CN108504993A - A kind of Cu-Mo gradient films material and preparation method thereof - Google Patents
A kind of Cu-Mo gradient films material and preparation method thereof Download PDFInfo
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- CN108504993A CN108504993A CN201810335076.8A CN201810335076A CN108504993A CN 108504993 A CN108504993 A CN 108504993A CN 201810335076 A CN201810335076 A CN 201810335076A CN 108504993 A CN108504993 A CN 108504993A
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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Abstract
The invention discloses a kind of Cu Mo gradient film materials and preparation method thereof, the method is using business copper foil or soda-lime glass as substrate, using high-purity copper target material, molybdenum target material as sputter material, high-vacuum multi-target magnetic control sputtering equipment is to prepare tool, sputtering power by fixing copper target target position sputtering power, change molybdenum target target position during cosputtering deposits realizes the adjusting of copper, molybdenum relative amount in membrane material, the thickness for preparing film is controlled by changing the cosputtering time, is finally prepared for the Cu Mo gradient film materials of variable thickness.The features such as the method for the invention preparation flow is short, easy to operate, and state modulator range is wide, easy to implement, and Thickness of Gradient Layer can be controlled arbitrarily has good Commercial Prospect.
Description
Technical field
The present invention relates to gradient film field of material preparation, and in particular to a kind of to prepare binary conjunction using magnetron sputtering technique
The method of golden gradient film material more particularly to a kind of double target magnetic control sputterings of utilization high vacuum prepare Cu-Mo gradient film materials
Method.
Background technology
Functionally gradient material (FGM) is the material for selecting two kinds of (or a variety of) performances different, by continuously changing both (or a variety of) materials
The Nomenclature Composition and Structure of Complexes of material makes its interface disappear, and the performance of material is caused slowly to become with the variation of the Nomenclature Composition and Structure of Complexes of material
Change.Due to functionally gradient material (FGM) component on certain direction in space consecutive variations, be not present sharp interface, so between adjacent layer
Performance is similar, and the performance of material entirety is in consecutive variations.Functionally gradient material (FGM) may be used as boundary layer to connect two kinds of incompatible materials
Material, greatly improves adhesion strength, is also used as boundary layer and reduces residual stress and thermal stress, while eliminating in connecting material
The Stress singularity of interface crosspoint and the free endpoint of stress；Traditional homogeneous material is replaced with functionally gradient material (FGM), can both be increased
Strong ties intensity can also reduce cracks deflection and bridge.
Currently, Cu based gradient materials are mainly made with Cu and another metal material.Prepare the side of Cu based gradient materials
Method is more, such as discharge plasma sintering, hot pressed sintering, electro-deposition, vapor deposition and self-propagating high-temperature synthesis.Pass through difference
Method synthesizes copper and another material laminate to obtain functionally gradient material (FGM) so that material had both had high mechanical strength and good tough
Property, and there is good tribological property and electric conductivity, the sliding material tool of electric energy is imported from contact net lines as electric locomotive
There is good application background.Meanwhile as functionally gradient material (FGM), the faying face between both materials is in gradual transition, face and face it
Between composition transfer it is smaller, effectively reduce the thermal stress between both sides, reduce material in use due to thermal stress
The probability for mismatching and crackle being caused to generate, extends the materials'use service life.
As the fast development of global economy is deposited in the industry such as oil, chemical industry, the energy, electric power, metallurgy, aerospace
In the fricting movement pair parts largely used under the adverse circumstances such as high temperature, corrosion, material is not required nothing more than with good resistance to
Mill property, corrosion resistance and oxidation resistance, it is also necessary to have excellent obdurability.And the homogenous material that property is uniform, it is often difficult to full
The above-mentioned field with a variety of application requirements of foot.
