CN116100027A - Preparation method of laser scanning assisted laminated foil - Google Patents
Preparation method of laser scanning assisted laminated foil Download PDFInfo
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- CN116100027A CN116100027A CN202310352697.8A CN202310352697A CN116100027A CN 116100027 A CN116100027 A CN 116100027A CN 202310352697 A CN202310352697 A CN 202310352697A CN 116100027 A CN116100027 A CN 116100027A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
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- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 103
- 239000000758 substrate Substances 0.000 claims abstract description 83
- 239000002002 slurry Substances 0.000 claims abstract description 49
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 230000001680 brushing effect Effects 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- 230000015572 biosynthetic process Effects 0.000 claims description 28
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- 239000002033 PVDF binder Substances 0.000 claims description 10
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000008213 purified water Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 7
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- 239000011261 inert gas Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 23
- 239000011148 porous material Substances 0.000 abstract description 13
- 238000009826 distribution Methods 0.000 abstract description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002344 surface layer Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- 230000001276 controlling effect Effects 0.000 description 14
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 239000011259 mixed solution Substances 0.000 description 10
- 230000006872 improvement Effects 0.000 description 8
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- 238000000635 electron micrograph Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 4
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- 238000000576 coating method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
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- 238000013461 design Methods 0.000 description 2
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- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
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- 239000002356 single layer Substances 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 description 1
- 239000001741 Ammonium adipate Substances 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
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- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000019293 ammonium adipate Nutrition 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
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- 239000003990 capacitor Substances 0.000 description 1
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- 238000003475 lamination Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
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- 230000000007 visual effect Effects 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
- B22F2007/042—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
- B22F2007/045—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method accompanied by fusion or impregnation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the technical field of electrode foil manufacturing, in particular to a laser scanning assisted laminated foil preparation method, which comprises the following steps: preparing aluminum powder slurry; brushing aluminum powder slurry on an aluminum foil substrate in a laser presintering stage, and performing full scanning by utilizing laser; repeating the above steps for a plurality of times; and a final sintering stage. In this way, the aluminum powder slurry on the aluminum foil substrate is presintered by means of laser before final high-temperature sintering, and is divided into a plurality of times. After the primary aluminum powder slurry is brushed, the aluminum powder at the bottommost layer is tightly fused with an aluminum oxide layer which is generated by heating and is not shaped, and the aluminum powder slurry in the solidified and formed state at the bottom layer contains a large number of pores with excellent overall distribution uniformity, and the aluminum powder slurry floating on the surface layer and not solidified and formed completely is removed before the next brushing operation is formally executed, so that the finally formed laminated foil has excellent gap distribution form and overall compactness.
Description
Technical Field
The invention relates to the technical field of electrode foil manufacturing, in particular to a preparation method of a laser scanning assisted laminated foil.
Background
The laminated foil is a new generation product of electrode foil, and a brand new powder sintering process is adopted. Compared with the traditional corrosion process electrode foil, the capacitor performance of the laminated foil is greatly improved (the specific volume is improved by more than 40 percent), the production process is environment-friendly, and no acid-base reaction and waste liquid discharge are caused.
At present, the laminated foil is produced mainly by loading treated aluminum powder particles on an aluminum conductive foil substrate through a binder and sintering at a high temperature. For example, the most common lamination foil is prepared by the following steps:
s1, grinding aluminum powder, mixing 100 weight portions of the ground powder, 30 weight portions of carboxymethyl cellulose salt and 10 weight portions of water, and uniformly stirring.
S2, coating the slurry mixed in the step S1 on the surface of an aluminum foil substrate, and then drying the aluminum foil.
S3, sintering the aluminum foil prepared in the step S2 as follows: 15 Heating to 110 ℃ at a constant rate within a minute, preserving heat for 15 minutes, heating to 450 ℃ at a constant rate within 3.5 hours, preserving heat for 2 hours, heating to 520 ℃ at a constant rate within a period of 1 hour, and preserving heat for 4 hours.
And S4, cooling the sintered foil obtained in the step S3, and performing conventional formation treatment.
