CN104928639A - Super tough carbon-based surface protection coating and preparation method thereof - Google Patents
Super tough carbon-based surface protection coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a super tough carbon-based surface protection coating and preparation method thereof. The coating is composed of carbon element, carbide-forming metal element and weak carbide-forming metal element. The carbon element exists in an amorphous mode in the coating to form a carbon amorphous network, the carbide-forming metal element combines with the carbon to form carbide nanometer particles, the weak carbide-forming metal element exists in a metal-state nanometer particles, the carbide nanometer particles and the metal nanometer particles are embedded in the carbon amorphous network, and amorphous carbon separation is conducted between the particles. When the super tough carbon-based surface protection coating is prepared, by bringing the carbide metal element and the weak carbide metal element in a carbon-based coating simultaneously, the flexibility and adhesive force of the coating are improved while the rigidity of the coating is improved and the stress is lowered, and the property of resistance to friction and wear and thermal endurance property of the coating are improved, so that the coating is more suitable for harsher environment, and a better surface protecting effect is achieved.
Description
Technical field
The present invention relates to a kind of carbon-base coating and preparation method thereof, belong to surface protection technique and related coating materials technical field.
Background technology
Along with industrial circle is to the requirement of the aspect such as energy-saving and emission-reduction, environment protection; and the high standard requirement of the aspect such as the high precision constantly promoted, high reliability and long lifetime; a new generation is energy-conservation, the industry field such as motor car engine, nuclear power mechanical sealing system, compressor oil-free lubricatoin system, textile manufacturing machine system, precision die, precision transmission system, bearing arrangement, machinofacture of consumption reduction, low-carbon type, invariably embodies the novel reinforced active demand with the integrated surface protection technique of lubrication.
Base coating (as diamond-like coating, amorphous carbon coating, class equadag coating) is class definition amorphous carbon material widely, primarily of the sp containing diamond phase
3hybrid bond and sp
2the three dimensional intersection network structure of the graphite cluster of key is formed, have and be similar to adamantine many excellent specific properties, as high rigidity, low-friction coefficient, abrasion resistant and corrosion resistant, wide transparency range, superior bio is compatible, is one of focus of low-friction surface technical field research always.But such as 1. toughness is low in carbon-base coating existence, fragility strong and poor heat stability; 2. heavily stressed and film base is in conjunction with weak; 3. the tribology behavior problem such as very large affected by environment, remains the critical bottleneck of such membrane life time of restriction and reliability.Under envrionment conditions complicated and changeable and special operation condition, how to play the advantage of such thin-film material, become the key technical problem being badly in need of solving.
Prior art is compared, the invention has the advantages that: in carbon-base coating, introduce carbide metal element and weak carbide metal element simultaneously, while raising coating hardness, reduction stress, strengthen snappiness and the sticking power of coating, improve coating wear Characteristics and thermal stability, coating is made to be more suitable for harsher applied environment, as the protection of the product surface such as component of machine, knife mold.
Summary of the invention
The object of the invention is to provide a kind of low-stress, high-strong toughness for above-mentioned the deficiencies in the prior art, friction is stable, the combination of film base is strong, can be applied to the carbon back protective coating of the product surface such as component of machine, knife mold.
Another object of the present invention is the preparation method providing above-mentioned a kind of carbon back protective coating.
The technical solution adopted in the present invention is: a kind of superpower hard carbon primary surface protective coating, this coating is elementary composition by carbon, carbide-forming metal element, weak carbide-forming metal, in coating, the atom percentage content of carbide-forming metal element is 5 ~ 20%, the atom percentage content of weak carbide-forming metal element is 5 ~ 20%, and surplus is carbon; In coating, carbon exists with decolorizing carbon form, forms the amorphous network of carbon, carbide-forming metal element is combined with carbon and forms carbide nanoparticles, its size is 5 ~ 10nm, and weak carbide-forming metal element exists with metallic state nano particle, and its size is 5 ~ 10nm; Carbide nanoparticles and metal nanoparticle are embedded in the amorphous network structure of carbon, are separated between particle with particle by decolorizing carbon, and between particle, average headway is 10 ~ 20nm.
Described carbide metal element is titanium or chromium or tungsten.
Described weak carbide forming element is copper or cobalt or nickel.
