-doped diamond-like carbon thick film has the benefits that a plurality of layers of nano-scale metal-bearing diamond-like carbon structures (for example, wolframium-bearing diamond-like carbon (DLC-W)) are doped in the pure DLC (diamond-like carbon) film, so that the internal stress of the DLC film is fully relieved, and meanwhile, the binding force between the film and the substrate is also effectively increased, as a result, the thickness of the film is more than 10 micron, and a scratch binding force of more than 100 N is achieved.
Description
Technical field
The present invention relates to a kind of quasi-diamond thick film with the containing metal doping of nanostructure, with and preparation method thereof, new material technology field belonged to.
Background technology
In recent years, various coating technology developments, for industry manufacture and daily life are brought many progress and facility.Rely on coating technology, can make product or component obtain better surface property, thereby make up some characteristic that material itself does not have.Diamond-film-like (Diamond-like Carbon), or be called for short DLC film, be the metastable amorphous substance that contains diamond lattic structure (sp3 key) and graphite-structure (sp2 key).
Because DLC film has the similar excellent properties of high rigidity, high-wearing feature, low-friction coefficient, high heat conductance, high resistivity, unreactiveness etc. and diamond film, so DLC film is one of the study hotspot in thin film technique field in recent years always, also because it has the feature that hardness is high, frictional coefficient is low in tribology, so be widely used among various tool, part.
But, because the internal stress of DLC film is higher, thus its coat-thickness not high (4 microns following), and because the bonding force between itself and base material is poor, restricted to a great extent its application.Because the internal stress of DLC is larger, thickness is that the pure DLC film of the individual layer of 10 μ m does not almost have bonding force, so without any using value.
Therefore, for overcoming the defect of prior art, reduce the internal stress of DLC film, strengthen the bonding force between base material, in the urgent need to a kind of new Film preparation technique.
Summary of the invention
For the deficiencies in the prior art, the present invention proposes a kind of quasi-diamond thick film and preparation technology thereof with the containing metal doping of nanostructure, in pure DLC film, adulterate several layers of nano level tungstenic quasi-diamond (DLC-W) structure or respective metal doped diamond structure, fully alleviate the internal stress of DLC film itself, also effectively increased the bonding force between coating and base material simultaneously.
Goal of the invention of the present invention is achieved through the following technical solutions: a kind of quasi-diamond thick film of containing metal doping, comprise base material, key coat, doped layer and functional layer, described doped layer and functional layer are in conjunction with forming a composite bed, the upper surface of described base material is provided with key coat, the upper surface of described key coat is provided with composite bed and described doped layer and the setting of functional layer interval of stack successively, the doped layer of described key coat in composite bed is combined, and the thickness of described quasi-diamond thick film is greater than 4 μ m.
Preferably, the thickness of described quasi-diamond thick film is greater than 10 μ m, and has cut bonding force more than 100N.
Preferably, described base material is a kind of in steel alloy, Si, pottery.
Preferably, described key coat is a kind of in Cr, Ti, Ni, Si, and the thickness of described key coat is 200 ~ 300nm.
Preferably, the metal adulterating in described doped layer is one or more in W, Ti, Cr, and the thickness of described doped layer is 80 ~ 120nm.
Preferably, described functional layer is DLC film, and its thickness is 450 ~ 550nm.
