CN108914072A - A kind of amorphous Cu-Ta nano-multilayer film and its preparation method and application - Google Patents
A kind of amorphous Cu-Ta nano-multilayer film and its preparation method and application Download PDFInfo
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- CN108914072A CN108914072A CN201810608107.2A CN201810608107A CN108914072A CN 108914072 A CN108914072 A CN 108914072A CN 201810608107 A CN201810608107 A CN 201810608107A CN 108914072 A CN108914072 A CN 108914072A
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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
- C23C14/06—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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/028—Including graded layers in composition or in physical properties, e.g. density, porosity, grain size
Abstract
The present invention relates to a kind of amorphous Cu-Ta nano-multilayer films and its preparation method and application.By the amorphous layer of two kinds of different structures, alternately superposition is formed the nano-multilayer film；Contain Cu and Ta in any one amorphous layer simultaneously.In the nano-multilayer film, the amorphous composition of layer continuous transition for two kinds of different structures being in contact.Preparation method is：First using pure Cu, pure Ta as target；Select substrate；Target is fixed in target head, the height and angle for adjusting two targets make two pinwheels focus on the center of sample stage；Substrate is placed on the setting position of sample stage；Then it vacuumizes, is passed through protective gas；Co-electrodeposition method deposition film on substrate is focused by magnetron sputtering；When deposition film, sample stage is rotated；Obtain the Cu-Ta amorphous nano multilayer film of setting structure.Of the invention designed and preparation product, application field include being used at least one of the anti-friction wear protection of material surface, solid lubrication, Electronic Packaging diffusion barrier layer, thermoelectricity interface.
Description
Technical field
The present invention relates to a kind of amorphous Cu-Ta nano-multilayer films and its preparation method and application；Belong to made of new structural material to set
Count preparation technical field.
Background technique
Metal nano multilayer film is to alternate the artificial material constituted by two or more metals.Because thickness in monolayer is being received
Rice magnitude, often with having special interfacial structure and stress state, mechanics, electricity, optics and in terms of function admirable,
Microelectronics and micromechanics field are used widely, such as Electronic Packaging, magnetic recording, high-strength and hard, wear-resistant film layer (Q Zhou,
et al.The mechanical behavior of nanoscale metallic multilayers:A survey.Acta
Mech Sin,2015,31(3):319-337).The electrical and thermal conductivity of copper is strong, plasticity is good, and Ta hardness and fusing point are high, anti-corrosion
Property it is good therefore similar to the film that many copper and transition element are constituted, Cu-Ta composite membrane and multilayer film are also because of its property
And it is controllable and deep concerned.For example, Cu-Ta multilayer film, which is reported in resistivity and mechanical property etc., all has size effect
Answer (MZ.Weiet al.Anomalous plastic deformation in nanoscale Cu/Ta
multilayers.Materials Science&Engineering A,2014,598(6):355-359.)。
Cu-Ta alloy is a kind of typical immiscible alloy since its enthalpy of mixing is positive.The conjunction prepared using sputtering method
Its golden structure and composition is related, and generally, for composite single layer film, the rich part Cu is face-centred cubic structure solid solution (α-Cu
(Ta)), the rich part Ta is body-centered cubic or β-phase solid solution (α-or β-Ta (Cu)), and remaining inter-level is non crystalline structure.And
Cu-Ta multilayer film is mostly Cu and Ta the alternating stacking of single layer, and structure is in alternating ordering growth, straight clear, without apparent ingredient
Mixed zone exists.
Currently, preparing metal nano multilayer film using magnetron sputtering method is mostly alternating deposit method, that is, pass through switch sample
Platform position successively under different sputtering target materials deposit nanoscale film layer or alternation switch difference sputtering target material power supply and
Baffle under its target cover reaches the deposition periodically variable purpose of ingredient (CM.M ü ller, et al.Nanoscale Cu/Ta
multilayer deposition by co-sputtering on a rotating substrate.Empirical
model and experiment.Surface&Coatings Technology,2016,302:284-292.).Such method
Implement relatively complicated, and the multilayer membrane interface prepared is obvious, and ingredient fluctuation is big.Especially when the crystal structure of multilayer membrane component not
Defect more non-coherence heterogeneous interface is easily formed when same or lattice equations are big.Such interface be influence multilayer membrane stability with
And an important factor for plasticity and toughness.