The preparation of superpower tough carbon-base coating of the present invention, adopt ionic fluid combined magnetic-controlled sputter coating equipment to carry out, described ionic fluid combined magnetic-controlled sputter coating equipment is made up of a vacuum chamber, two controlled sputtering sources, ion sources and the work support that can rotate simultaneously, work support is arranged on internal vacuum chamber, described two controlled sputtering sources all can load different metal targets, and concrete steps prepared by described carbon-base coating are as follows:
(1) ion beam etching: be placed in by matrix on the work support of vacuum chamber, vacuum chamber, to vacuum tightness 5.0 × 10
-3below Pa, open ion source, pass into 50 ~ 100sccm argon gas to ion source, arrange ion source power 0.6 ~ 0.8KW, arrange work support bias voltage 500 ~ 800V, the working hour is 30 minutes;
(2) deposit superpower tough carbon-base coating: open ion source, two controlled sputtering sources, two controlled sputtering sources load different, that purity is greater than 99.99% elemental metals target respectively simultaneously; Pass into hydrocarbon gas and argon gas to vacuum chamber simultaneously, control the overall air pressure 0.8 ~ 2Pa of vacuum chamber; Arranging ion source power is 0.8 ~ 1KW, magnetron sputtering power 1 ~ 2KW; The bias voltage of matrix is set to 100 ~ 300V, depositing time is 2 ~ 3 hours simultaneously;
(3) powered-down, treats that vacuum chamber temperature is down to room temperature, and open vacuum chamber and take out matrix, the coating formed at matrix surface is described superpower tough carbon-base coating;
Wherein, the described elemental metals target of step (2) is: simple substance titanium target or simple substance chromium target or simple substance tungsten target or elemental copper target or simple substance cobalt target or elemental nickel target; Described hydrocarbon gas is acetylene or methane gas.
In preferred described step (2), two controlled sputtering sources load different, that purity is greater than the elemental metals target of 99.99% mode respectively: controlled sputtering source loads simple substance titanium target or the purity simple substance chromium target or the purity simple substance tungsten target that is greater than 99.99% that are greater than 99.99% that purity is greater than 99.99%, and another controlled sputtering source loads elemental copper target or the purity simple substance cobalt target or the purity elemental nickel target that is greater than 99.99% that are greater than 99.99% that purity is greater than 99.99%.
Preferred further, the volume ratio of described hydrocarbon gas and argon gas is 1 ~ 4:9 ~ 6, and namely hydrocarbon gas accounts for and passes into 10% ~ 40% of vacuum chamber volume of gas.
The preparation method of carbon-base coating of the present invention also comprises following pre-treatment step: before ion beam etching step, utilizes alcohol ultrasonic cleaning matrix, then uses rinsed with deionized water, then dry up by dried compressed air.
Matrix described in technical solution of the present invention refers to sample to be coated, and namely method of the present invention is applicable but be not limited to as the surfacecti proteon of metal machinery component, precision die, precision drive mechanical means, bearing, electronic product, decorative product and material.
Accompanying drawing explanation
Fig. 1 is coating structure schematic diagram of the present invention, and wherein, pentagon represents metal nanoparticle 1, and hexagon represents carbide nanoparticles 2, and rest part is amorphous carbon structure region 3.
Fig. 2 is carbon-base coating nano indentation test figure prepared in the embodiment of the present invention 1.
Embodiment
Below in conjunction with accompanying drawing and case study on implementation, the present invention is described in further detail.
Embodiment 1 follows these steps to realize the present invention:
1, composite film coating machine prepares: this enforcements is selected to adopt ionic fluid combined magnetic-controlled sputter coating equipment, comprise a vacuum chamber, two controlled sputtering sources, an ion source and while revolvable work support, work support is arranged on internal vacuum chamber; Two controlled sputtering sources load respectively purity be 99.99% titanium target and purity be 99.99% copper target;
2, sample (matrix) pre-washing process: utilize alcohol ultrasonic cleaning sample to be coated (matrix), then use rinsed with deionized water, dry up by dried compressed air;
3, ion beam etching is utilized to clean sample surfaces in a vacuum chamber: to be placed in by matrix on the work support of vacuum chamber, by vacuum chamber to 5.0 × 10
-3below Pa, open ion source, pass into 100sccm argon gas to ion source, arrange ion source power 0.6KW, arrange work support bias voltage 800V, the working hour is 30 minutes;
4, the metal-doped superpower tough carbon-base coating preparation of Cu and Ti: the magnetron sputtering opened ion source simultaneously, be equipped with the magnetron sputtering of simple substance titanium target, be equipped with elemental copper target, pass into acetylene and argon gas (volume ratio of acetylene and argon gas is 1:9) to vacuum chamber simultaneously, acetylene accounts for 10% of volume of gas, controls overall air pressure 1Pa; Arranging ion source power is 1KW, magnetron sputtering power 2KW; The bias voltage of matrix is set to 300V, and depositing time is 2 hours;
5, powered-down, treats that vacuum chamber temperature is down to room temperature, and open vacuum chamber and take out matrix, this matrix surface forms superpower tough carbon-base coating.