The existing general laminated foil process has the following problems: 1) It is known that the porosity (i.e. the total ratio of pores in the sintered layer) is closely related to the performance parameters of the laminated foil, such as the capacity and the structural strength. However, in the current preparation process, the porosity can be regulated and controlled by changing the powder-gel ratio, however, uniformity is difficult to be consistent in the overall area of the aluminum foil matrix after coating, and finally, the uniformity of pore distribution of the formed laminated foil is extremely poor (as can be intuitively seen in the first figure); 2) The bonding strength of the solidified sizing agent and the aluminum foil matrix is seriously insufficient, and the sizing agent is extremely easy to peel off or fall off in a large area under the action of external force (can be intuitively seen in the figure I); 3) Because the aluminum powder is seriously unevenly distributed in the slurry, the structural strength in each area of the aluminum powder is relatively great after being presintered in the sintering process, the quality of the final finished product of the laminated foil is finally affected, and the most visual appearance is that the bending resistance times are obviously insufficient; 4) On the premise that the capacity and strength of the laminated foil meet the requirements of customers, a large number of orthogonal tests are needed in the process of developing new products in order to seek the optimal porosity, so that the development cost and difficulty are increased; 5) Due to the excessively high gum ratio in the slurry coating, the degumming time and the degumming difficulty tend to be greatly increased in the warm sintering process, and finally the preparation period of single-batch laminated foil is prolonged. Thus, a technician is required to solve the above problems.
Disclosure of Invention
Accordingly, in view of the above-mentioned problems and drawbacks, the present inventors have collected related data, and have conducted many experiments and modifications by those skilled in the art, which have been developed and experienced for many years, to finally result in the laser scanning assisted laminated foil manufacturing method.
In order to solve the technical problems, the invention relates to a preparation method of a laser scanning assisted laminated foil, which comprises the following steps:
s1, preparing a working stage; cleaning the precoated surface of the aluminum foil matrix, and screening aluminum powder for presintering;
s2, preparing aluminum powder slurry; immersing the aluminum powder obtained in the step S1 in polyvinylidene fluoride solution, and uniformly mixing;
s3, a laser presintering stage comprises the following substeps:
s31, brushing the aluminum powder slurry prepared in the step S2 on an aluminum foil substrate;
s32, placing the aluminum foil substrate obtained in the step S31 in an inert gas atmosphere, and carrying out full scanning on the brushed surface by utilizing laser;
s33, immersing the aluminum foil substrate obtained in the step S32 into sodium hydroxide solution until the aluminum powder sintered layer is completely immersed; after the aluminum foil substrate is immersed, applying ultrasonic waves to the sodium hydroxide solution;
s34, repeating the steps S31 to S33 at least twice;
s35, placing the aluminum foil substrate obtained in the step S34 into a high-temperature environment for drying until moisture is completely gasified and escapes;
s4, in the formal sintering stage,
s41, placing the aluminum foil substrate obtained in the step 35 into a muffle furnace, firstly, heating to 390-410 ℃ at uniform speed within 1-2 h, and preserving heat for 1-3 h; then, the temperature is increased to 550-600 ℃ at uniform speed within 0.5-1 h, and the temperature is kept for 3-5 h again until sintering is completed;
s42, continuously placing the aluminum foil substrate obtained in the step 41 in a muffle furnace for cooling along with the furnace, and naturally cooling the inner cavity of the muffle furnace due to the loss of power supply until the temperature is reduced to below 20 ℃.
S5, in the formation stage, the aluminum foil substrate obtained in the step 42 is subjected to formation treatment, and a laminated foil finished product is obtained.
As a further improvement of the technical scheme of the invention, in step S1, the aluminum foil substrate is immersed in a cleaning tank of an ultrasonic cleaner, and the cleaning liquid is purified water and drained.
As a further modification of the above-described solution, of course, in step S1 the precoated surface of the aluminum foil substrate is rinsed with high-pressure purified water and drained.
As a further improvement of the technical scheme of the invention, in the step S1, the initial thickness of the aluminum foil matrix is controlled to be 30-60 mu m, and the average particle size of the screened aluminum powder is controlled to be 3-8 mu m.
As a further improvement of the technical scheme of the invention, in the step S2, the concentration of the polyvinylidene fluoride solution is controlled to be 5-15 wt%.
As a further improvement of the technical scheme of the invention, in the step S31, the aluminum powder slurry is brushed on the aluminum foil matrix in an alternating manner of transverse brushing and longitudinal brushing, and the total layer thickness of the aluminum powder slurry in a fluid state is controlled to be 25-30 mu m.