In addition, studying more metallized multilayer film at present is mostly formed by single layer pure metal stacking, can divide from crystal structure
For monocrystalline/monocrystalline, polycrystalline/polycrystalline, amorphous/polycrystalline, amorphous/amorphous nano-multilayer film.Wherein amorphous multilayer film is since its is excellent
Magnetics, mechanics and photoelectric properties, be applied in multiple fields.But monofilm is amorphous alloy and ingredient is continuous
The multilayer film of variation not yet appears in the newspapers.Based on this, it is a kind of be made of different Cu-Ta non crystalline structure stackings as single layer, two-phase
The made of new structural material for the amorphous nano multilayer film that interface is smooth, ingredient continuously fluctuates is suggested in this context.
The present invention focuses codeposition technique using double target magnetic control sputterings and prepares amorphous layer alternating Cu-Ta nano-multilayer film, with
The method self-assembled nanometer multilayer film of successive sedimentation mixed film is not necessarily to frequent switching sample stage, only need to control two targets with respect to function
Rate, change sample stage autorotation speed and sample can be prepared by different modulating period, different modulating ratio from sample stage centre distance
And the smooth amorphous nano multilayer film of interfaces transition that heterogeneity rises and falls, this method simple process and low cost are high-efficient.
The amorphous layer alternating Cu-Ta nanometer multilayer film-strength and toughness, heat transfer, conduction etc. of preparation are had excellent performance, in flexible function
Energy device long-life usage etc. has great application prospect.
Summary of the invention
The multilayer film of more Cu-Ta nano-multilayer film and other immisicble metal systems is studied at present using alternating deposit
Method preparation only simply stacks up two kinds of pure metal thin layers that thickness direction is nanoscale are mechanical.This method
The metal nano multilayer membrane interface prepared is clearly demarcated, and interface structure on two sides is usually asymmetric and non-coherence, and component difference
Obviously, metallized multilayer film plasticity and toughness and structural stability are affected.The present invention according to the relationship of Cu-Ta membrane structure and ingredient,
The periodically alternate Cu-Ta nano-multilayer film of two kinds of non crystalline structures, the multilayer have been prepared using traditional focusing co-electrodeposition method
Membrane interface is smooth, two lateral element consecutive variations near interface.Such multilayer film has good intensity and moulding simultaneously.It is such new
The development of structural material provides a kind of new thinking for the research of metallized multilayer film.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, the Cu-Ta amorphous nano multilayer film is by two kinds of different structures
Alternately superposition is formed amorphous layer；Contain Cu and Ta in any one amorphous layer simultaneously.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, the ingredient of the amorphous layer for two kinds of different structures being in contact are different
It causes.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, in the Cu-Ta amorphous nano multilayer film, Cu and Ta are in continuous
The mode of fluctuation is distributed, and Cu+Ta=100%.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, in any one amorphous layer, Cu and the Ta preservation in the form of alloy.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, the amorphous layer of two kinds of different structures are in contact constituted interface
For straight interface；And the ingredient at interface is consecutive variations relative to the ingredient of the amorphous layer for two kinds of different structures being in contact.