The present invention has also disclosed a kind of preparation method of quasi-diamond thick film of containing metal doping, comprises the following steps:
S1) base material is fixed in vacuum film coating chamber, vacuum film coating chamber is bled, make it to reach 5.0 * 10
-3vacuum tightness more than Pa;
S2) passing into purity is Ar gas more than 5N, with ionic fluid, described base material is carried out to Ion Cleaning, Ar airshed 10 ~ 30sccm, operation pressure 1.2 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 800 ~ 1600V on ionic fluid, electric current 100 ~ 200mA, and scavenging period 10min, applies pulsed bias 1500 ~ 2000V on base material in this cleaning process, frequency 40 ~ 60kHz, dutycycle is greater than 90%;
S3) adopt magnetron sputtering technique to carry out the deposition preparation of key coat, in deposition process to the Ar gas that passes into airshed 35 ~ 50sccm in plated film vacuum chamber, operation pressure 2.0 ~ 3.0Pa, on magnetic control sputtering cathode, apply galvanic current 5.0 ~ 8.0A, depositing time 20 ~ 30min, in this deposition process, on base material, apply DC pulse bias voltage 100 ~ 120V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S4) adopt ion beam technology and magnetron sputtering technique to carry out the deposition preparation of doped layer simultaneously, in deposition process, in plated film vacuum chamber, pass into C
2h
2gas and Ar gas, C
2h
2flow 20 ~ 25sccm, Ar airshed 8 ~ 10sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa; The target of magnetic control sputtering cathode is metal to be adulterated in described doped layer, on it, apply radio frequency power 450 ~ 550W, on ionic fluid, apply volts DS 1200 ~ 1600V, electric current 120 ~ 220mA, coating depositing time 10 ~ 20min, in this deposition process, on base material, apply DC pulse bias voltage 1500 ~ 2000V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S5) adopt ion beam technology to carry out the deposition preparation of functional layer, in deposition process, pass into C
2h
2gas, flow 30 ~ 45sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 1200 ~ 1600V on ionic fluid, electric current 120 ~ 220mA, and coating depositing time 60 ~ 80min, applies DC pulse bias voltage 1500 ~ 2000V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90% on base material in this deposition process;
S6) alternately complete above step S4) and S5) until total thickness reaches requirement.
Preferably, the thickness of described functional layer is greater than the thickness of described doped layer.
Preferably, described step S4), the target of magnetic control sputtering cathode is one or more in W, Ti, Cr.
Beneficial effect of the present invention is mainly reflected in: the several layers of nano level containing metal quasi-diamond that adulterate in pure DLC film (for example: tungstenic quasi-diamond DLC-W) structure, fully alleviate the internal stress of DLC film itself, also effectively increased the bonding force between rete and base material simultaneously, make thicknesses of layers can surpass 10 μ m, and there is cut bonding force more than 100N.
Accompanying drawing explanation
Fig. 1: the structural representation of the quasi-diamond thick film of containing metal doping of the present invention.
Embodiment
Below, by exemplary embodiments, the present invention is further described, but the present invention is not limited to described embodiment.
As shown in Figure 1, the quasi-diamond thick film of containing metal doping of the present invention, comprise base material 1, key coat 2, doped layer 3 and functional layer 4, described doped layer 3 and functional layer 4 are in conjunction with forming a composite bed, the upper surface of described base material 1 is provided with key coat 2, the upper surface of described key coat 2 is provided with composite bed and described doped layer 3 and the functional layer 4 intervals settings of stack successively, doped layer 3 combinations in described key coat 2 and composite bed.Base material 1 is selected from a kind of in steel alloy, Si, pottery, and key coat 2 is a kind of in Cr, Ti, Ni, Si, and the thickness of described key coat 2 is 200 ~ 300nm.In doped layer 3, the metal of doping is one or more in W, Ti, Cr, and the thickness of described doped layer 3 is 80 ~ 120nm.Functional layer 4 is DLC film, and its thickness is 450 ~ 550nm.
Due to metal have well moulding, the therefore optional hotchpotch as improving the bonding force of DLC film.If doped layer adopts other metal, as Ti, Cr, because doped layer forms TiC or this bi-material of CrC, the very high while fragility of itself hardness is also very large, and the combination between they and DLC is not good enough in addition, so cause the bonding force variation of final coating, may normally use.Therefore, the preferred embodiment in the present invention one adopts W as the doping metals of doped layer.