As a still further improvement of the present invention, in step S32, the aluminum foil substrate is placed in a nitrogen or helium atmosphere. In the laser full scanning process, the power P of the laser is controlled to be 300-350W, the spot diameter d is controlled to be 0.3-0.5-mm, the scanning speed v is less than 1100 mm/min.
As a further improvement of the technical scheme of the invention, in the step S33, the concentration of the sodium hydroxide solution is controlled to be 0.05-0.2 wt percent.
As a further improvement of the technical scheme of the invention, in the step S33, the ultrasonic frequency is controlled to be 200-300 KHZ, and the duration is 0.5-2 min.
As a further improvement of the technical scheme of the invention, in the step S35, the aluminum foil substrate is placed in an environment of 100-150 ℃ and kept for 30-40 min.
In the technical scheme disclosed by the invention, the aluminum powder slurry on the aluminum foil substrate is presintered by means of laser before formal high-temperature sintering and is carried out for a plurality of times. After the primary aluminum powder slurry is brushed, the primary aluminum powder slurry is subjected to laser instant scanning, so that aluminum powder distributed at the bottommost layer is first tightly fused with an aluminum oxide layer which is generated by laser heat and is not shaped yet, the aluminum powder slurry in the bottom layer and in a fully solidified state contains a large number of pores, the overall distribution uniformity is excellent, the aluminum powder slurry which floats on the surface and is not fully solidified is removed through the cooperation of sodium hydroxide solution and ultrasonic waves, and the aluminum powder slurry is continuously brushed and densely molded to form a bedding for the follow-up aluminum powder slurry, so that the follow-up design of changing the aluminum powder proportion adhered on the surface of an aluminum foil substrate and optimizing the pore distribution uniformity of the finally molded laminated foil through adjusting laser power, scanning interval and spot diameter is expected to be possible.
Here, the number of laser presintering times of the aluminum powder slurry also has an important effect on the porosity and pore distribution morphology of the final molded laminated foil. The reason is that the larger the average size of the pores contained in the aluminum foil matrix is, the larger the total ratio is, the more the aluminum foil matrix is, for the single-layer aluminum powder slurry presintered layer, so that the porosity and the uniformity of pore distribution are effectively controlled by reducing the single brushing amount of the aluminum powder slurry and adopting a multi-time laser presintered mode.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a photograph of a laminate foil prepared by a conventional process (X350 in the cross-cut state) by electron microscopy.
FIG. 2 is an electron micrograph (cross cut) of a laminated foil prepared according to a first embodiment of the disclosed laser scanning assisted laminated foil preparation method (x 350).
FIG. 3 is a photograph of a first embodiment of a laser scanning assisted laminated foil according to the present invention (cross cut, 1000).
FIG. 4 is a photograph of a first embodiment of a laser scanning assisted laminated foil according to the present invention (cross cut, 5000).
FIG. 5 is an electron micrograph (cross cut) of a laminated foil prepared according to a second embodiment of the disclosed laser scanning assisted laminated foil preparation method (x 350).
FIG. 6 is an electron micrograph (cross cut) of a laminated foil prepared according to a third embodiment of the disclosed laser scanning assisted laminated foil preparation method (x 350).
FIG. 7 is an electron micrograph (cross cut) of a laminated foil prepared according to a fourth embodiment of the disclosed laser scanning assisted laminated foil preparation method (x 350).
Description of the embodiments
The present invention will be further described in detail with reference to examples, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention. The methods are conventional methods unless otherwise specified.
In order to more intuitively demonstrate the beneficial effects produced by the technical solution of the present invention, a set of comparative tests are also presented below, as indicated in the background section herein, and are not described in detail herein.
Fig. 1 shows an electron micrograph (cross cut, x 350) of a laminated foil prepared using a general procedure.
