CN108251800A - A kind of Cu-Al gradient films material and preparation method thereof - Google Patents
A kind of Cu-Al gradient films material and preparation method thereof Download PDFInfo
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- CN108251800A CN108251800A CN201810335010.9A CN201810335010A CN108251800A CN 108251800 A CN108251800 A CN 108251800A CN 201810335010 A CN201810335010 A CN 201810335010A CN 108251800 A CN108251800 A CN 108251800A
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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 Al 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 aluminium target as sputter material, high-vacuum multi-target magnetic control sputtering equipment is prepares tool, copper target target position sputtering power is fixed during by being deposited in cosputtering, the sputtering power of change aluminium target target position realizes the adjusting of copper, aluminium relative amount in membrane material, the thickness for preparing film is controlled by changing the cosputtering time, is finally prepared for the Cu Al 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-Al gradient film materials
Method.
Background technology
Functionally gradient material (FGM) is a kind of novel composite material, it is the material for selecting two kinds of (or a variety of) performances different, is passed through
Continuously changing the Nomenclature Composition and Structure of Complexes of both (or a variety of) materials makes its interface disappear, and leads to the performance of material with the group of material
Into the variation with structure and it is slowly varying.Due to functionally gradient material (FGM) component on certain direction in space consecutive variations, be not present
Sharp interface, so performance is similar between adjacent layer, the performance of material entirety is in consecutive variations.Functionally gradient material (FGM) may be used as interface
Layer connects two kinds of incompatible materials, greatly improves adhesion strength, is also used as boundary layer and reduces residual stress and heat
Stress, while eliminate the Stress singularity of connecting material median surface crosspoint and the free endpoint of stress；It is replaced with functionally gradient material (FGM)
Traditional homogeneous material can enhance bonding strength or reduce cracks deflection and bridge.
At present, Cu based gradient materials are mainly made with Cu and another metal material, such as Cu-Mo, Cu-W graded series
Material etc..The method for preparing Cu based gradient materials is more, as discharge plasma sintering, hot pressed sintering, electro-deposition, vapor deposition and
Self-propagating high-temperature synthesis etc..Copper and another material laminate are synthesized to obtain functionally gradient material (FGM) by distinct methods so that material
Not only had a high mechanical strength and good toughness, but also with good tribological property and electric conductivity, as electric locomotive from
The sliding material that contact net lines import electric energy has good application background.Meanwhile as functionally gradient material (FGM), between both materials
Faying face in gradual transition, the composition transfer between face and face is smaller, effectively reduces the thermal stress between both sides, reduces
Material due to the probability that thermal stress mismatches and crackle is caused to generate, extends the materials'use service life in use.
With the fast development of global economy, in the industry such as oil, chemical industry, the energy, electric power, metallurgy, aerospace, deposit
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 that rate of film build is high, 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 in itself
The distance at matter, the sputtering power of place target position and place target position target plane center and deposited samples platform center.In this way, pass through
The sputtering power and the distance at target plane center and deposited samples platform center for changing target position achieve that constituent element in membrane material
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-Al alloys gradient film material；The present invention also provides
A kind of side of low cost, simple for process that Cu-Al gradient film materials are prepared 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-Al films, while magnetron sputtering
In-situ annealing under the conditions of 300 DEG C；Under the premise of the distance at target plane center and deposited samples platform center is fixed, by changing
The sputtering power for becoming two target position adjusts the relative amount of copper and aluminium in Cu-Al films；What is contacted with substrate is internal layer pure copper layer,
Gradient layer from inside to outside for copper content gradually decreases and aluminium content gradually rises.
Double targets are copper target and aluminium target, and the copper content of copper target is more than the aluminum content of 99.99%, aluminium 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 of the cm of 5 cm × 5 ~ 10
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 aluminium 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 aluminium target is between 25 ~ 75 W, according to Al in Cu-Al bianry alloy films
The graded of content requires that the sputtering power for increasing aluminium target can be adjusted during cosputtering, and sputtering power adjustable range is 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
Pa, the work ar pressure of cosputtering is 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 sputtering at least 10 min, then start being total to for copper target and aluminium target
Sputtering.Copper target, which first sputters certain time one side, can form ultra-thin articulamentum, strengthen the attachment force of co-sputtered thin films and substrate；
On the other hand the pure copper layer of Cu-Al gradient film materials can be formed.
