CN106756868A - A kind of method for improving doped diamond-like film layer quality - Google Patents
A kind of method for improving doped diamond-like film layer quality Download PDFInfo
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- CN106756868A CN106756868A CN201610990847.8A CN201610990847A CN106756868A CN 106756868 A CN106756868 A CN 106756868A CN 201610990847 A CN201610990847 A CN 201610990847A CN 106756868 A CN106756868 A CN 106756868A
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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- Plasma & Fusion (AREA)
- Chemical Vapour Deposition (AREA)
- Physical Vapour Deposition (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a kind of method for improving doped diamond-like film layer quality, before workpiece upper plasma body chemical vapor phase growing doping diamond-like film layer, screening arrangement is set around the workpiece, and the screening arrangement has opening, and the positive plasma outlet in the opening；Plasma activated chemical vapour deposition doping diamond-like film layer excessively in, the screening arrangement does not rotate with the workpiece, but with the workpiece equipotential.The method that the present embodiment is provided, mainly in deposition process, set by around the workpiece of rotation, the position for making the close distribution of plasma nearby of its screen workpiece circumference extremely uneven, only receive the strong ion deposition of the plasma density of positive plasma outlet port, finally membrane uniformity and membranous layer binding force of acquisition etc. have and are significantly lifted, and are especially suitable for industrial mass production.
Description
Technical field
Technical field of surface of the present invention, more particularly to a kind of method for improving doped diamond-like film layer quality.
Background technology
Carbon-base coating such as tetrahedron DLC (ta-diamond-like carbon, abbreviation ta-DLC) film be with
Carbon is a kind of non-crystalline material that basic element is constituted.DLC film (DLC) it belong to amorphous metastable structure in structure
Amorphous carbon, be by sp3Hydridization and sp2Hydridization carbon is constituted：Sp in film3Structures shape DLC film has many
Similar to the good characteristic of diamond, and sp2 structures shapes DLC film has the characteristic of many graphite, in the world
The insulating rigid amorphous carbon film that hardness exceedes diamond hardness 20% is referred to as diamond-film-like.
In terms of preparation technology, DLC film (DLC) depositing temperature is relatively low, and depositional area is big, and face is smooth,
Technique relative maturity.In terms of practical application, because DLC film is under vacuum with to be respectively provided with good lubrication resistance under low temperature
Mill performance, therefore can effectively solve the technical barrier of moving parts surface lubrication etc. under some special operation conditions.Carbon-based thick film shows
Stage mainly uses chemical vapour deposition technique (Chemical vapor deposition method, CVD), including DC glow
Discharge plasma CVD, radio-frequency glow discharge plasma CVD, electron cyclotron CVD, high intensity DC arc plasma sink
Product, laser plasma deposition, direct-current plasma assistant depositing and microwave plasma assisted deposition etc.；It is existing according to investigation
Have using magnetron sputtering or the method for ion plating to deposit the speed of carbon-based film layer not higher than 40nm/min, permit in process conditions
Perhaps deposition obtains 30 μm carbon-based in the case of at least needs the time of 13 hours, but reality is that profit is difficult in this way
The carbon-based film layer of the preparation more than 20 μm of stabilization is repeated, it is inclined that carbon-based film layer still has internal stress and sedimentation rate very high in itself
Slow problem.It is to improve that existing CVD method improve carbon-based thicknesses of layers to reduce internal stress and the major way of raising sedimentation rate
The air inflow of carbonaceous gas and be passed through foreign gas (element for now adulterating mostly nonmetalloid, have few species containing gold
Belong to the gas of element), but increase rate is limited in terms of carbon-based film deposition rate, and because the increase vacuum chamber of gas is special
Do not pollute not easily；In terms of stress improvement the doping of metallic element more can release film layer stress but be confined to gas containing metal in itself
Body species is few, while gas containing metal species is not easy to operate, safety coefficient is relatively low.It is well known that such as in terms of air inflow generally
In the case of CVD method operating air pressure it is general in 1Pa~103Between Pa, electron density general range is 1010~1021/m3Between,
As the increase volume density of tolerance can reach saturation, while the mean free path of electronics can reduce the ionizing efficiency meeting of carbonaceous gas
Tend towards stability, so the sedimentation rate method in carbon-based film layer is difficult big breakthrough.But there is arc light as negative electrode in metal
Plasma is produced by negative electrode in discharge process, the ion concentration highest in plasma near negative electrode can be more than 1024/m3,
In view of the multivalent state of metal, wherein electron density is general higher than ion concentration, this it is more medium than chemical vapor deposition processes from
Daughter concentration wants the 3-10 order of magnitude high, by the use of metallic plasma as ionization source, while adding a biography for plasma
Defeated passage, increases the action time of electronics or ion and gas, and the ionizing efficiency of carbonaceous gas might have the lifting of matter.