In the present invention, the boundary layer is consecutive variations relative to the ingredient of the amorphous layer for two kinds of different structures being in contact；It can
To be understood as assuming that the amorphous layer for two kinds of different structures being in contact is respectively A layers；B layers；Wherein A layers of Ta content is greater than B layers
Ta content；Assuming that A layers and interface contact portions Ta of content is a；So interface and A layer contact site, the content of Ta for a ×
0.9-1.1, preferably a × 0.95-1.05；Along the content of interfacial layer thickness direction Ta, continuously or by a small margin gradient is successively decreased simultaneously,
And the content of Ta is greater than the content of B layers with interface contact portions Ta in interface.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, multilayer film modulation period is within the scope of 1~200nm.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, the modulation ratio range of two kinds of amorphous is 4 in multilayer film:1~1:
12。
A kind of Cu-Ta amorphous nano multilayer film of the present invention, the content of Ta is 15-90at.% in any one layer of amorphous layer.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, nano-indentation hardness are greater than 10GPa.The amorphous multilayer film is same
When with high intensity and plasticity, nano-indentation hardness is greater than 10GPa, vickers indentation flawless.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, amorphous multilayer film layer structure after 600 DEG C of annealing keep steady
It is fixed.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, amorphous multilayer film is after 600 DEG C of annealing, and nano-indentation hardness is still
Greater than 8GPa.
A kind of Cu-Ta amorphous nano multilayer film of the present invention, the overall thickness of the Cu-Ta amorphous nano multilayer film are 30nm-
3000nm.Any one amorphous layer with a thickness of 0.5-100nm.
A kind of preparation method of Cu-Ta amorphous nano multilayer film of the present invention；Include the following steps：
Step 1
Using pure Cu, pure Ta as target；Selected substrate；Target is fixed in target head, the height and angle of two targets are adjusted
Two pinwheels are made to focus on the center of sample stage；Substrate is placed on the setting position of sample stage；
Step 2
It vacuumizes, then passes to protective gas；Co-electrodeposition method deposition film on substrate is focused by magnetron sputtering；Deposition
When film, sample stage is rotated；Obtain the Cu-Ta amorphous nano multilayer film of setting structure.
A kind of preparation method of Cu-Ta amorphous nano multilayer film of the present invention；Co-electrodeposition method is focused by magnetron sputtering serving as a contrast
On bottom when deposition film, substrate temperature is 10-200 DEG C, preferably 20 DEG C.In specific operation process；Sample stage can lead to
Enter cooling medium (including water), reduces underlayer temperature, it is made to maintain 20 DEG C or so.
Industrially in application, substrate can be selected according to demand, such as with the monocrystalline silicon of single-sided polishing, most of metal
Substrate, alloy substrate, ceramic substrate, macromolecule polymer material substrate, carbon/ceramic composite material substrate, C/C composite substrate
And other composite substrates etc..
A kind of preparation method of Cu-Ta amorphous nano multilayer film of the present invention；In step 2；By adjusting Cu target and Ta target
Power primarily determines the ingredient section of cosputtering multilayer film to obtain different modulating than the Cu-Ta film with heterogeneity；It is described
The power adjustment of Cu target is 0-200W；The power adjustment of the Ta target is 0-300W.
A kind of preparation method of Cu-Ta amorphous nano multilayer film of the present invention；In step 2；By change two target power output ratios,
At least one of sample stage revolving speed, to regulate and control multilayer film modulation period.Preferably, the sample stage revolving speed is less than or equal to 30
Rev/min.
A kind of preparation method of Cu-Ta amorphous nano multilayer film of the present invention；In step 2；By changing substrate from sample stage
The distance r at center, preparation average assay is identical, modulation period and the different Cu-Ta nano-multilayer film of modulation ratio；The r is greater than
Equal to 0 less than or equal to the radius of sample stage, preferably 0-35mm.
A kind of preparation method of Cu-Ta amorphous nano multilayer film of the present invention；Specific step is as follows for it：
By monocrystalline silicon (100) substrate of single-sided polishing, it is sequentially placed into acetone and alcoholic solution and is cleaned by ultrasonic 15 minutes, drum
It is put on the sample stage in vacuum chamber after the drying of wind drying box.During the deposition process, sample stage can be passed through cooling water, reduce silicon
Substrate temperature makes it maintain 20 DEG C or so.
The pure Cu (99.99%) of Φ 50mm × 4mm and pure Ta (99.95%) target are fixed in target head, two targets of adjustment
Height and angle make two pinwheels focus on the center of sample stage.