In the coating formed, the atom percentage content of carbide-forming metal element titanium is 20%, the atom percentage content of weak carbide-forming metal elemental copper is 20%, and the atom percentage content of carbon is 60%; In coating, carbon exists with decolorizing carbon form, forms the amorphous network of carbon, carbide-forming metal element is combined with carbon and forms carbide nanoparticles, its size is 5 ~ 10nm, and weak carbide-forming metal element exists with metallic state nano particle, and its size is 5 ~ 10nm; Carbide nanoparticles and metal nanoparticle are embedded in the amorphous network structure of carbon, are separated between particle with particle by decolorizing carbon, and between particle, average headway is 10nm.
Through unrelieved stress, scratching instrument test, nano-indenter test (as shown in Figure 2), the unrelieved stress of prepared Ti and Cu doping carbon-base coating is 0.3GPa, coating adhesion property is excellent, film/base critical load reaches 10GPa, hardness is 30GPa, coatings goes out excellent snappiness simultaneously, and elastic resilience reaches 50%.
Embodiment 2 follows these steps to realize the present invention:
1, composite film coating machine prepare: this enforcements select adopt ionic fluid combined magnetic-controlled sputter coating equipment, comprise a vacuum chamber, two controlled sputtering sources, an ion source and while revolvable work support, work support is arranged on internal vacuum chamber; Two controlled sputtering sources load respectively purity be 99.99% chromium target and purity be 99.99% cobalt target;
2, sample (matrix) pre-washing process: utilize alcohol ultrasonic cleaning sample to be coated (matrix), then use rinsed with deionized water, dry up by dried compressed air;
3, ion beam etching is utilized to clean sample surfaces in a vacuum chamber: to be placed in by matrix on the work support of vacuum chamber, by vacuum chamber to 3.0 × 10
-3pa, open ion source, pass into 80sccm argon gas to ion source, arrange ion source power 0.6KW, arrange work support bias voltage 700V, the working hour is 30 minutes;
4, chromium and the metal-doped superpower tough carbon-base coating preparation of cobalt: the magnetron sputtering opened ion source simultaneously, be equipped with the magnetron sputtering of simple substance chromium target, be equipped with simple substance cobalt target, pass into methane and argon gas (volume ratio of methane and argon gas is 1:9) to vacuum chamber simultaneously, methane accounts for 10% of volume of gas, controls overall air pressure 1.5Pa; Arranging ion source power is 0.8KW, magnetron sputtering power 1KW; The bias voltage of matrix is set to 300V, and depositing time is 2.5 hours;
5, powered-down, treats that vacuum chamber temperature is down to room temperature, and open vacuum chamber and take out matrix, this matrix surface forms superpower tough carbon-base coating.
In the coating formed, the atom percentage content of carbide-forming metal elemental chromium is 10%, the atom percentage content of weak carbide-forming metal element cobalt is 15%, and the atom percentage content of carbon is 75%; In coating, carbon exists with decolorizing carbon form, forms the amorphous network of carbon, carbide-forming metal element is combined with carbon and forms carbide nanoparticles, its size is 5 ~ 10nm, and weak carbide-forming metal element exists with metallic state nano particle, and its size is 5 ~ 10nm; Carbide nanoparticles and metal nanoparticle are embedded in the amorphous network structure of carbon, are separated between particle with particle by decolorizing carbon, and between particle, average headway is 15nm.