Example 1
The preparation method of the laser scanning assisted laminated foil comprises the following steps:
s1, preparing a working stage; immersing an aluminum foil substrate with the thickness of 30 mu m into a cleaning tank of an ultrasonic cleaning machine, wherein the cleaning liquid is purified water, and draining to finish the cleaning operation of a precoated surface of the aluminum foil substrate, and screening aluminum powder for presintering, wherein the average particle size of the screened aluminum powder is controlled to be 3-8 mu m;
s2, preparing aluminum powder slurry; immersing the aluminum powder obtained in the step S1 in polyvinylidene fluoride solution (5 wt%) and uniformly mixing;
s3, a laser presintering stage comprises the following substeps:
s31, brushing the aluminum powder slurry prepared in the step S2 on an aluminum foil substrate in an alternating manner of horizontal brushing and vertical brushing, wherein the total layer thickness of the aluminum powder slurry in a fluid form is controlled to be 25-30 mu m;
s32, placing the aluminum foil substrate obtained in the step S31 in an inert gas atmosphere, and carrying out full scanning on the brushed surface by utilizing laser; in the laser full scanning process, the power P of the laser is 300W, the spot diameter d is 0.4mm, the raster scanning is performed, and the scanning speed v is 1100 mm/min.
S33, immersing the aluminum foil substrate obtained in the step S32 into sodium hydroxide solution (0.2 wt%) until the aluminum powder sintered layer is completely immersed; after the aluminum foil matrix is immersed, applying ultrasonic waves to the sodium hydroxide solution for 2min;
s34, repeating the steps S31 to S33 twice;
s35, placing the aluminum foil substrate obtained in the step S34 into a high-temperature environment at 120 ℃ for drying, and maintaining for 30min;
s4, in the formal sintering stage,
s41, placing the aluminum foil substrate obtained in the step 35 into a muffle furnace, firstly, uniformly heating to 390 ℃ within 1h, and preserving heat for 3h; then, the temperature is increased to 550 ℃ at uniform speed within 1h, and the temperature is kept for 4h again until the sintering is completed;
s42, continuously placing the aluminum foil substrate obtained in the step 41 in a muffle furnace for cooling along with the furnace, and naturally cooling the inner cavity of the muffle furnace due to the loss of power supply until the temperature is reduced to below 20 ℃;
s5, performing formation treatment to obtain a laminated foil finished product:
the specific steps taken in the specific experiments are listed here for reference, specifically:
the formation phase comprises the following sub-steps:
s51, placing the aluminum foil substrate obtained in the step S42 into pure water, and boiling the aluminum foil substrate in water at 80-98 ℃ for 8-10 min. Then placing the mixture into a mixed solution of adipic acid (0.1-0.15 wt%), ammonium adipate (0.1-0.2 wt%), boric acid (0.1-0.15 wt%) and maleic acid (0.01-0.03 wt%) for primary formation, controlling the temperature of the mixed solution at 80-90 ℃, controlling the duration at 5-10 min and controlling the formation voltage at 140-170V;
s52, placing the aluminum foil substrate obtained in the step S51 into a mixed solution of citric acid (0.04-0.06 wt%), ammonium citrate (0.01-0.05 wt%) and boric acid (0.1-0.2 wt%) for secondary formation, controlling the temperature of the mixed solution at 80-90 ℃, controlling the duration at 5-10 min, and controlling the formation voltage at 200-300V;
s53, placing the aluminum foil substrate obtained in the step S52 into a mixed solution of citric acid (0.03-0.05 wt%), ammonium citrate (0.03-0.05 wt%) and boric acid (0.4-1 wt%) for three-stage formation, controlling the temperature of the mixed solution at 80-90 ℃, controlling the duration at 5-10 min, and controlling the formation voltage at 400-450V;
s54, placing the aluminum foil substrate obtained in the step S53 into a mixed solution of citric acid (0.01-0.05 wt%), ammonium citrate (0.01-0.06 wt%), boric acid (0.4-1 wt%) and azelaic acid (0.001-0.005 wt%) for four-stage formation, controlling the temperature of the mixed solution at 80 and the aluminum foil substrate at 90 ℃ for 15-20 min, and controlling the formation voltage at 540-560V;
s55, immersing the aluminum foil substrate obtained in the step S54 in 75-80 wt% of ammonia water at 70-80 ℃ and keeping for 5-10 min;
s56, repeating the step S54 to perform the subsequent formation treatment on the aluminum foil substrate obtained in the step S55;
s57, repeating the step S55 to process the aluminum foil matrix obtained in the step S56;
s58, placing the aluminum foil substrate obtained in the step S57 into a high-temperature environment of 480-500 ℃ for heat treatment, and maintaining the duration of the heat treatment at 2-5 min;
s59, placing the aluminum foil substrate obtained in the step S58 into a mixed solution of citric acid (0.005-0.01 wt%), ammonium citrate (0.005-0.01 wt%) and boric acid (0.2-0.5 wt%) for secondary formation, controlling the temperature of the mixed solution at 80-90 ℃, controlling the duration at 10-15 min, and controlling the formation voltage at 540-560V;
s60, immersing the aluminum foil substrate obtained in the step S59 into phosphoric acid (5-10 wt%) at 70-90 ℃ for 5-10 min;
s61, repeating the step S58 to process the aluminum foil matrix obtained in the step S60;
s62, repeating the step S59 to perform post-tertiary formation on the aluminum foil substrate obtained in the step S61;
s63, immersing the aluminum foil substrate obtained in the step S62 into ammonium dihydrogen phosphate (5-10 wt%) at 70-90 ℃ for 5-10 min;
s64, placing the aluminum foil substrate obtained in the step S63 into an oven for drying, maintaining the temperature of the inner cavity of the oven at 100-120 ℃, and cooling to obtain a laminated foil finished product.