After shutting door for vacuum chamber, successively with mechanical pump and molecular pump to vacuum chamber, when background vacuum is better than 5.0
×10-4After pa, being passed through argon gas to vacuum chamber makes gas pressure in vacuum reach 1.0Pa, then opens the power supply of target Cu and Ta, adjusts phase
Answer the oxide layer for removing target surface after power to Cu and Ta target pre-sputtering 5 minutes.
Then vacuum chamber is restored into base vacuum, is passed through argon gas, vacuum degree is made to reach 1.0 × 10-2After Pa, open low energy from
Component (600V, 50mA) starts formal magnetron sputtering plating after cleaning 15 minutes to monocrystalline silicon.
By adjusting the power of Cu target (0-200W) and Ta (0-300W) target with obtain different modulating than with heterogeneity
Cu-Ta film primarily determines the ingredient section of cosputtering multilayer film；It is (small by changing two target power output ratios or sample stage revolving speed
In equal to 30 rpms) to regulate and control multilayer film modulation period；By changing substrate from sample stage centre distance r (0-35mm),
Prepare that ensemble average ingredient is identical, but modulation period and the different Cu-Ta nano-multilayer film of modulation ratio.
The application of of the invention designed and preparation Cu-Ta amorphous nano multilayer film, including be used for material surface and resist
The fields such as fretting wear protection, solid lubrication, Electronic Packaging diffusion barrier layer, thermoelectricity interface.Meanwhile system designed by the present invention
Preparation Method can be co-deposited other nanometer multilayer film systems containing diffusion barrier element.Principle and advantage
Device therefor of the present invention is common magnetic-controlled sputtering coating equipment, and used technology is that double target magnetic control sputterings focus
Codeposition technique, the schematic diagram that co-deposition prepares Cu-Ta film are as shown in Figure 1.Two sputtering targets of Cu and Ta are symmetrically distributed in sample
The two sides of sample platform, the angle and distance for adjusting two targets make two targets focus on the center of sample stage altogether, and opening shielding power supply can make
The standby film containing two kinds of elements of Cu-Ta.Deposition method shown in Fig. 1 (a) is the method for common preparation hybrid films, the present invention
It was found that there is the multilayer film that can be co-deposited layer structure when diffusion barrier element or compound in system.Cosputtering Cu, Ta target
When material, generated beneath region can have rich Cu and the richness area Ta of component distributing unevenness, when sample has centainly from sample stage central point
When distance r, when sample stage rotation, can make sample successively be in the different region of ingredient, can be heavy first when being in position 1 such as sample
The high thin layer of product Ta content, when sample stage rotation, sample gradually shifts to position 2 and obtains richness Cu film, sample stage rotation one
It is a modulation period after circle, so that multilayer film is formed, as shown in Fig. 1 (b).This method can pass through the function of adjusting Cu and Ta target
The modulation ratio and average assay of rate regulation multilayer film；Sample stage autorotation speed is adjusted to regulate and control multilayer film modulation period.
Major advantage
The alternate Cu-Ta of amorphous layer is successfully prepared present invention employs the focusing co-electrodeposition method for preparing common composite membrane to receive
This made of new structural material of rice multilayer film, advantage essentially consist in：
1) by soft, lubrication, highly conductive copper and hard, that wear-resisting, diffusion barrier tantalum element is combined into alloy is thin
Film is advantageously implemented the functions such as wear-resisting anti-friction, lubrication, diffusion barrier；
2) Cu-Ta film is deposited using magnetron sputtering, is easy to get noncrystal membrane, be conducive to improve film hardness；
3) using magnetron sputtering be co-deposited Cu-Ta film, available nano-multilayer film, multilayer film by two kinds of compositions alloy
Amorphous layer alternately forms, and amorphous layer thickness is in nanometer scale, and interface layer is smooth, ingredient consecutive variations, not pure metal Cu
Be conducive to the plasticity and toughness and thermal stability that improve noncrystal membrane while keeping amorphous high rigidity with the superposition of pure Ta film；
4) continuous interfacial of nano-multilayer film can be improved diffusion barrier performance and reduce heat-conductive characteristic, be conducive to electricity
The application such as son encapsulation and thermoelectricity interface；
5) when magnetron sputtering is co-deposited Cu-Ta multilayer film, Cu target and Ta target are to be focused on same sample platform simultaneously, are not necessarily to
The switching carried out between different sample stages can be prepared by multilayer film.This method is high-efficient, at low cost；
6) the Cu-Ta multilayer film in different modulating period only needs to can be realized by adjusting sample stage autorotation speed；
7) this method can be realized and be prepared averagely on same sample platform by changing sample and sample stage center distance r
Ingredient is identical, modulation period different Cu-Ta nano-multilayer film.