Embodiment mono-:
S1) base material is fixed in vacuum film coating chamber, vacuum film coating chamber is bled, make it to reach 5.0 * 10
-3vacuum tightness more than Pa;
S2) passing into purity is Ar gas more than 5N, with ionic fluid, described base material is carried out to Ion Cleaning, Ar airshed 10 ~ 30sccm, operation pressure 1.2 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 800 ~ 1600V on ionic fluid, electric current 100 ~ 200mA, and scavenging period 10min, applies pulsed bias 1500 ~ 2000V on base material in this cleaning process, frequency 40 ~ 60kHz, dutycycle is greater than 90%;
S3) adopt magnetron sputtering technique to carry out the deposition preparation of key coat, in deposition process to the Ar gas that passes into airshed 35 ~ 50sccm in plated film vacuum chamber, operation pressure 2.0 ~ 3.0Pa, on magnetic control sputtering cathode, apply galvanic current 5.0 ~ 8.0A, depositing time 20 ~ 30min, in this deposition process, on base material, apply DC pulse bias voltage 100 ~ 120V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S4) adopt ion beam technology and magnetron sputtering technique to carry out the deposition preparation of doped layer DLC-W simultaneously, in deposition process, in plated film vacuum chamber, pass into C
2h
2gas and Ar gas, C
2h
2flow 20 ~ 25sccm, Ar airshed 8 ~ 10sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa; The target of magnetic control sputtering cathode is W, on it, apply radio frequency power 450 ~ 550W, on ionic fluid, apply volts DS 1200 ~ 1600V, electric current 120 ~ 220mA, coating depositing time 10 ~ 20min, in this deposition process, on base material, apply DC pulse bias voltage 1500 ~ 2000V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S5) adopt ion beam technology to carry out the deposition preparation of functional layer, in deposition process, pass into C
2h
2gas, flow 30 ~ 45sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 1200 ~ 1600V on ionic fluid, electric current 120 ~ 220mA, and coating depositing time 60 ~ 80min, applies DC pulse bias voltage 1500 ~ 2000V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90% on base material in this deposition process;
S6) alternately complete above step S4) and S5) until total thickness reaches requirement.
Embodiment bis-:
S1) base material is fixed in vacuum film coating chamber, vacuum film coating chamber is bled, make it to reach 5.0 * 10
-3vacuum tightness more than Pa;
S2) passing into purity is Ar gas more than 5N, with ionic fluid, described base material is carried out to Ion Cleaning, Ar airshed 10 ~ 30sccm, operation pressure 1.2 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 800 ~ 1600V on ionic fluid, electric current 100 ~ 200mA, and scavenging period 10min, applies pulsed bias 1500 ~ 2000V on base material in this cleaning process, frequency 40 ~ 60kHz, dutycycle is greater than 90%;
S3) adopt magnetron sputtering technique to carry out the deposition preparation of key coat, in deposition process to the Ar gas that passes into airshed 35 ~ 50sccm in plated film vacuum chamber, operation pressure 2.0 ~ 3.0Pa, on magnetic control sputtering cathode, apply galvanic current 5.0 ~ 8.0A, depositing time 20 ~ 30min, in this deposition process, on base material, apply DC pulse bias voltage 100 ~ 120V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S4) adopt ion beam technology and magnetron sputtering technique to carry out the deposition preparation of doped layer DLC-Ti simultaneously, in deposition process, in plated film vacuum chamber, pass into C
2h
2gas and Ar gas, C
2h
2flow 20 ~ 25sccm, Ar airshed 8 ~ 10sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa; The target of magnetic control sputtering cathode is Ti, on it, apply radio frequency power 450 ~ 550W, on ionic fluid, apply volts DS 1200 ~ 1600V, electric current 120 ~ 220mA, coating depositing time 10 ~ 20min, in this deposition process, on base material, apply DC pulse bias voltage 1500 ~ 2000V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S5) adopt ion beam technology to carry out the deposition preparation of functional layer, in deposition process, pass into C
2h
2gas, flow 30 ~ 45sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 1200 ~ 1600V on ionic fluid, electric current 120 ~ 220mA, and coating depositing time 60 ~ 80min, applies DC pulse bias voltage 1500 ~ 2000V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90% on base material in this deposition process;
S6) alternately complete above step S4) and S5) until total thickness reaches requirement.
