CN107452964A - A kind of method for improving cathode of lithium battery copper foil colelctor electrode electrical property - Google Patents
A kind of method for improving cathode of lithium battery copper foil colelctor electrode electrical property Download PDFInfo
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- CN107452964A CN107452964A CN201710666733.2A CN201710666733A CN107452964A CN 107452964 A CN107452964 A CN 107452964A CN 201710666733 A CN201710666733 A CN 201710666733A CN 107452964 A CN107452964 A CN 107452964A
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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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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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0421—Methods of deposition of the material involving vapour deposition
- H01M4/0423—Physical vapour deposition
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
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Abstract
The present invention discloses a kind of method for improving cathode of lithium battery copper foil colelctor electrode electrical property, it is characterized in that one layer of nanometer Copper thin film is deposited on cathode of lithium battery colelctor electrode copper foil using vacuum plasma coating technique, ion gun bombardment processing is carried out to Copper thin film surface again, to improve the adhesive force of lithium cell cathode material and colelctor electrode copper foil, reduce interfacial effect, so as to improve the electrical property of lithium battery.
Description
Technical field
The present invention relates to lithium battery device and lithium battery material manufacturing technology field, and in particular to one kind improves lithium battery and born
The method of pole copper foil colelctor electrode electrical property.
Background technology
Lithium cell cathode material holds electrokinetic cell security lifeblood, in lithium ion battery negative material, except graphitization
Carbonaceous mesophase spherules (MCMB), amorphous carbon, silicon or tin class are occupied outside the fraction market share, and native graphite and Delanium account for
According to more than the 90% negative material market share.Graphitized carbon material, amorphous carbon material, nitride, silica-base material, tinbase
Material, novel alloy and other materials.
Lithium ion battery is mainly made up of positive pole, negative pole, barrier film and electrolyte.The potential that battery the two poles of the earth are added in during charging is compeled
The lithium intercalation compound of positive pole is set to discharge lithium ion, by the graphite cathode of embedded six square piece Rotating fields after barrier film;During electric discharge
Lithium ion then separates out from the graphite of lamellar structure, and the lithium intercalation compound with positive pole combines again, and the movement of lithium ion generates
Electric current.Although the structure and charge and discharge process chemical principle of lithium ion battery are very simple, but the commercialization in reality should
Need to consider many problems in.Such as the electric conductivity of positive and negative pole material, charge and discharge potential, activity, the structure of de- slotting lithium are steady
Qualitative energy, high rate performance and security performance etc., and the stability of electrolyte, electric conductivity and environmental suitability etc..
In addition to above-mentioned factor, the internal resistance of lithium ion battery must be sufficiently small, only in this way just can guarantee that the reliability used
Longer cycle life.This depends not only on both positive and negative polarity activity, and has sizable relation with collector.Lithium-ion electric
The main material of pond collector is metal foil (such as copper foil, copper foil), and its function is to collect electric current caused by cell active materials
Get up, to form larger electric current output, therefore collector should fully contact with active material, and internal resistance should be as far as possible
Small, this is also the main reason for why lithium ion battery is from price higher copper foil and copper foil.Copper foil has good lead
Electrically, pliability and moderate current potential, resistance to winding and spreading, production technology is more ripe, thus turns into negative electrode of lithium ion battery collection
The preferred material of fluid.
There is presently no international standard and national technical standard, copper foil industry production manufacturer for cathode of lithium battery colelctor electrode copper foil
It is both referred to《International Electro circuit interconnects and technical standard of the encapsulation association about copper foil》(standard number:IPC-4652 in)
Very the regulation of low profile degree copper foil (VLPC) performs;Lithium battery industry typically requires copper foil surface roughness Rz≤2.5um.
Current lithium battery negative collector electrode copper foil has two kinds, is rolled copper foil and electrolytic copper foil respectively.Traditional handicraft
The electrolytic copper foil feature of the manufacturing is:(1) it is that column crystal tissue (2) coarse grains (3) crystal defect is more that copper foil, which separates out face,
(4) surface is more coarse, Rz≤3um.