Detailed description of the invention
Fig. 1 is that magnetron sputtering of the present invention focuses the co-electrodeposition method alternate Cu-Ta nanometer multilayer of deposited amorphous layer on substrate
The schematic diagram of film；
Fig. 2 be embodiment 1 in, when revolving speed be 5r/min when, the section High-Resolution Map of products obtained therefrom Cu-Ta nano-multilayer film
Picture；
The HAADF-STEM image and line in the section of 1 products obtained therefrom Cu-Ta nano-multilayer film of the position Fig. 3 embodiment sweep analysis
Figure；
Specific embodiment
Embodiment 1
The monocrystalline silicon (100) of the single-sided polishing cut is individually positioned on the sample stage that autorotation speed is 5 rpms,
On the concentric circles that it is 15mm from sample stage centre distance r that each sample, which is located at, the function of Cu target (80W) and Ta (190W) target is adjusted
Rate, co-deposition average assay are Cu-60at.%Ta film.Transmission electron microscope analysis is carried out to sample in cross section, full resolution pricture is such as
Shown in Fig. 2, the results showed that, when sample revolving speed is 5 rpms, film has apparent multilayer film feature, the modulation week of film
Phase is about 12nm, and modulation ratio is about 1:2, two interface layers are straight and smooth, and interface two sides are respectively different non crystalline structures.Knot
Closing Fig. 3 can be seen that Ta, Cu are fluctuated in continuous in a certain range in its product, and Cu+Ta=100%.
Embodiment 2
Transmission electron microscope analysis is carried out to the sample in cross section in embodiment 1, Fig. 3 is its HAADF-STEM image and corresponding energy
Spectrum analysis.The result shows that the modulation period of Cu-Ta multilayer film and embodiment 1 are coincide, about 12nm, interfaces transition is smooth, layer with
Interlayer ingredient continuously fluctuates.
Embodiment 3
It can be made using technological parameter in the same manner as in Example 1 when sample stage autorotation speed is within the scope of 0-15rpm
Obtain the Cu-Ta multilayer film that range modulation period is about 1~200nm.
Embodiment 4
The monocrystalline silicon (100) of the single-sided polishing cut is individually positioned on the sample stage that autorotation speed is 5r/min, often
On the concentric circles that it is 15mm from sample stage centre distance r that a sample, which is located at, adjust the power of Cu target and Ta target, be co-deposited it is average at
It is divided into 20-70at.%Ta film, may occur in which the Cu-Ta multilayer film that amorphous layer is alternately present, amorphous layer modulation ratio range is 2:1
~1:Between 12.
Embodiment 6
The single crystalline Si (100) of the single-sided polishing cut is individually positioned on the sample stage that autorotation speed is 5r/min, often
On the concentric circles that it is 15mm from sample stage centre distance r that a sample, which is located at, adjust the power of Cu target and Ta target, be co-deposited it is average at
It is divided into 10-20at.%Ta film, may occur in which the Cu-Ta multilayer film that α-Cu (Ta) solid solution layer of different solid solubility is alternately present.