Preferably, annealing process of the invention is：300 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）The bright copper target of surface polishing and aluminium 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 aluminium 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 to the organic matter of 5 min removing remained on surface using acetone,
Then 5 min are cleaned by ultrasonic to copper foil substrate dilute hydrochloric acid and remove oxide on surface, it is residual finally to remove surface using absolute ethyl alcohol
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 sputtering is started
Rise to 300 DEG C.
（5）The sputtering power of copper target is arranged between 25 ~ 50 W and is remained unchanged during cosputtering；Aluminium target it is initial
Sputtering power is arranged between 25 ~ 75 W.
（6）Copper target starts after sputtering at least 10 min, opens aluminium target, starts the cosputtering of copper target and aluminium target.According to waiting to make
Standby Cu-Al bianry alloys film thickness and wherein Cu, the graded requirement of Al content, are spaced certain during cosputtering
Time tune increases the sputtering power of aluminium target, and sputtering power adjustable range is 25 ~ 175 W.
（7）After cosputtering deposits, air pressure in sputtering system cavity is kept, sample stage rotating speed is transferred to 0, closes sample stage
Heating power supply when being cooled to less than 50 DEG C, opens cavity, removes prepared sample.
The beneficial effects of the present invention are：
（1）The present invention provides a kind of thickness deposited in bulk substrate using the double target magnetic control sputtering technologies of high vacuum controllable copper
Aluminum alloy gradient thin-film material, albronze 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 aluminium
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 albronze film carry out in-situ annealing, improve metallic matrix and Coating Materials cohesive force, and
Reduce the generation of micro-crack.
（3）Albronze gradient film material is prepared using magnetically controlled sputter method, easy to operate, highly practical, at low cost,
Controllability is stronger, has the application prospect of large-scale commercialized production.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention is done and is further described, but of the invention
Protection domain be not limited to these embodiments.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-Al gradient film materials uses following concrete technologies.
（1）The bright copper target of surface polishing and aluminium 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 aluminium 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 sizes of 5 cm × 5 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, carries 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 sputtering is started
Rise to 300 DEG C.
（5）The sputtering power of copper target is arranged on 25 W and is remained unchanged during cosputtering；The initial sputter work(of aluminium target
Rate is arranged on 25 W.
（6）Copper target starts after sputtering 1 h, opens aluminium target, starts the cosputtering of copper target and aluminium target.After 1 h of cosputtering, adjust and increase
Aluminium target sputtering power continues cosputtering to 50 W；Again after 1 h of cosputtering, adjust and increase aluminium target sputtering power to 100 W, continue to splash altogether
It penetrates；Again after 1 h of cosputtering, adjust and increase aluminium target sputtering power to 150 W, continue cosputtering；After 1 h of cosputtering, shielding power supply is closed.
（7）After cosputtering deposits, air pressure in sputtering system cavity is kept, sample stage rotating speed is transferred to 0, closes sample stage
Heating power supply when being cooled to less than 50 DEG C, opens cavity, removes prepared sample, you can obtains the Cu-Al gradients
Thin-film material.
Embodiment 2：The preparation method of this Cu-Al gradient film materials uses following concrete technologies.
（1）The bright copper target of surface polishing and aluminium 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 aluminium target
Product sample stage centre distance is 6 cm, is remained unchanged during cosputtering.
（2）Soda-lime glass substrate is cleaned by ultrasonic to the organic matter of 5 min removing remained on surface using acetone, then using 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, carries 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 sputtering is started
Rise to 300 DEG C.
（5）The sputtering power of copper target is arranged on 50 W and is remained unchanged during cosputtering；The initial sputter work(of aluminium target
Rate is arranged on 75 W.
（6）Copper target starts after sputtering 1 h, opens aluminium target, starts the cosputtering of copper target and aluminium target.After 1 h of cosputtering, adjust and increase
Aluminium target sputtering power continues cosputtering to 125 W；Again after 1 h of cosputtering, adjust and increase aluminium 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, air pressure in sputtering system cavity is kept, sample stage rotating speed is transferred to 0, closes sample stage
Heating power supply when being cooled to less than 50 DEG C, opens cavity, removes prepared sample, you can obtains the Cu-Al gradients
Thin-film material.
