CN102965619A - Preparation method of multi-metal doping hydrogen-free diamond carbon film - Google Patents
Preparation method of multi-metal doping hydrogen-free diamond carbon film Download PDFInfo
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- CN102965619A CN102965619A CN 201210519901 CN201210519901A CN102965619A CN 102965619 A CN102965619 A CN 102965619A CN 201210519901 CN201210519901 CN 201210519901 CN 201210519901 A CN201210519901 A CN 201210519901A CN 102965619 A CN102965619 A CN 102965619A
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Abstract
The invention discloses a preparation technology of a multi-metal doping hydrogen-free diamond carbon film. The preparation technology is characterized in that by using an ion beam auxiliary deposition technology, a multi-metal mosaic target (formed by mosaicking a mosaic block 2 in a sputtering region 3 on a base target material 1) and a graphite target are used for double-target sputtering, and the multi-metal doping hydrogen-free diamond film is deposited and prepared on the surface of a workpiece. The preparation technology comprises the following specific steps: preparing the mosaic target, cleaning and activating ions on the surface of the workpiece, and depositing and preparing the multi-metal doping hydrogen-free diamond film. Compared with the prior art, the film prepared by the method has the advantages of higher hardness, film-based bonding force, elasticity modulus, abrasion resistance and hot stability property; and doping components can be adjusted so that the film can meet the requirement of transmission parts of precise instruments for accuracy and increases the reliability of the transmission parts. The film is suitable for surface treatment of silicon and various metal workpieces.
Description
Technical field
The present invention relates to the surface treatment of material, specifically a kind of deposition preparation of multi-element metal doping non-hydrogen diamond membrane.
Background technology
Diamond like carbon film is as a kind of novel composite lubricating film material, have the hardness height, the excellent performance such as frictional coefficient is little, friction durability is long, in severe rugged environment, be used as protection film and shown huge application prospect in association areas such as accurate apparatus, MEMS (micro electro mechanical system), space environment parts as the composite lubricating film material.But because simultaneously it has the defectives such as high internal stress, poor heat stability, environmental factor dependence are strong, be subject in actual applications great limitation.Adopt the diamond like carbon film of modern technologies preparation mainly to be divided into two kinds of hydrogeneous class and not hydrogeneous classes, but relative non-hydrogen diamond membrane, it is lower to contain the hardness ratio of hydrogen diamond membrane own, internal stress is relative also lower, abrasion resistance properties is also relatively relatively poor under atmospheric condition, and therefore the preparation for non-hydrogen diamond is subject to extensive concern.
There are the problems such as fine and close not, that surface quality is poor in the prepared film of tradition quasi-diamond preparation means.As one of modern technique for preparing diamond like carbon film, ion beam assisted deposition carries out ion beam bombardment and mixes in vapour deposition, can effectively improve film performance, as improving the cohesive strength of diamond-film-like.Simultaneously, different metal mixes and can so that the characteristic of diamond like carbon film is well improved, keep simultaneously its many advantage.Can effectively reduce its internal stress and in dry air or vacuum, can show excellent tribological property such as the molybdenum doped diamond, but the tribological property in its wet environment descends to some extent.Tungsten doped diamond film can greatly improve the hardness of DLC film and reduce its internal stress, but simultaneously so that its frictional coefficient increase.Therefore the preparation that has the metal-doped diamond like carbon film of multiple excellent specific property seems particularly important.
The present invention utilizes ion beam assisted deposition to carry out the dual-target sputtering deposition, the metallic target that adopts is the embedded with metal target, guaranteed that various metals while Uniform Doped is in diamond like carbon film, film hardness is low when having overcome prior art and preparing film, film-substrate cohesion is poor, the shortcomings such as surfaceness height.The simultaneously adjusting by different parameters has guaranteed that the film of preparation has the good characteristic of different metal when mixing, and has kept the plurality of advantages of original film.Prepared diamond like carbon film surface compact degree is high, and roughness is low, and film quality is better; The depositing temperature of film is low, has avoided causing the diamond like carbon film greying owing to excess Temperature in deposition process, has good process controllability.
Summary of the invention
The objective of the invention is to overcome the shortcoming and defect that existing diamond like carbon film technology exists, a kind of preparation method of multi-element metal doping non-hydrogen diamond membrane is provided.It utilizes ion beam assisted deposition, use embedded with metal target and graphite target, under the auxiliary bombardment effect of second source, prepare multi-element metal doping non-hydrogen diamond membrane by ion beam sputter depositing, the high rigidity of diamond like carbon film and the characteristics of low-friction coefficient have not only been kept, abrasion resistance properties and thermostability have greatly been improved again, reduced the internal stress of film, it is high to have solved the diamond like carbon film internal stress, the problem of the poor and poor heat stability of film-substrate cohesion, the film of preparation has single metal-doped not available good overall characteristic simultaneously, can be widely used in the surface treatment of silicon and various metallic substance.