Embodiment 7
The single crystalline Si (100) of the single-sided polishing cut is individually positioned on the sample stage that autorotation speed is 5r/min, often
On the concentric circles that it is 15mm from sample stage centre distance r that a sample, which is located at, adjust the power of Cu target and Ta target, be co-deposited it is average at
It is divided into 70-90at.%Ta film, may occur in which the Cu-Ta multilayer film that β-Ta (Cu) solid solution layer of different solid solubility is alternately present.
Embodiment 8
By (400,500,600 DEG C) the annealing 1h at different temperatures of the Cu-Ta multilayer film in embodiment 1.The result shows that Cu-
Ta multilayer film, there is no apparent mutually separation occurs, is mutually generated without pure Cu with pure Ta simple substance in different temperatures annealing process,
Multi-layer film structure saves preferably, and the thermal stability of film is good.
Embodiment 9
Using the hardness and elasticity modulus of Cu-Ta multilayer film in Nanoindentation measurement embodiment 1.The result shows that Cu-Ta
For Multilayer-film nanometer identation hardness in 10GP or more, nano impress pattern is displayed without crackle appearance, while having excellent tough
Property.
Embodiment 10
By the Cu-Ta multilayer film in embodiment 1 in 600 DEG C of annealing 1h, using the hardness of Nanoindentation measurement multilayer film
And elasticity modulus.The result shows that the mechanical property variation in annealing process of Cu-Ta multilayer film is small, hardness is high still in 8GPa or more
Higher mechanical property is still able to maintain after temperature annealing.
Claims (10)
1. a kind of Cu-Ta amorphous nano multilayer film, it is characterised in that：The Cu-Ta amorphous nano multilayer film is by two kinds of different knots
Alternately superposition is formed the amorphous layer of structure；Contain Cu and Ta in any one amorphous layer simultaneously.
2. a kind of Cu-Ta amorphous nano multilayer film according to claim 1, it is characterised in that：
In the Cu-Ta amorphous nano multilayer film, the ingredient of the amorphous layer for two kinds of different structures being in contact is inconsistent；
In any one amorphous layer of the Cu-Ta amorphous nano multilayer film, Cu and the Ta preservation in the form of alloy, and any one layer
The content of Ta is 15-90at.% in amorphous layer.
3. a kind of Cu-Ta amorphous nano multilayer film according to claim 1, it is characterised in that：Two kinds of different structures it is non-
Crystal layer is in contact constituted interface as straight interface；And amorphous of the ingredient at interface relative to two kinds of different structures being in contact
The ingredient of layer is consecutive variations.
4. a kind of Cu-Ta amorphous nano multilayer film according to claim 1, it is characterised in that：Multilayer film modulation period is 1
Within the scope of~200nm.
5. a kind of Cu-Ta amorphous nano multilayer film according to claim 1, it is characterised in that：Two kinds of amorphous in multilayer film
Modulation ratio range be 4:1~1:12.
6. a kind of Cu-Ta amorphous nano multilayer film according to claim 1, it is characterised in that：
The nano-indentation hardness of the Cu-Ta amorphous nano multilayer film is greater than 10GPa；
Cu-Ta amorphous nano multilayer film layer structure after 600 DEG C of annealing keeps stablizing；
For the Cu-Ta amorphous nano multilayer film after 600 DEG C of annealing, nano-indentation hardness is still greater than 8GPa.
7. a kind of Cu-Ta amorphous nano multilayer film according to claim 1, it is characterised in that：
The overall thickness of the Cu-Ta amorphous nano multilayer film is 30nm-3000nm；Any one amorphous layer with a thickness of 0.5nm-
100nm。
8. a kind of preparation method of the Cu-Ta amorphous nano multilayer film as described in claim 1-7 any one；It is characterized in that；
Include the following steps：
Step 1
Using pure Cu, pure Ta as target；Select substrate；Target is fixed in target head, the height and angle for adjusting two targets make two
Pinwheel focuses on the center of sample stage；Substrate is placed on the setting position of sample stage；
Step 2
It vacuumizes, then passes to protective gas；Co-electrodeposition method deposition film on substrate is focused by magnetron sputtering；Deposition film
When, rotate sample stage；Obtain the Cu-Ta amorphous nano multilayer film of setting structure.