The filtered arc cathodic plasma deposition method that industrialized production is based on arc-discharge techniques prepares thick hydrogeneous diamond film
Due to the rotation of workpiece during layer, in workpiece surface because the extreme of plasma density is uneven, workpiece circumference carbon nearby is caused
Plasma density distribution is extremely uneven, finally results in the film layer matter that film quality is extremely difficult to be reached during fixed deposition
Amount, such as film hardness, sp3Content, coefficient of friction etc..
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide a kind of side for improving doping diamond-like film quality
Method, before workpiece upper plasma body chemical vapor phase growing doping diamond-like film layer, screening arrangement is set around the workpiece,
The screening arrangement has opening, and the positive plasma outlet in the opening；In plasma activated chemical vapour deposition doping class
Buddha's warrior attendant film layer excessively in, the screening arrangement not with the workpiece rotate, but with the workpiece equipotential.
Preferably, the opening angle of the screening arrangement opening is adjustable.
Preferably, the opening angle of the screening arrangement opening is 60 °~180 °.
Relative to prior art, the embodiment of the present invention has the advantage that：
1st, alternative deposition plasma volume density is the plasma of certain definite value.
2nd, film hardness and coefficient of friction are controllable, are not influenceed by workpiece surrounding environment in vacuum chamber.
3rd, the ratio of element can be by external device parameters accuracy controlling in film layer.
Brief description of the drawings
The accompanying drawing for constituting embodiment of the present invention part is the embodiment of the present invention to be further understood for providing, the present invention
Schematic description and description be used for explain the present invention, be not construed as limiting the invention.
Fig. 1 is screening arrangement structural representation provided in an embodiment of the present invention；
Fig. 2 is the test point schematic diagram of selection when performance test is carried out to workpiece film layer
Description of reference numerals:
1-screening arrangement body；2-opening.
Specific embodiment
Below by drawings and Examples, technical scheme is described in further detail.Should be understood to
These embodiments are only used for specifically describing in more detail, but are not intended to limit the scope of the invention.
In addition it is also necessary to explanation, this part to the present invention experiment used in material and test method enter
The general description of row.Although for realize many materials that the object of the invention used and operating method be it is known in the art that
But the present invention is still described in detail as far as possible herein.It will be apparent to those skilled in the art that within a context, if do not said especially
Bright, material therefor of the present invention and operating method are well known in the art.
Embodiment one
To solve film layer fragility and adhesion deviation around current workpiece, the problem of commercial Application requirement, this reality are not met
Apply example and provide a kind of method for improving doped diamond-like film layer quality, plasma activated chemical vapour deposition is carried out on workpiece
Before doping diamond-like film layer, screening arrangement is set around rotational workpieces.Fig. 1 is screening arrangement provided in an embodiment of the present invention
Structural representation, as shown in figure 1, the screening arrangement has screening arrangement body 1, and opening 2.Preferably, to reach choosing
When selecting property deposition plasma volume density is the plasma of certain definite value, the opening angle of the opening 2 of screening arrangement is adjustable.In deposition
During, the positive plasma outlet of opening 2 of screening arrangement, screening arrangement body 1 does not rotate with the workpiece, but need to be with institute
State the same current potential of workpiece.In actual mechanical process, it is preferable that the opening angle of the opening 2 of screening arrangement is 60 °~180 °.