What very low-profile electrolytic copper foil production technology was different from traditional electrolyte copper foil be to the hole of crystalline texture in copper foil,
Ratio (concentration) shared by the crystal defects such as rearrangement, twin crystal is controlled by, and Main Means are to use new additive agent and foliation bar
The improvement of part (Electrolytic conditions), emphasis be copper foil overall characteristic, surface roughness can reach Rz≤2.5, but electrically
Energy (current density) can decrease.Copper foil surface roughness after conventional process is as shown in table 1.
The traditional electrolyte copper foil surface roughness meter of table 1.
Negative current collector of the lithium ion battery by the use of electrolytic copper foil as lithium ion battery, copper foil both serve as negative pole in the battery
The carrier of active material, collection and the transmission body, therefore, electricity of the copper foil current collector to lithium ion battery of negative pole electron stream are served as again
Chemical property has a great impact, i.e., must have good electric conductivity, and surface energy is uniformly coated negative material and do not fallen off.
Therefore research improves negative current collector copper foil electric conductivity and surface roughness performance, to lithium ion battery charge-discharge performance
Raising have great importance.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide one kind improves cathode of lithium battery copper foil collection
The method of electrode electrical property, specifically deposit one on cathode of lithium battery colelctor electrode copper foil using vacuum plasma coating technique
Layer nanometer Copper thin film, then ion gun bombardment processing is carried out to Copper thin film surface, to improve lithium cell cathode material and colelctor electrode
The adhesive force of copper foil.
To achieve the above object, the technical solution adopted by the present invention is:
A kind of method for improving cathode of lithium battery copper foil colelctor electrode electrical property, using vacuum plasma coating technique in lithium electricity
One layer of nanometer Copper thin film is deposited on the negative collector electrode copper foil of pond, then ion gun bombardment processing is carried out to Copper thin film surface, to carry
The adhesive force of high lithium cell cathode material and colelctor electrode copper foil.
As the present invention preferably scheme, further, this method, which includes, to have the following steps:
A, using take-up type vacuum magnetic-controlled sputtering coating equipment, by 8-16um thickness tradition cathode of lithium battery collection to be processed
Copper foil for electrode is cut to the size of needs in purification room, and the copper foil to be coated after described cut then is loaded into the winding
In formula vacuum magnetron sputtering coating film equipment;
B, the take-up type vacuum magnetic-controlled sputtering coating equipment is operated, adjusting device is extremely plated at Copper thin film and ion gun bombardment
The process conditions of reason;
C, the reel system of the take-up type vacuum magnetic-controlled sputtering coating equipment is adjusted, the take-up type vacuum magnetic will be in
The copper foil to be coated expansion on the let off roll of sputtering coating equipment is controlled, adjustment copper foil winding tension is so that plated film copper foil can unreel
Stable operation on roller;
D, certain thickness is deposited in the copper foil surface to be coated using the take-up type vacuum magnetic-controlled sputtering coating equipment
Copper thin film, copper foil to be coated after plasma deposition Copper thin film, filled and led up by coarse surface crater, surface roughness drop
It is low;
E, using the ion gun of the take-up type vacuum magnetic-controlled sputtering coating equipment to the copper foil surface after deposition Copper thin film
Plasma bombardment processing is carried out, makes to have deposited Copper thin film and is intended to be densified, Copper thin film surface polishes, and roughness is further
Reduce, eliminate the metal internal stress of deposition Copper thin film.
As the present invention preferably scheme, further, 8-16um thickness copper foil described in step a cut after breadth chi
It is very little to be:0.2-0.6m.
As the present invention preferably scheme, further, the work of Copper thin film and ion gun bombardment processing is plated described in step b
Skill condition:Background vacuum 5x10-3Pa, plate Copper thin film and ion gun bombardment processing vacuum 3x10-1Pa。
As the present invention preferably scheme, further, start on the take-up type vacuum magnetic-controlled sputtering coating equipment
Gas mass flow gauge, is filled with high-purity argon gas, plating Copper thin film and ion gun bombardment processing vacuum is reached 3x10-1Pa。
As the present invention preferably scheme, further, the adjustment take-up type vacuum magnetron sputtering described in step c
The reel system of film device includes, and winding speed is arranged to:1.5-3m/min, tension force scope:15-50N.
