CN110340174B - Production method of tantalum-aluminum composite plate strip for capacitor - Google Patents
Production method of tantalum-aluminum composite plate strip for capacitor Download PDFInfo
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- CN110340174B CN110340174B CN201910627691.0A CN201910627691A CN110340174B CN 110340174 B CN110340174 B CN 110340174B CN 201910627691 A CN201910627691 A CN 201910627691A CN 110340174 B CN110340174 B CN 110340174B
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- 239000002131 composite material Substances 0.000 title claims abstract description 107
- RVSGESPTHDDNTH-UHFFFAOYSA-N alumane;tantalum Chemical compound [AlH3].[Ta] RVSGESPTHDDNTH-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000003990 capacitor Substances 0.000 title claims abstract description 62
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 89
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 89
- 238000000034 method Methods 0.000 claims abstract description 61
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052709 silver Inorganic materials 0.000 claims abstract description 56
- 239000004332 silver Substances 0.000 claims abstract description 56
- 230000008569 process Effects 0.000 claims abstract description 44
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 30
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000013329 compounding Methods 0.000 claims abstract description 22
- 238000005098 hot rolling Methods 0.000 claims abstract description 21
- 238000009713 electroplating Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000007747 plating Methods 0.000 claims description 29
- 238000005097 cold rolling Methods 0.000 claims description 28
- 238000005406 washing Methods 0.000 claims description 25
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 24
- 238000000137 annealing Methods 0.000 claims description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- 230000009467 reduction Effects 0.000 claims description 17
- 230000004913 activation Effects 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 15
- 239000002585 base Substances 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 10
- 238000005096 rolling process Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 238000005282 brightening Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000011247 coating layer Substances 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 3
- 229910000765 intermetallic Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical class NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical class NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical class NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Chemical class CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical class [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Chemical class CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/02—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of sheets
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
- C25D5/028—Electroplating of selected surface areas one side electroplating, e.g. substrate conveyed in a bath with inhibited background plating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
- B21B2003/001—Aluminium or its alloys
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- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Power Engineering (AREA)
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- Electroplating Methods And Accessories (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention discloses a production method of a tantalum-aluminum composite plate strip for a capacitor, which comprises the following steps of pretreating the tantalum plate strip, and electroplating silver on the surface of the tantalum plate strip to obtain a tantalum plate strip blank with a silver coating; step two, carrying out hot rolling compounding on the tantalum plate strip blank on the silver-plated side and an aluminum plate base material to obtain a tantalum-aluminum composite plate strip; and step three, obtaining the tantalum-aluminum composite plate strip for the capacitor after the tantalum-aluminum composite plate strip is subjected to a heat treatment process. The invention has the advantages of simple production process, energy saving, environmental protection, high product composite strength, high composite rate and the like.
Description
Technical Field
The invention belongs to the field of tantalum-aluminum composite plates and strips, relates to a production method of a tantalum-aluminum composite plate and strip, and particularly relates to a production method of a tantalum-aluminum composite plate and strip for a capacitor.
Background
The chemical stability of tantalum is good, the corrosion resistance of tantalum capacitor is very strong, and stable electrical property and good physical and chemical properties can be maintained under various environmental conditions. The resistivity of tantalum is high and can reach 7.5 multiplied by 1012Omega cm; the dielectric constant is as large as 27.6, and the leakage current is small. Tantalum has valve metal properties, and a dense oxide film formed on the surface of tantalum has one-way conductivity, and is suitable for manufacturing capacitors. The tantalum capacitor has large capacity and small volume, the capacitance of the tantalum capacitor is 3 times of that of an aluminum capacitor, and the volume of the tantalum capacitor is much smaller than that of the aluminum capacitor. The working temperature range of the tantalum capacitor is-80-200 ℃ can meet different temperature requirements. In addition, the tantalum capacitor has strong stability and heat resistance, becomes a material with high reliability in the electronic industry, and is widely applied to military technology and high-technology fields needing high reliability. Aluminum has good electric conduction and heat conduction performance, tantalum is in shortage compared with aluminum, aluminum resources are rich, aluminum specific weight is small, and price is low. The tantalum and aluminum composite metal plate is a bimetallic plate which takes aluminum as a base body and is compounded with tantalum at the outer layer. The capacitor material is a capacitor material which combines the high-quality conductivity and low-cost resources of aluminum and the high chemical stability and lower contact resistance of tantalum into a whole. The aluminum and tantalum composite metal plate strip integrates the advantages of tantalum and aluminum, replaces the tantalum plate strip with the tantalum and aluminum composite metal plate strip, is widely applied to the fields of computers, mobile phone communication, aerospace, national defense and military industry, instruments and meters, household appliances and the like, and is a development direction and a research focus of the current new metal materials.
At present, the production of tantalum and aluminum composite metal plate strips mainly adopts a solid-solid composite method, a solid-liquid composite method and a liquid-liquid composite method. The diffusion welding method has the advantages of small pressure, no macroscopic plastic deformation, low bonding strength and suitability for precision parts which are not machined after welding. The explosion cladding method has the disadvantages of high noise, high potential safety hazard, low production efficiency and difficult accurate control. The cast-rolling composite method has high temperature, is easy to oxidize, has different melting points of the bimetal and is easy to generate melting loss. The extrusion drawing method has poor continuity and is only suitable for metal composite pipes, bars and wires.
Disclosure of Invention
The invention provides a production method of a tantalum-aluminum composite plate strip for a capacitor, which aims to overcome the defects of the prior art.