Embodiment 3：The preparation method of this Cu-Al gradient film materials uses following concrete technologies.
（1）The bright copper target of surface polishing and aluminium 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 aluminium 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 sizes of 10 cm × 10 as substrate, copper foil substrate is surpassed 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, carries 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 sputtering is started
Rise to 300 DEG C.
（5）The sputtering power of copper target is arranged on 50 W and is remained unchanged during cosputtering；The initial sputter work(of aluminium target
Rate is arranged on 50 W.
（6）Copper target starts after sputtering 2 h, opens aluminium target, starts the cosputtering of copper target and aluminium target.After 2 h of cosputtering, adjust and increase
Aluminium target sputtering power continues cosputtering to 75 W；Again after 2 h of cosputtering, adjust and increase aluminium target sputtering power to 100 W, continue to splash altogether
It penetrates；Again after 2 h of cosputtering, adjust and increase aluminium target sputtering power to 125 W, continue cosputtering；Again after 2 h of cosputtering, increasing aluminium 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, air pressure in sputtering system cavity is kept, sample stage rotating speed is transferred to 0, closes sample stage
Heating power supply when being cooled to less than 50 DEG C, opens cavity, removes prepared sample, you can obtains the Cu-Al gradients
Thin-film material.
Embodiment 4：The preparation method of this Cu-Al gradient film materials uses following concrete technologies.
（1）The bright copper target of surface polishing and aluminium 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 aluminium 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 sizes of 8 cm × 8 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, carries out vacuum pumping.
（4）It is 8.0 × 10 to be extracted into back end vacuum-5Pa 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 sputtering is started
Rise to 300 DEG C.
（5）The sputtering power of copper target is arranged on 40 W and is remained unchanged during cosputtering；The initial sputter work(of aluminium target
Rate is arranged on 50 W.
（6）Copper target starts after sputtering 1 h, opens aluminium target, starts the cosputtering of copper target and aluminium target.After 1 h of cosputtering, adjust and increase
Aluminium target sputtering power continues cosputtering to 75 W；Again after 1 h of cosputtering, adjust and increase aluminium target sputtering power to 100 W, continue to splash altogether
It penetrates；Again after 1 h of cosputtering, adjust and increase aluminium target sputtering power to 125 W, continue cosputtering；Again after 1 h of cosputtering, increasing aluminium target is adjusted to splash
Power is penetrated to 150 W, continues cosputtering；It adjusts and increases aluminium target sputtering power to 175 W, continue cosputtering；After 1 h of cosputtering, close
Shielding power supply.
（7）After cosputtering deposits, air pressure in sputtering system cavity is kept, sample stage rotating speed is transferred to 0, closes sample stage
Heating power supply when being cooled to less than 50 DEG C, opens cavity, removes prepared sample, you can obtains the Cu-Al gradients
Thin-film material.
Embodiment 5：The preparation method of this Cu-Al gradient film materials uses following concrete technologies.
（1）The bright copper target of surface polishing and aluminium 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 aluminium 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 sizes of 10 cm × 10 as substrate, copper foil substrate is surpassed 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, carries 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 sputtering is started
Rise to 300 DEG C.
（5）The sputtering power of copper target is arranged on 50 W and is remained unchanged during cosputtering；The initial sputter work(of aluminium target
Rate is arranged on 50 W.
（6）Copper target starts after sputtering 10 min, opens aluminium target, starts the cosputtering of copper target and aluminium target.10 min of cosputtering
Afterwards, it adjusts and increases aluminium target sputtering power to 100 W, continue cosputtering；Again after 10 min of cosputtering, adjust and increase aluminium target sputtering power to 150
W continues cosputtering；After 10 min of cosputtering, shielding power supply is closed.
（7）After cosputtering deposits, air pressure in sputtering system cavity is kept, sample stage rotating speed is transferred to 0, closes sample stage
Heating power supply when being cooled to less than 50 DEG C, opens cavity, removes prepared sample, you can obtains the Cu-Al gradients
Thin-film material.