For achieving the above object, the present invention proposes a kind of deposition preparation of multi-element metal doping non-hydrogen diamond membrane, it is characterized in that: adopt the multi-element metal mosaic target, this mosaic target is in sputtering zone 3, use mosaic block 2 evenly to be embedded on the basic target 1 and consist of, the method may further comprise the steps successively:
Damascene target and high purity graphite targets that a, according to demand preparation difference form, and be installed on the rotary water-cooled target platform;
B, pending surface is carried out being fixed on the sample table of equipment vacuum chamber after clean the processing;
C, vacuum chamber is evacuated to base vacuum, continues to pass into reactant gases, gas passes into that gas pressure in vacuum keeps being stabilized in certain limit in the process;
D, unlatching Work piece rotary disc are opened ion source and second source, and sputter begins to deposit multi-element metal doping non-hydrogen diamond membrane after removing target and pending surface contaminant;
E, close Work piece rotary disc, take out sample after waiting temperature fully reduces.
Described mosaic block or and basic target form by metal-powder compacting, material is any metal in tungsten (W), molybdenum (Mo), iron (Fe), chromium (Cr), titanium (Ti), silver (Ag), copper (Cu), zirconium (Zr), the aluminium (Al).
Described mosaic block or and basic target form by metal-powder compacting, material is any metal in tungsten (W), molybdenum (Mo), iron (Fe), chromium (Cr), titanium (Ti), silver (Ag), copper (Cu), zirconium (Zr), the aluminium (Al).
Described mosaic target is embedded in basic target by mosaic block and consists of, and in the target as sputter zone, mosaic block is uniformly distributed on the basic target, and the sputter area equates that mosaic block can be that one or more mosaic blocks are evenly distributed on basic target mosaic area.
Described graphite target is purity greater than 99.97% high purity graphite target.
The clean treating processes in described pending surface comprises that effects on surface carries out polished finish, utilizes the clean and drying and processing of deionized water ultrasonic cleaning
Described base vacuum is 2 * 10
-4Pa, reactant gases can continue to pass in the gas process for any gas in argon gas (Ar), helium (He), neon (Ne), the Krypton (Kr) or the mixed gas of several gases, and the pressure in vacuum tank scope is 1.2 * 10
-2～1.5 * 10
-2Between the Pa.
Described plasma sputter source is Kaufman type ion source, and the plate voltage setting range is 2.0～3.5KV, ion beam current 20～100mA, and the working hour is 60min～180min, the sputtering source ionic fluid carries out sputtering sedimentation simultaneously to two targets in the deposition process.
Film preparation is carried out in the auxiliary bombardment of second source in the described ion source sputter deposition process, and second source is Kaufman type ion source, and second source voltage-regulation scope is 0.2～0.8KV, and beam current density is 20～100mA
Described abundant cooling is that temperature is near room temperature.
Metal-doped diamond like carbon film of the present invention has the performances such as higher film hardness, film-substrate cohesion, Young's modulus, abrasion resistance, thermal stability.Technique is workable, good reproducibility, and film performance is alternative strong, applicable to the wear-resistant processing of silicon and all kinds of surface of workpieces.
Description of drawings:
Fig. 1 is polynary embedded with metal target synoptic diagram.1 is basic target among the figure, and 2 is mosaic block, and 3 is the sputtering zone border.
Embodiment:
In order to understand better the present invention, describe by following specific embodiment.
Embodiment 1:
1, adopts tungsten mosaic target (tungsten is made basic target, and the mosaic block material is molybdenum);
2, the stainless steel substrates ultrasonic cleaning is clean, after the oven dry, be fixed on the work rest in the ion beam assisted depositing filming equipment vacuum chamber and vacuumize forvacuum to 2.0 * 10
-4Pa;
3, connect plasma sputter source and second source source of the gas, argon gas is passed into vacuum chamber, keep air pressure to be lower than 1.4 * 10
-2Pa, sputtering source adopts voltage 2.7KV, and the ion beam current of electric current 100mA bombards target; Second source adopts voltage 0.2KV, and line 100mA carries out Bombardment and cleaning and surface active to sample; Bombardment time is 10min.
4, sputtering source voltage 2.7KV, the ion beam current bombardment graphite target of ion beam current 75mA; Voltage 2.2KV, the ion beam current bombardment tungsten mosaic target of line 25mA, second source adopts voltage 0.2KV, and line 20mA is at workpiece surface deposition tungsten doping non-hydrogen diamond membrane, and depositing time is 120min.