9. a kind of preparation method of Cu-Ta amorphous nano multilayer film according to claim 8；
In step 2；By magnetron sputtering focus co-electrodeposition method on substrate deposition film when, substrate temperature be 10-200 DEG C；
In step 2；By adjusting the power of Cu target and Ta target to obtain different modulating than the Cu-Ta film with heterogeneity, just
Walk the ingredient section for determining cosputtering multilayer film；The power adjustment of the Cu target is 0-200W；The power tune of the Ta target
Whole range is 0-300W.
In step 2；By changing at least one of two target power output ratios, sample stage revolving speed, to regulate and control multilayer film modulation period；
The sample stage revolving speed is less than or equal to 30 revs/min；
In step 2；By changing substrate from sample stage center distance r, preparation average assay is identical, modulation period and modulation
Than different Cu-Ta nano-multilayer films；The r is more than or equal to 0 radius for being less than or equal to sample stage.
10. a kind of application of the Cu-Ta amorphous nano multilayer film as described in claim 1-7 any one, it is characterised in that：Including
It is used for the anti-friction wear protection of material surface, solid lubrication, Electronic Packaging diffusion barrier layer, at least one in thermoelectricity interface
Kind.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110144485A (en) * | 2019-05-29 | 2019-08-20 | 西安交通大学 | A kind of Cu-Ta alloy and preparation method thereof |
| CN111020513A (en) * | 2019-12-30 | 2020-04-17 | 西安理工大学 | Method for improving toughness of nano metal multilayer film |
| CN113151793A (en) * | 2021-03-26 | 2021-07-23 | 西安交通大学 | Preparation method of high-strength high-plasticity copper-aluminum nano metal multilayer film |
| CN113652660A (en) * | 2021-08-18 | 2021-11-16 | 南京工程学院 | Multi-refractory metal doped nano multilayer structure Ni-based film and preparation method and application thereof |
| CN113802100A (en) * | 2021-08-25 | 2021-12-17 | 西安交通大学 | Method for regulating and controlling processing hardening capacity of amorphous/amorphous nano multilayer film |
| CN115287599A (en) * | 2022-08-25 | 2022-11-04 | 长安大学 | High-wear-resistance CoFeTaB/MgCuY amorphous/amorphous multilayer film and preparation method thereof |
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| CN107841716A (en) * | 2017-11-10 | 2018-03-27 | 湖南大学 | A kind of nano-multilayer film and preparation method thereof |
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| CLAUDIA M. MÜLLER 等: "Nanoscale Cu/Ta multilayer deposition by co-sputtering on a rotating substrate. Empirical model and experiment", 《SURFACE & COATINGS TECHNOLOGY》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110144485A (en) * | 2019-05-29 | 2019-08-20 | 西安交通大学 | A kind of Cu-Ta alloy and preparation method thereof |
| CN111020513A (en) * | 2019-12-30 | 2020-04-17 | 西安理工大学 | Method for improving toughness of nano metal multilayer film |
| CN113151793A (en) * | 2021-03-26 | 2021-07-23 | 西安交通大学 | Preparation method of high-strength high-plasticity copper-aluminum nano metal multilayer film |
| CN113652660A (en) * | 2021-08-18 | 2021-11-16 | 南京工程学院 | Multi-refractory metal doped nano multilayer structure Ni-based film and preparation method and application thereof |
| CN113652660B (en) * | 2021-08-18 | 2023-10-13 | 南京工程学院 | Multi-element refractory metal doped nano multilayer structure Ni-based film and preparation method and application thereof |
| CN113802100A (en) * | 2021-08-25 | 2021-12-17 | 西安交通大学 | Method for regulating and controlling processing hardening capacity of amorphous/amorphous nano multilayer film |
| CN115287599A (en) * | 2022-08-25 | 2022-11-04 | 长安大学 | High-wear-resistance CoFeTaB/MgCuY amorphous/amorphous multilayer film and preparation method thereof |
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