Embodiment 3 follows these steps to realize the present invention:
1, composite film coating machine prepare: this enforcements select adopt ionic fluid combined magnetic-controlled sputter coating equipment, comprise a vacuum chamber, two controlled sputtering sources, an ion source and while revolvable work support, work support is arranged on internal vacuum chamber; Two controlled sputtering sources load respectively purity be 99.99% tungsten target and purity be 99.99% nickel target;
2, sample (matrix) pre-washing process: utilize alcohol ultrasonic cleaning sample to be coated (matrix), then use rinsed with deionized water, dry up by dried compressed air;
3, ion beam etching is utilized to clean sample surfaces in a vacuum chamber: to be placed in by matrix on the work support of vacuum chamber, by vacuum chamber to 4.0 × 10
-3pa, open ion source, pass into 50sccm argon gas to ion source, arrange ion source power 0.7KW, arrange work support bias voltage 600V, the working hour is 30 minutes;
4, tungsten and the metal-doped superpower tough carbon-base coating preparation of nickel: the magnetron sputtering opened ion source simultaneously, be equipped with the magnetron sputtering of simple substance tungsten target, be equipped with elemental nickel target, pass into acetylene and argon gas (volume ratio of acetylene and argon gas is 4:6) to vacuum chamber simultaneously, acetylene accounts for 40% of volume of gas, controls overall air pressure 0.8Pa; Arranging ion source power is 0.8KW, magnetron sputtering power 1.5KW; The bias voltage of matrix is set to 100V, and depositing time is 3 hours;
5, powered-down, treats that vacuum chamber temperature is down to room temperature, and open vacuum chamber and take out matrix, this matrix surface forms superpower tough carbon-base coating.
In the coating formed, the atom percentage content of carbide-forming metal elemental tungsten is 12%, the atom percentage content of weak carbide-forming metal elemental nickel is 5%, and the atom percentage content of carbon is 83%; In coating, carbon exists with decolorizing carbon form, forms the amorphous network of carbon, carbide-forming metal element is combined with carbon and forms carbide nanoparticles, its size is 5 ~ 10nm, and weak carbide-forming metal element exists with metallic state nano particle, and its size is 5 ~ 10nm; Carbide nanoparticles and metal nanoparticle are embedded in the amorphous network structure of carbon, are separated between particle with particle by decolorizing carbon, and between particle, average headway is 20nm.
Embodiment 4 follows these steps to realize the present invention:
1, composite film coating machine prepare: this enforcements select adopt ionic fluid combined magnetic-controlled sputter coating equipment, comprise a vacuum chamber, two controlled sputtering sources, an ion source and while revolvable work support, work support is arranged on internal vacuum chamber; Two controlled sputtering sources load respectively purity be 99.99% tungsten target and purity be 99.99% copper target;
2, sample (matrix) pre-washing process: utilize alcohol ultrasonic cleaning sample to be coated (matrix), then use rinsed with deionized water, dry up by dried compressed air;
3, ion beam etching is utilized to clean sample surfaces in a vacuum chamber: to be placed in by matrix on the work support of vacuum chamber, by vacuum chamber to 3.5 × 10
-3pa, open ion source, pass into 90sccm argon gas to ion source, arrange ion source power 0.8KW, arrange work support bias voltage 500V, the working hour is 30 minutes;
4, tungsten and the metal-doped superpower tough carbon-base coating preparation of copper: the magnetron sputtering opened ion source simultaneously, be equipped with the magnetron sputtering of simple substance tungsten target, be equipped with elemental copper target, simultaneously pass into methane to vacuum chamber and argon gas (volume ratio of methane and argon gas is 2:8) methane accounts for 20% of volume of gas, control overall air pressure 2Pa; Arranging ion source power is 1KW, magnetron sputtering power 2KW; The bias voltage of matrix is set to 200V, and depositing time is 2 hours;
5, powered-down, treats that vacuum chamber temperature is down to room temperature, and open vacuum chamber and take out matrix, this matrix surface forms superpower tough carbon-base coating.
In the coating formed, the atom percentage content of carbide-forming metal elemental tungsten is 5%, the atom percentage content of weak carbide-forming metal elemental copper is 10%, and the atom percentage content of carbon is 85%; In coating, carbon exists with decolorizing carbon form, forms the amorphous network of carbon, carbide-forming metal element is combined with carbon and forms carbide nanoparticles, its size is 5 ~ 10nm, and weak carbide-forming metal element exists with metallic state nano particle, and its size is 5 ~ 10nm; Carbide nanoparticles and metal nanoparticle are embedded in the amorphous network structure of carbon, are separated between particle with particle by decolorizing carbon, and between particle, average headway is 18nm.