5, deposition finishes, and closes the ion beam assisted depositing filming equipment, and keeps vacuum to treat the sample cooling, takes out sample when the sample table temperature is lower than 50 ℃, obtains W-DLC thin film at stainless steel substrates.
Prepared thicknesses of layers is 950nm, W content is 3.08%, molybdenum content is 5.02%, internal stress is 0.18GP, film-substrate cohesion is 70N, surfacing (surface undulation is less than 30nm), and nano hardness is 16.8GPa, the average friction coefficient that with the GCr15 steel couple is rubbed under atmospheric environment is 0.20, and the film wear rate is 1.68 * 10
-6Mm
3/ Nm.Film has good stainless property in the moist atmosphere environment simultaneously.
Embodiment 2:
1, adopts titanium chromium mosaic target (titanium is made basic target, and the mosaic block material is chromium);
2, the ultrasonic cleaning of high speed steel mould sheet is clean, after the oven dry, be fixed on the work rest in the ion beam assisted depositing filming equipment vacuum chamber and vacuumize forvacuum to 2.0 * 10
-4Pa;
3, connect plasma sputter source and second source source of the gas, argon gas is passed into vacuum chamber, keep air pressure to be lower than 1.5 * 10
-2Pa, sputtering source adopts voltage 2.7KV, and the ion beam current of electric current 100mA bombards target; Second source adopts voltage 0.2KV line 100mA that sample is carried out Bombardment and cleaning and surface active; Bombardment time is 10min.
3, sputtering source voltage 2.5KV, the ion beam current bombardment graphite target of ion beam current 80mA; Voltage 2.2KV, the ion beam current bombardment tungsten mosaic target of line 50mA, second source adopts voltage 0.4KV, and line 20mA is at workpiece surface deposition tungsten doping non-hydrogen diamond membrane, and depositing time is 150min.
4, deposition finishes, and closes the ion beam assisted depositing filming equipment, and keeps vacuum to treat the sample cooling, takes out sample when the sample table temperature is lower than 50 ℃, obtains W-DLC thin film at stainless steel substrates.
Prepared thicknesses of layers is about 1100nm, titanium content is 6.25%, chromium content is 6.47%, internal stress is 0.18GP, film-substrate cohesion is 86N, surfacing (surface undulation is less than 30nm), and nano hardness is 21.6GPa, the average friction coefficient that with the GCr15 steel couple is rubbed under atmospheric environment is 0.19, and the film wear rate is 0.94 * 10
-6Mm
3/ Nm.
Claims (9)
1. the deposition preparation of a multi-element metal doping non-hydrogen diamond membrane,, it is characterized in that: adopt the multi-element metal mosaic target, this mosaic target is in sputtering zone 3, use mosaic block 2 evenly to be embedded on the basic target 1 and consist of, the method may further comprise the steps successively:
Damascene target and high purity graphite targets that a, according to demand preparation difference form, and be installed on the rotary water-cooled target platform;
B, pending surface is carried out being fixed on the sample table of equipment vacuum chamber after clean the processing;
C, vacuum chamber is evacuated to base vacuum, continues to pass into reactant gases, gas passes into that gas pressure in vacuum keeps being stabilized in certain limit in the process;
D, unlatching Work piece rotary disc are opened ion source and second source, and sputter begins to deposit multi-element metal doping non-hydrogen diamond membrane after removing target and pending surface contaminant;
E, close Work piece rotary disc, take out sample after waiting temperature fully reduces.
2. the preparation method of multi-element metal doping non-hydrogen diamond membrane according to claim 1, it is characterized in that described mosaic block or and basic target form by metal-powder compacting, material is any metal in tungsten (W), molybdenum (Mo), iron (Fe), chromium (Cr), titanium (Ti), silver (Ag), copper (Cu), zirconium (Zr), the aluminium (Al).
3. the preparation method of multi-element metal doping non-hydrogen diamond membrane according to claim 1, it is characterized in that described mosaic target is embedded in basic target by mosaic block and consists of, in the target as sputter zone, mosaic block is uniformly distributed on the basic target and bi-material sputter area equates that mosaic block can be that one or more mosaic blocks are evenly distributed on basic target mosaic area.
4. the preparation method of multi-element metal doping non-hydrogen diamond membrane according to claim 1 is characterized in that described graphite target is purity greater than 99.97% high purity graphite target.
5. the preparation method of multi-element metal doping non-hydrogen diamond membrane according to claim 1 is characterized in that the clean treating processes in described pending surface comprises that effects on surface carries out polished finish, utilizes the clean and drying and processing of deionized water ultrasonic cleaning.