Fig. 2, 3 and 4 show electron microscope scanning photographs of laminated foils prepared by the first embodiment of the disclosed laser scanning assisted laminated foil preparation method at different magnifications (x 350, ×1000, ×5000), respectively.
Examples
The preparation method of the laser scanning assisted laminated foil comprises the following steps:
s1, preparing a working stage; immersing an aluminum foil substrate with the thickness of 30 mu m into a cleaning tank of an ultrasonic cleaning machine, wherein the cleaning liquid is purified water, and draining to finish the cleaning operation of a precoated surface of the aluminum foil substrate, and screening aluminum powder for presintering, wherein the average particle size of the screened aluminum powder is controlled to be 3-8 mu m;
s2, preparing aluminum powder slurry; immersing the aluminum powder obtained in the step S1 in polyvinylidene fluoride solution (5 wt%) and uniformly mixing;
s3, a laser presintering stage comprises the following substeps:
s31, brushing the aluminum powder slurry prepared in the step S2 on an aluminum foil substrate in an alternating manner of horizontal brushing and vertical brushing, wherein the total layer thickness of the aluminum powder slurry in a fluid form is controlled to be 25-30 mu m;
s32, placing the aluminum foil substrate obtained in the step S31 in an inert gas atmosphere, and carrying out full scanning on the brushed surface by utilizing laser; in the laser full scanning process, the power P of the laser is 400W, the spot diameter d is 0.45mm, the raster scanning is performed, and the scanning speed v is 750 mm/min.
S33, immersing the aluminum foil substrate obtained in the step S32 into sodium hydroxide solution (0.2 wt%) until the aluminum powder sintered layer is completely immersed; after the aluminum foil matrix is immersed, applying ultrasonic waves to the sodium hydroxide solution for 2min;
s34, repeating the steps S31 to S33 twice;
s35, placing the aluminum foil substrate obtained in the step S34 into a high-temperature environment at 120 ℃ for drying, and maintaining for 30min;
s4, in the formal sintering stage,
s41, placing the aluminum foil substrate obtained in the step 35 into a muffle furnace, firstly, uniformly heating to 400 ℃ within 1.5h, and preserving heat for 1.5 h; then, the temperature is increased to 550 ℃ at uniform speed within 1h, and the temperature is kept for 4h again until the sintering is completed;
s42, continuously placing the aluminum foil substrate obtained in the step 41 in a muffle furnace for cooling along with the furnace, and naturally cooling the inner cavity of the muffle furnace due to the loss of power supply until the temperature is reduced to below 20 ℃.
S5, in the formation stage, the aluminum foil substrate obtained in the step 42 is subjected to formation treatment, and a laminated foil finished product is obtained.
The formation steps disclosed in embodiment 1 are performed completely, and are not repeated here for the sake of brevity.