For example, the filtered arc cathodic plasma deposition method that industrialized production is based on arc-discharge techniques prepares Ti doping
DLC film layer, is the film for ensureing to be deposited on workpiece during depositing Ti doping DLC on rotational workpieces in industrial processes
The uniformity of Ti and C element in layer, and film layer and workpiece adhesion Optimality, it is necessary in preparation process, in rotation
Screen apparatus are set around workpiece, and in deposition process, screen apparatus do not rotate with workpiece, but need to be with the same current potential of workpiece, and screen
The positive plasma outlet in the opening of proscenia, in addition, for can selective deposition plasma density be certain definite value carbon ion and
Metal Ti ions, the opening angle of screen apparatus opening can adjust.By adding screen apparatus, plasma density distribution is extremely
Do not deposited around the workpiece of uneven position, directly shielded by screen apparatus, only received just to Magnetic filter outlet port
The strong ion deposition of plasma density.Therefore, the final film hardness for obtaining and film layer coefficient can be controlled, not by vacuum
The influence of room workpiece surrounding environment, in addition, the ratio of C and Ti can be by external device parameters accuracy controlling in the film layer for obtaining.
The present embodiment provide raising doping diamond-like film quality method, mainly in deposition process, by
Screen apparatus are set around the workpiece of rotation, the position for making the close distribution of plasma nearby of its screen workpiece circumference extremely uneven
Put, only receive the strong ion deposition of the plasma density of positive plasma outlet port, the final membrane uniformity for obtaining
Have with membranous layer binding force etc. and significantly lifted, be especially suitable for industrial mass production.
Preferably to embody the technical scheme provided using the present invention, the film layer of more preferable uniformity and adhesion can be obtained,
Below, it is described with reference to the drawings, prepares film layer using technical scheme provided in an embodiment of the present invention, and performance survey is carried out to film layer
Examination, and the film layer that during with without screen equipment prepared by (when workpiece is fixed deposition and deposit during workpiece autobiography), carry out performance ratio
Compared with.
It should be noted that the equal depositing Ti doping DCL film layers of workpiece in subsequent embodiment, choose identical in experimentation
Cylindrical workpieces, and before being deposited, prepare before identical deposition is carried out to workpiece, such as：Table is carried out to workpiece surface
Face cleaning etc..Fig. 2 is the test point schematic diagram of selection when performance test is carried out to workpiece film layer, as shown in Fig. 2 to film performance
During test, 8 points (1,2-1,2-2,3-1,3-2,4-1,4-2 and 5) are chosen altogether carries out performance test.
Embodiment two
Without screen apparatus, cylindrical workpieces carry out deposition 300min when fixing, and test circumferencial direction film performance, test
Result is as shown in table 1 below.
Table 1
As shown in Table 1, without screen apparatus, cylindrical workpieces fix when deposited, the film layer film layer fragility of acquisition and
What adhesion had meets the requirements, and some deviations, that is, the membrane uniformity for obtaining is inadequate.
Embodiment three
Without screen apparatus, deposition 300min is carried out during cylindrical workpieces autobiography, test circumferencial direction film performance, test
Result is as shown in table 2 below.
Table 2
As shown in Table 2, without screen apparatus, deposited during cylindrical workpieces autobiography, the film hardness of acquisition is substantially inclined
It is soft, and film layer fragility and adhesion deviation, the film layer that its film quality is reached when being deposited when not reaching workpiece fixation
Quality, does not meet commercial Application requirement.
Example IV
Method using being provided in embodiment one, prepares film layer：
Addition screen apparatus, the opening angle of screen apparatus opening is 100 °, is deposited during cylindrical workpieces autobiography
300min, tests circumferencial direction film performance, and test result is as shown in table 3 below.