6. the preparation method of multi-element metal doping non-hydrogen diamond membrane according to claim 1 is characterized in that described base vacuum is 2 * 10
-4Pa, reactant gases can continue to pass in the gas process for any gas in argon gas (Ar), helium (He), neon (Ne), the Krypton (Kr) or the mixed gas of several gases, and the pressure in vacuum tank scope is 1.2 * 10
-2～1.5 * 10
-2Between the Pa.
7. the preparation method of multi-element metal doping non-hydrogen diamond membrane according to claim 1, it is characterized in that described plasma sputter source is Kaufman type ion source, the plate voltage setting range is 2.0～3.5KV, ion beam current 20～100mA, working hour is 60min～180min, and the sputtering source ionic fluid carries out sputtering sedimentation simultaneously to two targets in the deposition process.
8. the preparation method of multi-element metal doping non-hydrogen diamond membrane according to claim 1, it is characterized in that film preparation is carried out in the auxiliary bombardment of second source in the described ion source sputter deposition process, second source is Kaufman type ion source, second source voltage-regulation scope is 0.2～0.8KV, and beam current density is 20～100mA.
9. the preparation method of multi-element metal doping non-hydrogen diamond membrane according to claim 1 is characterized in that described abundant cooling is that temperature is near room temperature.
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| CN104294230A (en) * | 2014-10-09 | 2015-01-21 | 中国科学院宁波材料技术与工程研究所 | High-hardness and low-stress multi-element composite diamond-like coating and preparation method thereof |
| US20150376532A1 (en) * | 2014-06-30 | 2015-12-31 | Ihi Hauzer Techno Coating B.V. | Coating and Method for its Deposition to Operate in Boundary Lubrication Conditions and at Elevated Temperatures |
| CN105369199A (en) * | 2015-10-15 | 2016-03-02 | 南京理工大学 | Method for preparing frictional wear resisting and corrosion resisting carbon-based film |
| CN106756847A (en) * | 2016-12-21 | 2017-05-31 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of witch culture DLC film |
| CN108728802A (en) * | 2018-06-05 | 2018-11-02 | 湘潭大学 | Multilayer high temperature resistant Ti/Zr co-doped diamond coatings and preparation method thereof |
| CN109371375A (en) * | 2018-11-23 | 2019-02-22 | 东南大学 | A kind of diamond-like original position autoreaction is graphitized lubricant coating cutter and preparation method thereof |
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| CN113913735A (en) * | 2021-09-07 | 2022-01-11 | 广州今泰科技股份有限公司 | Vanadium/yttrium co-doped DLC coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20150376532A1 (en) * | 2014-06-30 | 2015-12-31 | Ihi Hauzer Techno Coating B.V. | Coating and Method for its Deposition to Operate in Boundary Lubrication Conditions and at Elevated Temperatures |
| CN104294230A (en) * | 2014-10-09 | 2015-01-21 | 中国科学院宁波材料技术与工程研究所 | High-hardness and low-stress multi-element composite diamond-like coating and preparation method thereof |
| CN105369199A (en) * | 2015-10-15 | 2016-03-02 | 南京理工大学 | Method for preparing frictional wear resisting and corrosion resisting carbon-based film |
| CN106756847B (en) * | 2016-12-21 | 2019-03-22 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of witch culture DLC film |
| CN106756847A (en) * | 2016-12-21 | 2017-05-31 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of witch culture DLC film |
| CN108728802A (en) * | 2018-06-05 | 2018-11-02 | 湘潭大学 | Multilayer high temperature resistant Ti/Zr co-doped diamond coatings and preparation method thereof |
| CN108728802B (en) * | 2018-06-05 | 2020-06-19 | 湘潭大学 | Multilayer high-temperature-resistant Ti/Zr co-doped diamond-like coating and preparation method thereof |
| CN109371375A (en) * | 2018-11-23 | 2019-02-22 | 东南大学 | A kind of diamond-like original position autoreaction is graphitized lubricant coating cutter and preparation method thereof |
| CN109609920A (en) * | 2019-01-09 | 2019-04-12 | 福建工程学院 | Anti- plug net screen printing screens of one kind and preparation method thereof |
| CN109609920B (en) * | 2019-01-09 | 2021-01-05 | 福建工程学院 | Anti-blocking screen printing plate and preparation method thereof |
| CN113403588A (en) * | 2020-03-16 | 2021-09-17 | 南京理工大学 | Preparation method of high-hardness high-wear-resistance silver-doped diamond infrared antireflection film |
| CN113403588B (en) * | 2020-03-16 | 2022-11-25 | 南京理工大学 | Preparation method of high-hardness high-wear-resistance silver-doped diamond infrared antireflection film |
| CN113913735A (en) * | 2021-09-07 | 2022-01-11 | 广州今泰科技股份有限公司 | Vanadium/yttrium co-doped DLC coating and preparation method thereof |
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Application publication date: 20130313 |