As the present invention preferably scheme, further, Copper thin film deposit thickness described in step d is 180-400nm.
As the present invention preferably scheme, further, the process conditions of the processing of plasma bombardment described in step e
For:Ion gun bombardment power is 3-5kw, and bombardment speed is 1.5-3m/min.
As the present invention preferably scheme, further, also include step:Bang having plated Copper thin film and having carried out ion gun
The cathode of lithium battery colelctor electrode copper foil for hitting processing carries out conductance and surface roughness test, is vacuum-packed.
After the above method, the present invention has the beneficial effect that:Using magnetic control sputtering vacuum coating technology in negative collector electrode
One layer of nanometer Copper thin film is deposited on copper foil to improve the adhesive force of lithium cell cathode material and colelctor electrode copper foil, reduces interface effect
Should, so as to improve cathode of lithium battery electric conductivity.
Figure of description
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is the handling process principle schematic of the present invention;
Fig. 2 is the process schematic representation using take-up type vacuum magnetron sputtering copper plating film and plasma processing;
Embodiment
Below in conjunction with embodiment of the present invention, the technology in embodiment of the present invention is clearly and completely described,
Obviously, described embodiment only a part of scheme of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment party that those of ordinary skill in the art are obtained under the premise of creative work is not made
Case, belong to the scope of protection of the invention.
With reference to shown in figure 1, a kind of method for improving cathode of lithium battery copper foil colelctor electrode electrical property, plated using vacuum plasma
Membrane technology deposits one layer of nanometer Copper thin film to improve lithium cell cathode material and colelctor electrode copper foil on negative collector electrode copper foil
Adhesive force.
In the present embodiment, the filming equipment used is SJ-RTR-SDH350 take-up type vacuum magnetron sputtering coater, reference
Described in Fig. 2, specifically, implementation steps are as follows:
A, using SJ-RTR-SDH350 take-up type vacuum magnetic-controlled sputtering coating equipments, 8-16um thickness to be processed is passed
System cathode of lithium battery colelctor electrode is cut to breadth size with copper foil in purification room:0.2-0.6m, to be plated after then cutting
The copper foil of film loads in take-up type vacuum magnetic-controlled sputtering coating equipment, prepares at magnetic control sputtering plating copper film and vacuum plasma bombardment
Reason;
B, SJ-RTR-SDH350 take-up type vacuum magnetic-controlled sputtering coating equipments are operated, background vacuum is evacuated to and reaches
5x10-3Pa, it is rear to start gas mass flow gauge, high-purity argon gas is filled with, adjustment flowmeter makes vacuum chamber vacustat exist
3x10-1Pa, meet the process conditions of copper plating film and ion gun bombardment processing;
C, the reel system of SJ-RTR-SDH350 equipment is adjusted, will be in the copper foil exhibition to be coated on let off roll (substrate frame)
Open, according to 1.5m/min-3m/min winding speed (coating speed), the accurate adjustment copper foil surface volume in the range of 15-50N
It is stable to copper foil around tension force, reach copper plating film and bombardment processing condition;
D, the magnetically controlled DC sputtering cathode of SJ-RTR-SDH350 equipment reel systems is opened, is sunk respectively in copper foil surface
The copper film of product 180nm, 300nm, 500nm thickness, surface roughness of the sampling and measuring copper foil after plasma deposition copper film and
Conductance, resistivity;
E, the ion source system of SJ-RTR-SDH350 equipment is opened, it is super to depositing in the range of winding speed 1.5-3m/min
The copper foil surface for crossing 100nm copper films carries out carrying out ion gun bombardment processing, sampling and testing copper film by 3kw, 4kw, 5kw power respectively
Thickness and surface roughness change, judge that ion gun bombardment causes copper film to be intended to densification, roughness reduction;Utilize ion gun
Bombarding energy eliminates the metal internal stress of deposition copper film.