Magnetron sputtering technique is to be intended to the material that deposition forms a film the cathode that target is placed in sputtering depositing system is made, to be sputtered
System is filled with argon gas and specific reaction gas after being evacuated to high vacuum（Can there is no reaction gas）；Gas ionizes to be formed under high pressure
Plasma be accelerated under the action of electric field and alternating magnetic field, it is former that bombardment target material surface causes the atom of target material surface to be detached from
Lattice escapes, and is transferred to the matrix surface of anode sample stage and deposits film forming.The characteristics of magnetron sputtering is rate of film build height, substrate
Temperature is low, and the adhesiveness of film is good, it can be achieved that large-area coating film.By installing the target of unlike material in different target position, utilize
Multi-target magnetic control sputtering, so that it may obtain the membrane material of different constituent elements.With the relative amount of constituent element in the thin-film material of this method preparation
It is related from deposition rate of the different target position targets in substrate.And the deposition rate of certain constituent element depends on the property of the constituent element itself
Matter, the sputtering power of place target position and place target position target plane center are at a distance from deposited samples platform center.In this way, passing through
The sputtering power and target plane center for changing target position achieve that constituent element in membrane material at a distance from deposited samples platform center
The adjusting of relative amount.These features of multi-target magnetic control sputtering technology are adapted for being used to prepare gradient film material.
Invention content
The technical problem to be solved in the present invention is to provide a kind of Cu-Mo alloys gradient film material；The present invention also provides
A kind of side of low cost, simple for process preparing Cu-Mo gradient film materials using the double target magnetic control sputtering technologies of high vacuum
Method.
In order to achieve the above object, the technical solution adopted in the present invention is as follows：
In copper foil substrate or soda-lime glass substrate, the double targets of magnetron sputtering are co-deposited Cu-Mo films, while magnetron sputtering
In-situ annealing under the conditions of 350 DEG C；Under the premise of target plane center is fixed at a distance from deposited samples platform center, by changing
The sputtering power for becoming two target position adjusts the relative amount of copper and molybdenum in Cu-Mo films；What is contacted with substrate is internal layer pure copper layer,
Gradient layer from inside to outside for copper content gradually decreases and molybdenum content gradually rises.
Double targets are copper target and molybdenum target, and the copper content of copper target is more than the amount containing molybdenum of 99.99%, molybdenum target more than 99.99%.
The copper-based bottom is the business copper foil of 9 μm of thickness, and area can be in cm × 10 the cm ~ 10 of 5 cm × 5
Change between cm；The soda-lime glass substrate is the common soda lime glass of 100 μm of thickness, and area is the cm of 5 cm × 5.
Preferably, the condition of the magnetron sputtering is：Planar central where copper target is 8 apart from deposited samples platform centre distance
~ 10 cm, planar central is 4 ~ 6 cm apart from deposited samples platform centre distance where molybdenum target, is remained unchanged during cosputtering.
Preferably, the condition of the magnetron sputtering is：The sputtering power of copper target is arranged between 25 ~ 50 W and in cosputtering
It remains unchanged in the process；The initial sputter power setting of molybdenum target is between 25 ~ 75 W, according to Mo in Cu-Mo bianry alloy films
The graded of content requires that the sputtering power for increasing molybdenum target, sputtering power adjustable range can be adjusted during cosputtering to be 25 ~ 175
W。
Preferably, the condition of the magnetron sputtering is：The back end vacuum degree that sputter chamber is reached is not less than 1.0 × 10-4
The work ar pressure of Pa, cosputtering are 1.0 Pa or so, and the rotary speed of substrate is 15 r/ min.
Preferably, the condition of the magnetron sputtering is：After copper target sputters at least 10 min, then start being total to for copper target and molybdenum target
Sputtering.Copper target, which first sputters certain time one side, can form ultra-thin articulamentum, reinforce the attachment force of co-sputtered thin films and substrate；
On the other hand the pure copper layer of Cu-Mo gradient film materials can be formed.
Preferably, annealing process of the invention is：350 DEG C of in-situ annealings during cosputtering, to eliminate co-deposition process
The stress of middle generation prevents the generation of micro-crack.
The present invention step be：
（1）Surface polishing bright copper target and molybdenum target are placed in two d.c. sputtering target position of high vacuum magnetic control sputtering system
On；Planar central where adjusting copper target is 8 ~ 10 cm apart from deposited samples platform centre distance, and planar central distance is heavy where molybdenum target
Product sample stage centre distance is 4 ~ 6 cm, is remained unchanged during cosputtering.
（2）Copper foil substrate or soda-lime glass substrate are cleaned by ultrasonic the organic matter that 5 min remove remained on surface using acetone,
Then 5 min are cleaned by ultrasonic to copper foil substrate dilute hydrochloric acid and remove oxide on surface, finally use absolute ethyl alcohol to remove surface residual
The solion stayed and rapid draing.