Claims (7)
1. a superpower tough carbon-base coating, it is characterized in that: this coating is elementary composition by carbon, carbide-forming metal element, weak carbide-forming metal, in coating, the atom percentage content of carbide-forming metal element is 5 ~ 20%, the atom percentage content of weak carbide-forming metal element is 5 ~ 20%, and surplus is carbon; In coating, carbon exists with decolorizing carbon form, forms the amorphous network of carbon, carbide-forming metal element is combined with carbon and forms carbide nanoparticles, its size is 5 ~ 10nm, and weak carbide-forming metal element exists with metallic state nano particle, and its size is 5 ~ 10nm; Carbide nanoparticles and metal nanoparticle are embedded in the amorphous network structure of carbon, are separated between particle with particle by decolorizing carbon, and between particle, average headway is 10 ~ 20nm.
2. superpower tough carbon-base coating according to claim 1, is characterized in that: described carbide metal element is titanium or chromium or tungsten.
3. superpower tough carbon-base coating according to claim 1, is characterized in that: described weak carbide forming element is copper or cobalt or nickel.
4. the preparation method of a superpower tough carbon-base coating according to claim 1, it is characterized in that: adopt ionic fluid combined magnetic-controlled sputter coating equipment to carry out, described ionic fluid combined magnetic-controlled sputter coating equipment is made up of a vacuum chamber, two controlled sputtering sources, ion sources and the work support that can rotate simultaneously, work support is arranged on internal vacuum chamber, described two controlled sputtering sources all can load different metal targets, and concrete steps prepared by described carbon-base coating are as follows:
(1) ion beam etching: be placed in by matrix on the work support of vacuum chamber, vacuum chamber is to vacuum tightness 5.0 × 10
-3below Pa, open ion source, pass into 50 ~ 100sccm argon gas to ion source, arrange ion source power 0.6 ~ 0.8KW, arrange work support bias voltage 500 ~ 800V, the working hour is 30 minutes;
(2) deposit superpower tough carbon-base coating: open ion source, two controlled sputtering sources, two controlled sputtering sources load different, that purity is greater than 99.99% elemental metals target respectively simultaneously; Pass into hydrocarbon gas and argon gas to vacuum chamber simultaneously, control the overall air pressure 0.8 ~ 2Pa of vacuum chamber; Arranging ion source power is 0.8 ~ 1KW, magnetron sputtering power 1 ~ 2KW; The bias voltage of matrix is set to 100 ~ 300V, and depositing time is 2 ~ 3 hours;
(3) powered-down, treats that vacuum chamber temperature is down to room temperature, and open vacuum chamber and take out matrix, the coating formed at matrix surface is described superpower tough carbon-base coating;
Wherein, the described elemental metals target of step (2) is: simple substance titanium target or simple substance chromium target or simple substance tungsten target or elemental copper target or simple substance cobalt target or elemental nickel target; Described hydrocarbon gas is acetylene or methane gas.
5. the preparation method of superpower tough carbon-base coating according to claim 4, it is characterized in that: in described step (2), two controlled sputtering sources load different, that purity is greater than the elemental metals target of 99.99% mode respectively: controlled sputtering source loads simple substance titanium target or the purity simple substance chromium target or the purity simple substance tungsten target that is greater than 99.99% that are greater than 99.99% that purity is greater than 99.99%, and another controlled sputtering source loads elemental copper target or the purity simple substance cobalt target or the purity elemental nickel target that is greater than 99.99% that are greater than 99.99% that purity is greater than 99.99%.
6. the preparation method of superpower tough carbon-base coating according to claim 4, is characterized in that: the volume ratio of described hydrocarbon gas and argon gas is 1 ~ 4:9 ~ 6.
7. the preparation method of superpower tough carbon-base coating according to claim 4, it is characterized in that: the method also comprises following pre-treatment step: before ion beam etching step, utilize alcohol ultrasonic cleaning matrix, then use rinsed with deionized water, then dry up by dried compressed air.
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| CN113039602A (en) * | 2018-11-06 | 2021-06-25 | 新加坡国立大学 | Two-dimensional amorphous carbon as overcoat for thermally-assisted magnetic recording media |
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