F. after copper plating film and ion gun bombardment processing, SJ-RTR-SDH350 equipment is operated, magnetically controlled DC sputtering is closed with this
Cathode, ion gun, gas mass flow gauge, stop winding transmission, copper foil removal will have been plated after vacuum breaker, has checked copper foil conductance
And it is vacuum-packed after the performance such as surface roughness.
Profit with the aforedescribed process after, draw such as table 2 to the conclusion (of pressure testing) of table 4.
Table 2:Copper foil sputter copper film front and rear surfaces electrical property compares
It can be seen from Table 2 that by the copper layer deposition of 180nm, 300nm, 500nm thickness, find as film thickness increases
Copper foil electrical conductivity is added also to gradually step up, electrical conductivity no longer increases after deposition copper film thickness is more than 300nm, has reduction to become on the contrary
Gesture;Resistivity is gradually reduced also with the increase of copper film thickness simultaneously, and when depositing copper film thickness more than 300nm, resistivity is not
Reduce again and increase tendency is presented, therefore, the thickness of copper film answers value 250-350nm preferable, and optimal value is 300nm.
Table 3:Aluminium foil copper plating film front and rear surfaces roughness ratio compared with
It can be seen from Table 3 that by the copper layer deposition of 180nm, 300nm, 500nm thickness, find as film thickness increases
Copper foil surface roughness is added to be gradually lowered, roughness no longer reduces after deposition of aluminum film thickness is more than 300nm, there is increase on the contrary
Trend, therefore, the thickness of copper film answer value 250-350nm preferable, and optimal value is 300nm.
Table 4:Film characteristics before and after the bombardment of copper plating film copper foil ion gun
No. | Crystallite dimension (nm) | Film thickness change (nm) | Bombard power | Copper foil mean roughness (Rz) |
1 | 37.2 | 1035±10 | 0 | 5.2 |
2 | 29.6 | 915±10 | 2kw | 3.0 |
3 | 30.0 | 848±10 | 3kw | 2.7 |
As can be seen from Table 4, the copper film thickness without ion gun bombardment is 1035nm, and the copper film thickness by bombardment occurs
Change is 915nm, 848nm respectively.As can be seen that when ion gun bombardment time increase, film thickness reduces, and film is intended to
Densification, film surface substantially polish, and roughness reduces.As can be seen that after sputter bombards, the obvious darkening of film surface
Sliding, roughness reduces, and film mean roughness is reduced to 2.7nm by 5.2nm, and film crystallite dimension reduces, and is not banged using ion gun
Hit, ion gun bombardment 1min and 2min rear film crystallite dimensions are respectively 37,29.5 and 30.0nm.Number is bombarded by ion gun
Increase, bombarding energy accumulation, reduce roughness of film and crystallite dimension.
In the description of this specification, reference term " embodiment ", " some embodiments ", " an implementation
The description of example ", " some embodiments ", " example ", " specific example " or " some examples " etc. means to combine the embodiment or example
Specific features, structure, material or the feature of description are contained at least one embodiment or example of the present invention.In this explanation
In book, identical embodiment or example are not necessarily referring to the schematic representation of above-mentioned term.Moreover, the specific spy of description
Sign, structure, material or feature can combine in an appropriate manner in any one or more embodiments or example.
Above content is to combine specific embodiment further description made for the present invention, it is impossible to assert this hair
Bright specific implementation is confined to these explanations.For general technical staff of the technical field of the invention, do not taking off
On the premise of from present inventive concept, some simple deduction or replace can also be made.
Claims (9)
- A kind of 1. method for improving cathode of lithium battery copper foil colelctor electrode electrical property, it is characterised in that utilize vacuum plasma plated film skill Art deposits one layer of nanometer Copper thin film on cathode of lithium battery colelctor electrode copper foil, then Copper thin film surface is carried out at ion gun bombardment Reason, to improve the adhesive force of lithium cell cathode material and colelctor electrode copper foil.