（3）Copper foil substrate or soda-lime glass substrate are transferred to magnetron sputtering apparatus substrate sample platform centre, with double
It leads copper foil tape to fix, closes magnetron sputtering reaction chamber, carry out vacuum pumping.
（4）It is 1.0 × 10 to be extracted into back end vacuum-4Pa is passed through argon gas with default 20sccm flows, and fine tuning argon flow amount is extremely
Air pressure is 1.0 Pa or so in sputtering system cavity, and sample stage rotating speed is transferred to 15 r/min, and sample stage temperature is before starting sputtering
Rise to 350 DEG C.
（5）The sputtering power setting of copper target remains unchanged between 25 ~ 50 W and during cosputtering；Molybdenum target it is initial
Sputtering power is arranged between 25 ~ 75 W.
（6）Copper target starts after sputtering at least 10 min, opens molybdenum target, starts the cosputtering of copper target and molybdenum target.According to waiting making
The graded of standby Cu-Mo bianry alloys film thickness and wherein Cu, Mo content requires, and is spaced during cosputtering certain
Time tune increases the sputtering power of molybdenum target, and sputtering power adjustable range is 25 ~ 175 W.
（7）After cosputtering deposits, keeps air pressure in sputtering system cavity, sample stage rotating speed to be transferred to 0, close sample stage
Heating power supply when being cooled to 50 DEG C or less, opens cavity, removes prepared sample.
The beneficial effects of the present invention are：
（1）The present invention provides a kind of copper that the thickness deposited in bulk substrate using the double target magnetic control sputtering technologies of high vacuum is controllable
Molybdenum alloy gradient film material, copper molybdenum alloy gradient film scantling prepared by such method is controllable, thickness is controllable, ingredient can
It adjusts, large area, large-scale use can be met.Film dimensions can be controlled by size of foundation base；Film thickness is 1 μm ~ 50 μ
M can be adjusted by controlling the time of cosputtering；The changes of contents section of Cu is 50% ~ 100% in film, can be by changing molybdenum
The sputtering power of target is adjusted.
（2）The present invention selects copper foil or soda-lime glass as base material, in inert gas shielding in magnetron sputtering process
Under to magnetron sputtering formed copper molybdenum alloy film carry out in-situ annealing, improve metallic matrix and Coating Materials cohesive force, and
Reduce the generation of micro-crack.
（3）Copper molybdenum alloy gradient film material is prepared using magnetically controlled sputter method, easy to operate, highly practical, at low cost,
Controllability is stronger, the application prospect with large-scale commercialized production.
Specific implementation mode
The following is specific embodiments of the present invention, and technical scheme of the present invention is further described, but of the invention
Protection domain be not limited to these examples.It is every to be included in this hair without departing substantially from the change of present inventive concept or equivalent substitute
Within bright protection domain.
Embodiment 1：The preparation method of this Cu-Mo gradient film materials uses following concrete technologies.
（1）Surface polishing bright copper target and molybdenum target are placed in two d.c. sputtering targets of high vacuum magnetic control sputtering system
On position；Planar central where adjusting copper target is 8 cm apart from deposited samples platform centre distance, and planar central distance is heavy where molybdenum target
Product sample stage centre distance is 4 cm, is remained unchanged during cosputtering.
（2）The business copper foil bought is cut into the cm of 5 cm × 5 sizes as substrate, copper foil substrate uses acetone ultrasound
The organic matter that 5 min remove remained on surface is cleaned, being then cleaned by ultrasonic 5 min with dilute hydrochloric acid removes oxide on surface, finally makes
Solion and the rapid draing of remained on surface are removed with absolute ethyl alcohol.
（3）Copper foil substrate is transferred to magnetron sputtering apparatus substrate sample platform centre, is fixed with double copper foil tapes of leading,
Magnetron sputtering reaction chamber is closed, vacuum pumping is carried out.
（4）It is 1.0 × 10 to be extracted into back end vacuum-4Pa is passed through argon gas with default 20sccm flows, and fine tuning argon flow amount is extremely
Air pressure is 1.0 Pa or so in sputtering system cavity, and sample stage rotating speed is transferred to 15 r/min, and sample stage temperature is before starting sputtering
Rise to 350 DEG C.
（5）The sputtering power setting of copper target is remained unchanged in 25 W and during cosputtering；The initial sputter work(of molybdenum target
Rate is arranged in 25 W.