FIG. 5 is a photograph of a second embodiment of a laser scanning assisted laminated foil manufacturing method according to the present invention (cross cut, x 350)
Examples
The preparation method of the laser scanning assisted laminated foil comprises the following steps:
s1, preparing a working stage; immersing an aluminum foil substrate with the thickness of 30 mu m into a cleaning tank of an ultrasonic cleaning machine, wherein the cleaning liquid is purified water, and draining to finish the cleaning operation of a precoated surface of the aluminum foil substrate, and screening aluminum powder for presintering, wherein the average particle size of the screened aluminum powder is controlled to be 3-8 mu m;
s2, preparing aluminum powder slurry; immersing the aluminum powder obtained in the step S1 in polyvinylidene fluoride solution (5 wt%) and uniformly mixing;
s3, a laser presintering stage comprises the following substeps:
s31, brushing the aluminum powder slurry prepared in the step S2 on an aluminum foil substrate in an alternating manner of horizontal brushing and vertical brushing, wherein the total layer thickness of the aluminum powder slurry in a fluid form is controlled to be 25-30 mu m;
s32, placing the aluminum foil substrate obtained in the step S31 in an inert gas atmosphere, and carrying out full scanning on the brushed surface by utilizing laser; in the laser full scanning process, the power P of the laser is 300W, the spot diameter d is 0.42mm, the raster scanning is performed, and the scanning speed v is 950 mm/min.
S33, immersing the aluminum foil substrate obtained in the step S32 into sodium hydroxide solution (0.2 wt%) until the aluminum powder sintered layer is completely immersed; after the aluminum foil matrix is immersed, applying ultrasonic waves to the sodium hydroxide solution for 2min;
s34, repeating the steps S31 to S33 twice;
s35, placing the aluminum foil substrate obtained in the step S34 into a high-temperature environment at 120 ℃ for drying, and maintaining for 30min;
s4, in the formal sintering stage,
s41, placing the aluminum foil substrate obtained in the step 35 into a muffle furnace, firstly, uniformly heating to 400 ℃ within 1.5h, and preserving heat for 3h; then, the temperature is increased to 550 ℃ at uniform speed within 1h, and the temperature is kept for 3.5h again until the sintering is completed;
s42, continuously placing the aluminum foil substrate obtained in the step 41 in a muffle furnace for cooling along with the furnace, and naturally cooling the inner cavity of the muffle furnace due to the loss of power supply until the temperature is reduced to below 20 ℃.
S5, in the formation stage, the aluminum foil substrate obtained in the step 42 is subjected to formation treatment, and a laminated foil finished product is obtained.
The formation steps disclosed in embodiment 1 are performed completely, and are not repeated here for the sake of brevity.
Fig. 6 shows an electron microscope photograph (cross cut, x 350) of a laminated foil prepared using a third embodiment of the disclosed laser scanning assisted laminated foil preparation method.
Examples
The preparation method of the laser scanning assisted laminated foil comprises the following steps:
s1, preparing a working stage; immersing an aluminum foil substrate with the thickness of 30 mu m into a cleaning tank of an ultrasonic cleaning machine, wherein the cleaning liquid is purified water, and draining to finish the cleaning operation of a precoated surface of the aluminum foil substrate, and screening aluminum powder for presintering, wherein the average particle size of the screened aluminum powder is controlled to be 3-8 mu m;
s2, preparing aluminum powder slurry; immersing the aluminum powder obtained in the step S1 in polyvinylidene fluoride solution (5 wt%) and uniformly mixing;
s3, a laser presintering stage comprises the following substeps:
s31, brushing the aluminum powder slurry prepared in the step S2 on an aluminum foil substrate in an alternating manner of horizontal brushing and vertical brushing, wherein the total layer thickness of the aluminum powder slurry in a fluid form is controlled to be 25-30 mu m;
s32, placing the aluminum foil substrate obtained in the step S31 in an inert gas atmosphere, and carrying out full scanning on the brushed surface by utilizing laser; in the laser full scanning process, the power P of the laser is 400W, the spot diameter d is 0.45mm, the raster scanning is performed, and the scanning speed v is 830 mm/min.
S33, immersing the aluminum foil substrate obtained in the step S32 into sodium hydroxide solution (0.2 wt%) until the aluminum powder sintered layer is completely immersed; after the aluminum foil matrix is immersed, applying ultrasonic waves to the sodium hydroxide solution for 2min;
s34, repeating the steps S31 to S33 twice;
s35, placing the aluminum foil substrate obtained in the step S34 into a high-temperature environment at 120 ℃ for drying, and maintaining for 30min;
s4, in the formal sintering stage,
s41, placing the aluminum foil substrate obtained in the step 35 in a muffle furnace, firstly, heating to 410 ℃ at uniform speed within 2h, and preserving heat for 2 h; then, the temperature is increased to 600 ℃ at uniform speed within 2 hours, and the temperature is kept for 4.5 hours again until the sintering is completed;
s42, continuously placing the aluminum foil substrate obtained in the step 41 in a muffle furnace for cooling along with the furnace, and naturally cooling the inner cavity of the muffle furnace due to the loss of power supply until the temperature is reduced to below 20 ℃.