Claims (5)
1. a kind of Cu-Al gradient films material and preparation method thereof, including：
The Cu-Al bianry alloy thin-film materials that a kind of Cu and Al constituent contents change in gradient, the material is using the double targets of high vacuum
Magnetically controlled sputter method is prepared.
2. Cu-Al 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 Al elements.
3. Cu-Al 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 of the cm of 5 cm × 5 ~ 10 ×
Change between 10 cm.
4. the double target magnetic control sputtering methods of high vacuum according to claim 1 prepare the side of Cu-Al bianry alloy thin-film materials
Method, it is characterised in that：
The double targets of magnetron sputtering are co-deposited Cu-Al films on copper-based bottom or soda-lime glass substrate, and double targets used are copper target and aluminium target,
While magnetron sputtering under the conditions of 300 DEG C in-situ annealing；
The condition of the magnetron sputtering is：Planar central where copper target is 8 ~ 10 cm apart from deposited samples platform centre distance, aluminium target
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 of copper target is arranged between 25 ~ 50 W and is kept during cosputtering
It is constant；
The condition of the magnetron sputtering is：The initial sputter power setting of aluminium target is closed between 25 ~ 75 W according to Cu-Al binary
The graded of Al content requires that the sputtering power for increasing aluminium target can be adjusted during cosputtering in gold thin film, and sputtering power adjusts model
It encloses for 25 ~ 175 W.
5. according to the method described in claim 4, it is characterized in that：
Copper-based bottom used must be cleaned by ultrasonic the organic matter that at least 5 min remove remained on surface through acetone, and dilute hydrochloric acid is cleaned by ultrasonic
At least 5 min remove oxide on surface, and absolute ethyl alcohol removes the solion of remained on surface, and magnetic is then transferred to after rapid draing
It controls on sputtering equipment matrix sample platform；
Soda-lime glass substrate used must be cleaned by ultrasonic the organic matter that 5 min remove remained on surface through acetone, and absolute ethyl alcohol removes
The solion of remained on surface, and be then transferred to after rapid draing on magnetron sputtering apparatus matrix sample platform；
The aluminum content that the copper content of the copper target is more than 99.99%, aluminium target is more than 99.99%；
The back end vacuum degree that sputter chamber is reached is not less than 1.0 × 10-4Pa, the work ar pressure of cosputtering is 1 .0 Pa
Left and right, the rotary speed of substrate is 15 r/ min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110911524A (en) * | 2019-11-05 | 2020-03-24 | 中国电子科技集团公司第十一研究所 | Preparation method and preparation device of chip electrode |
| CN112151400A (en) * | 2020-09-23 | 2020-12-29 | 锦州七七七微电子有限责任公司 | Method for solving SMD tube shell bonding point gold-aluminum system |
| CN112941481A (en) * | 2021-02-08 | 2021-06-11 | 浙江东尼电子股份有限公司 | Method for sputtering aluminum layer on copper substrate and aluminum atom transfer copper plastic film |
| CN114759419A (en) * | 2022-03-17 | 2022-07-15 | 江苏海洋大学 | Preparation method of copper-aluminum gradient alloy transition joint for submarine cable welding |
-
2018
- 2018-04-15 CN CN201810335010.9A patent/CN108251800A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110911524A (en) * | 2019-11-05 | 2020-03-24 | 中国电子科技集团公司第十一研究所 | Preparation method and preparation device of chip electrode |
| CN112151400A (en) * | 2020-09-23 | 2020-12-29 | 锦州七七七微电子有限责任公司 | Method for solving SMD tube shell bonding point gold-aluminum system |
| CN112941481A (en) * | 2021-02-08 | 2021-06-11 | 浙江东尼电子股份有限公司 | Method for sputtering aluminum layer on copper substrate and aluminum atom transfer copper plastic film |
| CN114759419A (en) * | 2022-03-17 | 2022-07-15 | 江苏海洋大学 | Preparation method of copper-aluminum gradient alloy transition joint for submarine cable welding |
| CN114759419B (en) * | 2022-03-17 | 2024-01-09 | 江苏海洋大学 | Preparation method of copper-aluminum gradient alloy transition joint for submarine cable welding |
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