（6）Copper target starts after sputtering 1 h, opens molybdenum target, starts the cosputtering of copper target and molybdenum target.After 1 h of cosputtering, adjusts and increase
Molybdenum target sputtering power continues cosputtering to 50 W；Again after 1 h of cosputtering, adjusts and increase molybdenum target sputtering power to 100 W, continue to splash altogether
It penetrates；Again after 1 h of cosputtering, adjusts and increase molybdenum target sputtering power to 150 W, continue cosputtering；After 1 h of cosputtering, shielding power supply is closed.
（7）After cosputtering deposits, keeps air pressure in sputtering system cavity, sample stage rotating speed to be transferred to 0, close sample stage
Heating power supply when being cooled to 50 DEG C or less, opens cavity, removes prepared sample, you can obtains the Cu-Mo gradients
Thin-film material.
Embodiment 2：The preparation method of this Cu-Mo gradient film materials uses following concrete technologies.
（1）Surface polishing bright copper target and molybdenum target are placed in two d.c. sputtering targets of high vacuum magnetic control sputtering system
On position；Planar central where adjusting copper target is 10 cm apart from deposited samples platform centre distance, and planar central distance is heavy where molybdenum target
Product sample stage centre distance is 6 cm, is remained unchanged during cosputtering.
（2）Soda-lime glass substrate is cleaned by ultrasonic the organic matter that 5 min remove remained on surface using acetone, then uses nothing
Water-ethanol removes the solion of remained on surface and rapid draing.
（3）Soda-lime glass substrate is transferred to magnetron sputtering apparatus substrate sample platform centre, copper foil tape is led with double
It is fixed, magnetron sputtering reaction chamber is closed, vacuum pumping is carried out.
（4）It is 1.0 × 10 to be extracted into back end vacuum-4Pa is passed through argon gas with default 20sccm flows, and fine tuning argon flow amount is extremely
Air pressure is 1.0 Pa or so in sputtering system cavity, and sample stage rotating speed is transferred to 15 r/min, and sample stage temperature is before starting sputtering
Rise to 350 DEG C.
（5）The sputtering power setting of copper target is remained unchanged in 50 W and during cosputtering；The initial sputter work(of molybdenum target
Rate is arranged in 75 W.
（6）Copper target starts after sputtering 1 h, opens molybdenum target, starts the cosputtering of copper target and molybdenum target.After 1 h of cosputtering, adjusts and increase
Molybdenum target sputtering power continues cosputtering to 125 W；Again after 1 h of cosputtering, adjusts and increase molybdenum target sputtering power to 175 W, continue to splash altogether
It penetrates；After 1 h of cosputtering, shielding power supply is closed.
（7）After cosputtering deposits, keeps air pressure in sputtering system cavity, sample stage rotating speed to be transferred to 0, close sample stage
Heating power supply when being cooled to 50 DEG C or less, opens cavity, removes prepared sample, you can obtains the Cu-Mo gradients
Thin-film material.
Embodiment 3：The preparation method of this Cu-Mo gradient film materials uses following concrete technologies.
（1）Surface polishing bright copper target and molybdenum target are placed in two d.c. sputtering targets of high vacuum magnetic control sputtering system
On position；Planar central where adjusting copper target is 8 cm apart from deposited samples platform centre distance, and planar central distance is heavy where molybdenum target
Product sample stage centre distance is 5 cm, is remained unchanged during cosputtering.
（2）The business copper foil bought is cut into the cm of 10 cm × 10 sizes as substrate, copper foil substrate is super using acetone
Sound cleans the organic matter that 5 min remove remained on surface, and being then cleaned by ultrasonic 5 min with dilute hydrochloric acid removes oxide on surface, finally
Solion and the rapid draing of remained on surface are removed using absolute ethyl alcohol.
（3）Copper foil substrate is transferred to magnetron sputtering apparatus substrate sample platform centre, is fixed with double copper foil tapes of leading,
Magnetron sputtering reaction chamber is closed, vacuum pumping is carried out.
（4）It is 1.0 × 10 to be extracted into back end vacuum-4Pa is passed through argon gas with default 20sccm flows, and fine tuning argon flow amount is extremely
Air pressure is 1.0 Pa or so in sputtering system cavity, and sample stage rotating speed is transferred to 15 r/min, and sample stage temperature is before starting sputtering
Rise to 350 DEG C.