S5, in the formation stage, the aluminum foil substrate obtained in the step 42 is subjected to formation treatment, and a laminated foil finished product is obtained.
The formation steps disclosed in embodiment 1 are performed completely, and are not repeated here for the sake of brevity.
Fig. 7 shows an electron microscope photograph (in cross-cut state, x 350) of a laminated foil prepared by a fourth embodiment of the disclosed laser scanning assisted laminated foil preparation method.
As can be seen from the subsequent comparative analysis, the following technical effects are obtained in comparison with the comparative examples, whether in example 1 or examples 2, 3 and 4:
1) The porosity of the aluminum powder sintered layer is greatly improved, the uniformity of pore distribution is better, and the capacity and the structural strength of the final imaging laminated foil are further improved. With respect to the porosity index only, in the comparative example, the porosity was 18.4%, whereas in examples 1, 2, 3, 4, the porosities were 20.1%,24.5%, 22.1%,23.6%, respectively;
2) After the detail comparison of the electron microscope photo, the cured aluminum powder slurry and the aluminum foil matrix keep good combination degree, namely, the formed laminated foil can still keep good structural stability for a long time even if the laminated foil is acted by external force in the actual application process, and layering phenomenon can not occur;
3) The distribution uniformity of aluminum powder in the slurry is greatly improved, so that the structural strength values in all areas of the pre-sintered laminated foil are not greatly different in the sintering process, the final formed laminated foil is ensured to have higher finished product quality, and the bending resistance times of the final formed laminated foil are obviously improved;
4) The polyvinylidene fluoride has extremely low duty ratio in aluminum paste coating, so that the reduction of degumming time and the reduction of degumming difficulty in the subsequent sintering process at a temperature are facilitated.
According to mechanism analysis, in the technical scheme disclosed by the invention, the aluminum powder slurry on the aluminum foil substrate is presintered by means of laser before formally sintering at high temperature and is carried out in multiple times. After the primary aluminum powder slurry is brushed, the primary aluminum powder slurry is subjected to laser instant scanning, so that aluminum powder distributed at the bottommost layer is tightly fused with an unshaped aluminum oxide layer generated by laser heat through a very small amount of polyvinylidene fluoride solution (adhesive), the aluminum powder slurry in the bottom layer and the completely solidified state contains a large number of pores, the overall distribution uniformity is very good, the uncured aluminum powder slurry is removed through the cooperation of sodium hydroxide solution and ultrasonic waves, and the aluminum powder slurry is continuously brushed and padded, so that the follow-up design of changing the aluminum powder proportion adhered on the surface of an aluminum foil substrate and optimizing the pore distribution uniformity of the finally formed laminated foil through adjusting the laser power, the scanning interval and the spot diameter is expected to be possible.
Here, the number of laser presintering times of the aluminum powder slurry also has a great influence on the porosity of the final molded laminated foil. The reason is that the larger the average size of the pores contained in the aluminum foil matrix is, the larger the total ratio is, the more the aluminum foil matrix is, for the single-layer aluminum powder slurry presintered layer, so that the porosity and the uniformity of pore distribution are effectively controlled by reducing the single brushing amount of the aluminum powder slurry and adopting a multi-time laser presintered mode.
Finally, table 1 is a summary of the test results of specific volume, porosity and number of bending resistance of the laminated foils obtained in examples 1-4 and comparative tests.