Embodiment tri-:
S1) base material is fixed in vacuum film coating chamber, vacuum film coating chamber is bled, make it to reach 5.0 * 10
-3vacuum tightness more than Pa;
S2) passing into purity is Ar gas more than 5N, with ionic fluid, described base material is carried out to Ion Cleaning, Ar airshed 10 ~ 30sccm, operation pressure 1.2 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 800 ~ 1600V on ionic fluid, electric current 100 ~ 200mA, and scavenging period 10min, applies pulsed bias 1500 ~ 2000V on base material in this cleaning process, frequency 40 ~ 60kHz, dutycycle is greater than 90%;
S3) adopt magnetron sputtering technique to carry out the deposition preparation of key coat, in deposition process to the Ar gas that passes into airshed 35 ~ 50sccm in plated film vacuum chamber, operation pressure 2.0 ~ 3.0Pa, on magnetic control sputtering cathode, apply galvanic current 5.0 ~ 8.0A, depositing time 20 ~ 30min, in this deposition process, on base material, apply DC pulse bias voltage 100 ~ 120V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S4) adopt ion beam technology and magnetron sputtering technique to carry out the deposition preparation of doped layer DLC-Cr simultaneously, in deposition process, in plated film vacuum chamber, pass into C
2h
2gas and Ar gas, C
2h
2flow 20 ~ 25sccm, Ar airshed 8 ~ 10sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa; The target of magnetic control sputtering cathode is Cr, on it, apply radio frequency power 450 ~ 550W, on ionic fluid, apply volts DS 1200 ~ 1600V, electric current 120 ~ 220mA, coating depositing time 10 ~ 20min, in this deposition process, on base material, apply DC pulse bias voltage 1500 ~ 2000V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S5) adopt ion beam technology to carry out the deposition preparation of functional layer, in deposition process, pass into C
2h
2gas, flow 30 ~ 45sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 1200 ~ 1600V on ionic fluid, electric current 120 ~ 220mA, and coating depositing time 60 ~ 80min, applies DC pulse bias voltage 1500 ~ 2000V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90% on base material in this deposition process;
S6) alternately complete above step S4) and S5) until total thickness reaches requirement.
For the characteristic property of thick film prepared by the present invention is described, the containing metal doped diamond thick film with nanostructure that above technique is made and the performance perameter of the DLC film that ordinary process makes contrast, as shown in table 1:
| Coating kind | Common DLC | Tungstenic DLC-W | Tungstenic DLC-Ti | Tungstenic DLC-Cr |
| Coating structure | Individual layer non-nano | Nano level MULTILAYER COMPOSITE | Nano level MULTILAYER COMPOSITE | Nano level MULTILAYER COMPOSITE |
| Composition | Single DLC(a:C-H) | Contain W and mix formation nanostructure (a:C-H, W) | Contain Ti and mix formation nanostructure (a:C-H, Ti) | Contain Cr and mix formation nanostructure (a:C-H, Cr) |
| Thickness (μ m) | 10.2 | 10.3 | 10.0 | 10.0 |
| Hardness (Hv) | 2500~2700 | 2500~2700 | 2500~2700 | 2500~2700 |
| Frictional coefficient (for steel) | 0.08 | 0.08 | 0.08 | 0.08 |
| Bonding force (adopting scratch method judgement) | 0~3 | 100N | 6N | 12N |
| Wear resisting property (circle) | 0~2 | 50,000 | 10 | 50 |
By above-described embodiment, can find out, the thickness of the tungstenic quasi-diamond DLC-W with nanostructure prepared by the present invention can surpass 10 μ m, and keep the bonding force between good and base material, there is cut bonding force and the wear resisting property stronger than common DLC film.
Although invention has been described with reference to preferred embodiment, without departing from the present invention, can carry out various improvement and can replace material wherein by equivalent substance it.The present invention is not limited to disclosed specific embodiment in literary composition, but comprises all technical schemes that fall within the scope of claim.
Claims (9)
1. the quasi-diamond thick film of containing metal doping, it is characterized in that: comprise base material (1), key coat (2), doped layer (3) and functional layer (4), described doped layer (3) and functional layer (4) are in conjunction with forming a composite bed, the upper surface of described base material (1) is provided with key coat (2), the upper surface of described key coat (2) is provided with composite bed and described doped layer (3) and the setting of functional layer (4) interval of stack successively, doped layer (3) combination in described key coat (2) and composite bed, the thickness of described quasi-diamond thick film is greater than 4 μ m.