（5）The sputtering power setting of copper target is remained unchanged in 50 W and during cosputtering；The initial sputter work(of molybdenum target
Rate is arranged in 50 W.
（6）Copper target starts after sputtering 2 h, opens molybdenum target, starts the cosputtering of copper target and molybdenum target.After 2 h of cosputtering, adjusts and increase
Molybdenum target sputtering power continues cosputtering to 75 W；Again after 2 h of cosputtering, adjusts and increase molybdenum target sputtering power to 100 W, continue to splash altogether
It penetrates；Again after 2 h of cosputtering, adjusts and increase molybdenum target sputtering power to 125 W, continue cosputtering；Again after 2 h of cosputtering, increasing molybdenum target is adjusted to splash
Power is penetrated to 150 W, continues cosputtering；After 2 h of cosputtering, shielding power supply is closed.
（7）After cosputtering deposits, keeps air pressure in sputtering system cavity, sample stage rotating speed to be transferred to 0, close sample stage
Heating power supply when being cooled to 50 DEG C or less, opens cavity, removes prepared sample, you can obtains the Cu-Mo gradients
Thin-film material.
Embodiment 4：The preparation method of this Cu-Mo gradient film materials uses following concrete technologies.
（1）Surface polishing bright copper target and molybdenum target are placed in two d.c. sputtering targets of high vacuum magnetic control sputtering system
On position；Planar central where adjusting copper target is 8 cm apart from deposited samples platform centre distance, and planar central distance is heavy where molybdenum target
Product sample stage centre distance is 4 cm, is remained unchanged during cosputtering.
（2）The business copper foil bought is cut into the cm of 8 cm × 8 sizes as substrate, copper foil substrate uses acetone ultrasound
The organic matter that 5 min remove remained on surface is cleaned, being then cleaned by ultrasonic 5 min with dilute hydrochloric acid removes oxide on surface, finally makes
Solion and the rapid draing of remained on surface are removed with absolute ethyl alcohol.
（3）Copper foil substrate is transferred to magnetron sputtering apparatus substrate sample platform centre, is fixed with double copper foil tapes of leading,
Magnetron sputtering reaction chamber is closed, vacuum pumping is carried out.
（4）It is 1.0 × 10 to be extracted into back end vacuum-4Pa is passed through argon gas with default 20sccm flows, and fine tuning argon flow amount is extremely
Air pressure is 1.0 Pa or so in sputtering system cavity, and sample stage rotating speed is transferred to 15 r/min, and sample stage temperature is before starting sputtering
Rise to 350 DEG C.
（5）The sputtering power setting of copper target is remained unchanged in 40 W and during cosputtering；The initial sputter work(of molybdenum target
Rate is arranged in 50 W.
（6）Copper target starts after sputtering 1 h, opens molybdenum target, starts the cosputtering of copper target and molybdenum target.After 1 h of cosputtering, adjusts and increase
Molybdenum target sputtering power continues cosputtering to 75 W；Again after 1 h of cosputtering, adjusts and increase molybdenum target sputtering power to 100 W, continue to splash altogether
It penetrates；Again after 1 h of cosputtering, adjusts and increase molybdenum target sputtering power to 125 W, continue cosputtering；Again after 1 h of cosputtering, increasing molybdenum target is adjusted to splash
Power is penetrated to 150 W, continues cosputtering；It adjusts and increases molybdenum target sputtering power to 175 W, continue cosputtering；After 1 h of cosputtering, close
Shielding power supply.
（7）After cosputtering deposits, keeps air pressure in sputtering system cavity, sample stage rotating speed to be transferred to 0, close sample stage
Heating power supply when being cooled to 50 DEG C or less, opens cavity, removes prepared sample, you can obtains the Cu-Mo gradients
Thin-film material.
Embodiment 5：The preparation method of this Cu-Mo gradient film materials uses following concrete technologies.
（1）Surface polishing bright copper target and molybdenum target are placed in two d.c. sputtering targets of high vacuum magnetic control sputtering system
On position；Planar central where adjusting copper target is 8 cm apart from deposited samples platform centre distance, and planar central distance is heavy where molybdenum target
Product sample stage centre distance is 5 cm, is remained unchanged during cosputtering.