Table 3
As shown in Table 3, the method for being provided using the embodiment of the present invention one, screening arrangement is added around the workpiece of rotation,
Deposit the film layer of acquisition, although thin when thicknesses of layers is than unshielded device, but the property such as membrane uniformity and membranous layer binding force
Can have and significantly be lifted, hence it is evident that (when workpiece is fixed deposition or deposit during workpiece autobiography) system during better than without screen equipment
Standby film layer, is especially suitable for industrial mass production.
Although it should be noted that present invention has been a certain degree of description, it will be apparent that, it is of the invention not departing from
Under conditions of spirit and scope, the appropriate change of each condition can be carried out.Can be understood as the invention is not restricted to the embodiment party
Case, and it is attributed to the scope of claim, its equivalent for including each factor.
Above-described specific embodiment, has been carried out further to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail, should be understood that and the foregoing is only specific embodiment of the invention, be not intended to limit the present invention
Protection domain, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc. all should include
Within protection scope of the present invention.
Claims (3)
1. it is a kind of improve doping diamond-like film quality method, it is characterised in that in workpiece plasma chemical vapor deposition
Before product doping diamond-like film layer, screening arrangement is set around the workpiece, the screening arrangement has opening, and described opens
The positive plasma outlet of mouth；Plasma activated chemical vapour deposition doping diamond-like film layer excessively in, the screening arrangement not with
Workpiece rotation, but with the workpiece equipotential.
2. method according to claim 1, it is characterised in that the opening angle of the screening arrangement opening is adjustable.
3. method according to claim 1, it is characterised in that the opening angle of the screening arrangement opening is 60 °~
180°。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610990847.8A CN106756868B (en) | 2016-11-10 | 2016-11-10 | A method of improving doped diamond-like film layer quality |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610990847.8A CN106756868B (en) | 2016-11-10 | 2016-11-10 | A method of improving doped diamond-like film layer quality |
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| Publication Number | Publication Date |
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| CN106756868A true CN106756868A (en) | 2017-05-31 |
| CN106756868B CN106756868B (en) | 2019-07-09 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003277937A (en) * | 2002-03-19 | 2003-10-02 | Matsushita Electric Ind Co Ltd | Electrode member |
| CN1798864A (en) * | 2003-04-01 | 2006-07-05 | 马特森技术公司 | Plasma uniformity |
| CN102355792A (en) * | 2011-10-19 | 2012-02-15 | 中微半导体设备(上海)有限公司 | Electromagnetic coupling plasma device capable of improving uniformity and efficiency of plasma |
| JP2013234366A (en) * | 2012-05-09 | 2013-11-21 | Mitsubishi Plastics Inc | Method for producing gas barrier film |
| CN106011771A (en) * | 2016-08-04 | 2016-10-12 | 北京师范大学 | Apparatus for rapidly depositing DLC film on surface of piston ring, and method thereof |
-
2016
- 2016-11-10 CN CN201610990847.8A patent/CN106756868B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003277937A (en) * | 2002-03-19 | 2003-10-02 | Matsushita Electric Ind Co Ltd | Electrode member |
| CN1798864A (en) * | 2003-04-01 | 2006-07-05 | 马特森技术公司 | Plasma uniformity |
| CN102355792A (en) * | 2011-10-19 | 2012-02-15 | 中微半导体设备(上海)有限公司 | Electromagnetic coupling plasma device capable of improving uniformity and efficiency of plasma |
| JP2013234366A (en) * | 2012-05-09 | 2013-11-21 | Mitsubishi Plastics Inc | Method for producing gas barrier film |
| CN106011771A (en) * | 2016-08-04 | 2016-10-12 | 北京师范大学 | Apparatus for rapidly depositing DLC film on surface of piston ring, and method thereof |
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| CN106756868B (en) | 2019-07-09 |
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