2. the quasi-diamond thick film of containing metal doping as claimed in claim 1, is characterized in that: the thickness of described quasi-diamond thick film is greater than 10 μ m, and has cut bonding force more than 100N.
3. the quasi-diamond thick film of containing metal as claimed in claim 1 doping, is characterized in that: a kind of in steel alloy, Si, pottery of described base material (1).
4. the quasi-diamond thick film of containing metal as claimed in claim 1 doping, is characterized in that: a kind of in Cr, Ti, Ni, Si of described key coat (2), the thickness of described key coat (2) is 200 ~ 300nm.
5. the quasi-diamond thick film of containing metal doping as claimed in claim 1, is characterized in that: in described doped layer (3), the metal of doping is one or more in W, Ti, Cr, and the thickness of described doped layer (3) is 80 ~ 120nm.
6. the quasi-diamond thick film of containing metal doping as claimed in claim 1, is characterized in that: described functional layer (4) is DLC film, and its thickness is 450 ~ 550nm.
7. the preparation method of the quasi-diamond thick film that the containing metal as described in any one in claim 1-6 adulterates, is characterized in that: comprise the following steps:
S1) base material (1) is fixed in vacuum film coating chamber, vacuum film coating chamber is bled, make it to reach 5.0 * 10
-3vacuum tightness more than Pa;
S2) passing into purity is Ar gas more than 5N, with ionic fluid, described base material (1) is carried out to Ion Cleaning, Ar airshed 10 ~ 30sccm, operation pressure 1.2 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 800 ~ 1600V on ionic fluid, electric current 100 ~ 200mA, and scavenging period 10min, base material in this cleaning process applies pulsed bias 1500 ~ 2000V on (1), frequency 40 ~ 60kHz, dutycycle is greater than 90%;
S3) adopt magnetron sputtering technique to carry out the deposition preparation of key coat (2), in deposition process to the Ar gas that passes into airshed 35 ~ 50sccm in plated film vacuum chamber, operation pressure 2.0 ~ 3.0Pa, on magnetic control sputtering cathode, apply galvanic current 5.0 ~ 8.0A, depositing time 20 ~ 30min, on base material in this deposition process (1), apply DC pulse bias voltage 100 ~ 120V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S4) adopt ion beam technology and magnetron sputtering technique to carry out the deposition preparation of doped layer (3) simultaneously, in deposition process, in plated film vacuum chamber, pass into C
2h
2gas and Ar gas, C
2h
2flow 20 ~ 25sccm, Ar airshed 8 ~ 10sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa; The target of magnetic control sputtering cathode is metal to be adulterated in described doped layer (3), on it, apply radio frequency power 450 ~ 550W, on ionic fluid, apply volts DS 1200 ~ 1600V, electric current 120 ~ 220mA, coating depositing time 10 ~ 20min, on base material in this deposition process (1), apply DC pulse bias voltage 1500 ~ 2000V, frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S5) adopt ion beam technology to carry out the deposition preparation of functional layer (4), in deposition process, pass into C
2h
2gas, flow 30 ~ 45sccm, operation pressure 2.0 * 10
-1~ 3.0 * 10
-1pa, applies volts DS 1200 ~ 1600V on ionic fluid, electric current 120 ~ 220mA, and coating depositing time 60 ~ 80min, applies DC pulse bias voltage 1500 ~ 2000V on base material in this deposition process (1), frequency 40 ~ 60kHz, dutycycle 70 ~ 90%;
S6) alternately complete above step S4) and S5) until total thickness reaches requirement.
8. the preparation method of the quasi-diamond thick film of containing metal doping as claimed in claim 7, is characterized in that: the thickness of described functional layer (4) is greater than the thickness of described doped layer (3).
9. the preparation method of the quasi-diamond thick film of containing metal doping as claimed in claim 7, is characterized in that: described step S4), the target of magnetic control sputtering cathode is one or more in W, Ti, Cr.
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