（2）The business copper foil bought is cut into the cm of 10 cm × 10 sizes as substrate, copper foil substrate is super using acetone
Sound cleans the organic matter that 5 min remove remained on surface, and being then cleaned by ultrasonic 5 min with dilute hydrochloric acid removes oxide on surface, finally
Solion and the rapid draing of remained on surface are removed using absolute ethyl alcohol.
（3）Copper foil substrate is transferred to magnetron sputtering apparatus substrate sample platform centre, is fixed with double copper foil tapes of leading,
Magnetron sputtering reaction chamber is closed, vacuum pumping is carried out.
（4）It is 1.0 × 10 to be extracted into back end vacuum-4Pa is passed through argon gas with default 20sccm flows, and fine tuning argon flow amount is extremely
Air pressure is 1.0 Pa or so in sputtering system cavity, and sample stage rotating speed is transferred to 15 r/min, and sample stage temperature is before starting sputtering
Rise to 350 DEG C.
（5）The sputtering power setting of copper target is remained unchanged in 50 W and during cosputtering；The initial sputter work(of molybdenum target
Rate is arranged in 50 W.
（6）Copper target starts after sputtering 10 min, opens molybdenum target, starts the cosputtering of copper target and molybdenum target.10 min of cosputtering
Afterwards, it adjusts and increases molybdenum target sputtering power to 100 W, continue cosputtering；Again after 10 min of cosputtering, adjusts and increase molybdenum target sputtering power to 150
W continues cosputtering；After 10 min of cosputtering, shielding power supply is closed.
（7）After cosputtering deposits, keeps air pressure in sputtering system cavity, sample stage rotating speed to be transferred to 0, close sample stage
Heating power supply when being cooled to 50 DEG C or less, opens cavity, removes prepared sample, you can obtains the Cu-Mo gradients
Thin-film material.
Claims (4)
1. a kind of Cu-Mo gradient films material and preparation method thereof, including：
A kind of Cu-Mo bianry alloy thin-film materials that Cu and Mo constituent contents change in gradient, the material is using the double targets of high vacuum
Magnetically controlled sputter method is prepared.
2. Cu-Mo bianry alloys thin-film material according to claim 1, it is characterised in that：
Atomic percentage content of the Cu elements in alloy firm can change between 50% ~ 100%, and surplus is Mo elements.
3. Cu-Mo bianry alloys thin-film material according to claim 1, it is characterised in that：
The thickness of film can change between 1 μm ~ 50 μm, the area of film can the cm ~ 10 of 5 cm × 5 cm ×
Change between 10 cm.
4. the double target magnetic control sputtering methods of high vacuum according to claim 1 prepare the side of Cu-Mo bianry alloy thin-film materials
Method, it is characterised in that：
The double targets of magnetron sputtering are co-deposited Cu-Mo films on copper-based bottom or soda-lime glass substrate, and double targets used are copper target and molybdenum target,
While magnetron sputtering under the conditions of 350 DEG C in-situ annealing；
The condition of the magnetron sputtering is：Planar central where copper target is 8 ~ 10 cm, molybdenum target apart from deposited samples platform centre distance
Place planar central is 4 ~ 6 cm apart from deposited samples platform centre distance, is remained unchanged during cosputtering；
The condition of the magnetron sputtering is：The sputtering power setting of copper target is kept between 25 ~ 50 W and during cosputtering
It is constant；
The condition of the magnetron sputtering is：The initial sputter power setting of molybdenum target is closed between 25 ~ 75 W according to Cu-Mo binary
The graded of Mo contents requires that the sputtering power for increasing molybdenum target, sputtering power can be adjusted to adjust model during cosputtering in gold thin film
It encloses for 25 ~ 175 W.
Priority Applications (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113573458A (en) * | 2021-06-11 | 2021-10-29 | 中科超睿(青岛)技术有限公司 | Nano-gradient neutron target and preparation method thereof |
| CN117904581A (en) * | 2024-03-15 | 2024-04-19 | 中南大学 | High-strength and high-toughness nano multilayer metal composite material and gradient interface design method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113573458A (en) * | 2021-06-11 | 2021-10-29 | 中科超睿(青岛)技术有限公司 | Nano-gradient neutron target and preparation method thereof |
| CN117904581A (en) * | 2024-03-15 | 2024-04-19 | 中南大学 | High-strength and high-toughness nano multilayer metal composite material and gradient interface design method thereof |
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