- A kind of 2. method for improving cathode of lithium battery copper foil colelctor electrode electrical property according to claim 1, it is characterised in that Comprising having the following steps:A, using take-up type vacuum magnetic-controlled sputtering coating equipment, by 8-16um thickness tradition cathode of lithium battery colelctor electrode to be processed The size of needs is cut in purification room with copper foil, it is true that the copper foil to be coated after described cut then is loaded into the takeup type In empty magnetic-controlled sputtering coating equipment;B, the take-up type vacuum magnetic-controlled sputtering coating equipment is operated, adjusting device extremely plating Copper thin film and ion gun bombardment processing Process conditions;C, the reel system of the take-up type vacuum magnetic-controlled sputtering coating equipment is adjusted, will be splashed in the take-up type vacuum magnetic control The copper foil to be coated expansion penetrated on the let off roll of filming equipment, adjustment copper foil winding tension is so that plated film copper foil can be on let off roll Stable operation;D, certain thickness copper is deposited in the copper foil surface to be coated using the take-up type vacuum magnetic-controlled sputtering coating equipment Film, copper foil to be coated after plasma deposition Copper thin film, filled and led up by coarse surface crater, and surface roughness reduces;E, the copper foil surface after deposition Copper thin film is carried out using the ion gun of the take-up type vacuum magnetic-controlled sputtering coating equipment Plasma bombardment processing, makes to have deposited Copper thin film and is intended to be densified, and Copper thin film surface polishes, and roughness further drops It is low, eliminate the metal internal stress of deposition Copper thin film.
- A kind of 3. method for improving cathode of lithium battery copper foil colelctor electrode electrical property according to claim 2, it is characterised in that Breadth size after 8-16um thickness copper foil described in step a is cut is:0.2-0.6m.
- A kind of 4. method for improving cathode of lithium battery copper foil colelctor electrode electrical property according to claim 2, it is characterised in that The process conditions of Copper thin film and ion gun bombardment processing are plated described in step b:Background vacuum 5x10-3Pa, plate Copper thin film and from Component bombardment processing vacuum 3x10-1Pa。
- A kind of 5. method for improving cathode of lithium battery copper foil colelctor electrode electrical property according to claim 2, it is characterised in that The reel system of the adjustment take-up type vacuum magnetic-controlled sputtering coating equipment described in step c includes, and winding speed is arranged to: 1.5-3m/mi n, tension force scope:15-50N.
- A kind of 6. method for improving cathode of lithium battery copper foil colelctor electrode electrical property according to claim 2, it is characterised in that Copper thin film deposit thickness described in step d is 250-350nm.
- A kind of 7. method for improving cathode of lithium battery copper foil colelctor electrode electrical property according to claim 2, it is characterised in that Plasma bombardment described in step e processing process conditions be:Ion gun bombardment power is 3-5kw, and bombardment speed is 1.5- 3m/mi n。
- A kind of 8. method for improving cathode of lithium battery copper foil colelctor electrode electrical property according to claim 2, it is characterised in that Also include step:Led to having plated Copper thin film and having carried out the cathode of lithium battery colelctor electrode copper foil of ion gun bombardment processing Electric rate and surface roughness test, is vacuum-packed.
- A kind of 9. method for improving cathode of lithium battery copper foil colelctor electrode electrical property according to claim 4, it is characterised in that Start gas mass flow gauge on the take-up type vacuum magnetic-controlled sputtering coating equipment, be filled with high-purity argon gas, make plating Copper thin film And ion gun bombardment processing vacuum reaches 3x10-1Pa。
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CN110993886A (en) * | 2019-12-26 | 2020-04-10 | 北京师范大学 | Preparation device for lithium battery current collector |
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CN107768677A (en) * | 2017-09-18 | 2018-03-06 | 深圳市烯谷能源控股有限公司 | A kind of method for improving lithium ion cell positive colelctor electrode corrosion resisting property |
CN116751070B (en) * | 2023-07-03 | 2023-11-17 | 江苏富乐华功率半导体研究院有限公司 | Preparation method of ceramic aluminum-clad substrate and ceramic aluminum-clad substrate prepared by same |
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