TABLE 1
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The preparation method of the laser scanning assisted laminated foil is characterized by comprising the following steps of:
s1, preparing a working stage; cleaning the precoated surface of the aluminum foil matrix, and screening aluminum powder for presintering;
s2, preparing aluminum powder slurry; immersing the aluminum powder obtained in the step S1 in polyvinylidene fluoride solution, and uniformly mixing;
s3, a laser presintering stage comprises the following substeps:
s31, brushing the aluminum powder slurry prepared in the step S2 on an aluminum foil substrate;
s32, placing the aluminum foil substrate obtained in the step S31 in an inert gas atmosphere, and carrying out full scanning on the brushed surface by utilizing laser;
s33, immersing the aluminum foil substrate obtained in the step S32 into sodium hydroxide solution until the aluminum powder sintered layer is completely immersed; after the aluminum foil substrate is immersed, applying ultrasonic waves to the sodium hydroxide solution;
s34, repeating the steps S31 to S33 at least twice;
s35, placing the aluminum foil substrate obtained in the step S34 into a high-temperature environment for drying until moisture is completely gasified and escapes;
s4, in the formal sintering stage,
s41, placing the aluminum foil substrate obtained in the step 35 into a muffle furnace, firstly, heating to 390-410 ℃ at uniform speed within 1-2 h, and preserving heat for 1-3 h; then, the temperature is increased to 550-600 ℃ at uniform speed within 0.5-1 h, and the temperature is kept for 3-5 h again until sintering is completed;
s42, continuously placing the aluminum foil substrate obtained in the step 41 in a muffle furnace for cooling along with the furnace, and naturally cooling the inner cavity of the muffle furnace due to the loss of power supply until the temperature is reduced to below 20 ℃;
s5, in the formation stage, the aluminum foil substrate obtained in the step 42 is subjected to formation treatment, and a laminated foil finished product is obtained.
2. The method of manufacturing a laser scanning assisted laminated foil according to claim 1, wherein in step S1, the aluminum foil substrate is immersed in a cleaning tank of an ultrasonic cleaner, and the cleaning liquid is purified water and drained.
3. The method of manufacturing a laser scanning assisted laminated foil according to claim 1, characterized in that in step S1 the pre-coated surface of the aluminum foil substrate is rinsed with purified water under high pressure and drained.
4. The method of manufacturing a laser scanning-assisted laminated foil according to claim 1, wherein in step S1, the initial thickness of the aluminum foil substrate is controlled to be 30 to 60 μm, and the average particle diameter of the aluminum powder after screening is controlled to be 3 to 8 μm.
5. The method of producing a laser scanning assisted laminated foil according to any of claims 2 to 4, wherein in step S2 the concentration of the polyvinylidene fluoride solution is controlled to be 5 to 15wt%.
6. The method of manufacturing a laser scanning assisted laminated foil according to claim 5, wherein in step S31, the aluminum powder slurry is brushed on the aluminum foil substrate in an alternating manner of horizontal brushing and vertical brushing, and the total layer thickness of the aluminum powder slurry in the fluid state is controlled to be 25-30 μm.
7. The method of manufacturing a laser scanning assisted laminated foil according to claim 6, wherein in step S32, the aluminum foil substrate is placed in a nitrogen or helium atmosphere; in the laser full scanning process, the power P of the laser is controlled to be 300-350W, the spot diameter d is controlled to be 0.3-0.5-mm, the scanning speed v is less than 1100 mm/min.
8. The method of manufacturing a laser scanning assisted laminated foil according to claim 7, wherein in step S33, the concentration of the sodium hydroxide solution is controlled to be 0.05 to 0.2 wt%.
9. The method of manufacturing a laser scanning assisted laminated foil according to claim 8, wherein in step S33, the ultrasonic frequency is controlled to be 200 to 300KHZ for a duration of 0.5 to 2 minutes.
10. The method of manufacturing a laser scanning assisted laminated foil according to claim 9, wherein in step S35, the aluminum foil substrate is placed in an environment of 100 to 150 ℃ and left for 30 to 40 minutes.
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| CN110257679A (en) * | 2019-07-31 | 2019-09-20 | 安徽工业大学 | A kind of preparation method of molybdenum-base alloy coating |
| CN111804920A (en) * | 2020-07-01 | 2020-10-23 | 益阳艾华富贤电子有限公司 | Preparation method of anode foil of aluminum electrolytic capacitor based on laser sintering |
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| CN110257679A (en) * | 2019-07-31 | 2019-09-20 | 安徽工业大学 | A kind of preparation method of molybdenum-base alloy coating |
| CN111804920A (en) * | 2020-07-01 | 2020-10-23 | 益阳艾华富贤电子有限公司 | Preparation method of anode foil of aluminum electrolytic capacitor based on laser sintering |
| CN112024892A (en) * | 2020-08-27 | 2020-12-04 | 中南大学 | Method for manufacturing aluminum electrolytic capacitor anode foil by electric field auxiliary sintering |
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