In order to achieve the purpose, the invention provides a production method of a tantalum-aluminum composite plate strip for a capacitor, which comprises the following steps of firstly, pretreating the tantalum plate strip, and then electroplating silver on the surface of the tantalum plate strip to obtain a tantalum plate strip blank with a silver coating; step two, carrying out hot rolling compounding on the tantalum plate strip blank on the silver-plated side and an aluminum plate base material to obtain a tantalum-aluminum composite plate strip; and step three, obtaining the tantalum-aluminum composite plate strip for the capacitor after the tantalum-aluminum composite plate strip is subjected to a heat treatment process, namely the tantalum-aluminum composite plate strip for manufacturing the capacitor can be used.
And in the second step, silver is plated on only one side of the tantalum plate strip, and the side is hot-rolled and compounded with the aluminum plate base material. The aluminum plate base material is a 1-6 series alloy.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: in the first step, the silver electroplating process comprises the following steps: and immersing the pretreated tantalum plate strip into silver plating solution for electroplating, wherein the silver plating solution is solution comprising silver nitrate and potassium cyanide.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: wherein, in the first step, in the silver electroplating process, the voltage is 380V, the current is 500-1000A, and the current density is 0.2A/dm2～5A/dm2The temperature of silver plating is 280-300 ℃.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: in the first step, in the silver electroplating process, the concentration of silver nitrate is 35-55 g/L, and the concentration of potassium cyanide is 55-75 g/L in the silver plating solution.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: in the first step, in the silver electroplating process, the silver plating solution also comprises a brightener, and the concentration of the brightener is 35-40 g/L.
The brightener can enable the silver coating to be easily polished, and has good heat conduction, electric conduction and welding performance. The brightening agent can be carbon disulfide, after the carbon disulfide is added into the silver plating solution, the carbon disulfide reacts with CN in the original silver plating solution to generate certain compounds in substituted urea, thiourea, guanidine, sulfide, cyanamide and other sulfides, and the compounds can have the function of the brightening agent. Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: in the second step, in the hot rolling compounding process, the hot rolling compounding temperature is 250-450 ℃, the rolling speed is 5-10 m/min, and the first pass processing rate of the hot rolling compounding is 25-50%.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: wherein, in the third step, the heat treatment process is an annealing process and a cold rolling process in sequence.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: in the third step, in the annealing process, the temperature of the annealing treatment is 350-450 ℃, and the time of the annealing treatment is 8-15 h.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: in the third step, in the cold rolling process, the cold rolling temperature is 150-250 ℃, the cold rolling speed is 100m/min, and the first time reduction rate of the cold rolling is 20-35%.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: in the first step, the thickness of the tantalum plate strip is 0.3-0.6 mm, and the thickness of the silver coating layer on one side of the tantalum plate strip is 2-6 microns; in the second step, the thickness of the aluminum plate base material is 8-12 mm; and in the third step, the thickness of the obtained tantalum-aluminum composite plate strip for the capacitor is 2.0 mm.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: in the first step, the pretreatment comprises acid-base cleaning, electrolytic activation and hydrogen heating reduction treatment to degrease and deoxidize.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: in the first step, the specific process of pretreatment is as follows: the method comprises the steps of firstly carrying out alkali washing on a tantalum plate strip, then carrying out acid washing, loading voltage while carrying out acid washing by taking the tantalum plate strip as an anode and a tank body of an electrolytic tank as a cathode, carrying out electrolytic activation on the tantalum plate strip, and finally carrying out hydrogen heating reduction treatment.
And when the tantalum plate belt continuously passes through the electrolyte, partial surface tantalum enters the solution through ions, so that the aged tantalum surface metal layer can be further removed.
The hydrogen heating reduction treatment is to respectively control nitrogen and hydrogen by two sets of current/voltage stabilizing devices, purge the tantalum plate band after electrolytic activation by nitrogen, then heat up, then introduce hydrogen, stop heating after reduction, continue introducing the mixed gas of nitrogen and hydrogen until the tantalum plate band is cooled to room temperature, and obtain the tantalum plate band after pretreatment.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: wherein, in the alkali washing treatment, a NaOH solution with the mass concentration of 15% is adopted; in the acid washing treatment, 25 percent of H by mass is adopted2SO4And (3) solution.
Further, the invention provides a production method of the tantalum-aluminum composite plate strip for the capacitor, which can also have the following characteristics: wherein, in the electrolytic activation, the applied voltage is 6V.
The invention has the beneficial effects that: compared with the traditional production processes of the tantalum-aluminum composite plate strip, such as a solid-solid composite method, a solid-liquid composite method, a liquid-liquid composite method and the like, the production method of the tantalum-aluminum composite plate strip for the capacitor simplifies the production process. And secondly, compared with other methods, the method has the advantages of high yield, energy conservation, material conservation and consumption reduction, and other methods such as an explosion method are not environment-friendly, so that the whole process of the production process is environment-friendly. In addition, the method is suitable for compounding of aluminum alloys and tantalum plates of various grades, including different series of aluminum alloys and different plate widths, and the obtained tantalum-aluminum composite plate strip for the capacitor is large in variety and specification and wide in application range. In addition, the tantalum-aluminum composite plate strip with the thickness of about 2.0mm can be produced by the method, the tantalum in the tantalum-aluminum composite plate strip can account for 2-3% of the total volume, the composite strength of the tantalum-aluminum composite plate strip for the capacitor is high (not less than 12N/mm), the two composite metal plates of tantalum and aluminum are not easy to peel, the elongation is high (not less than 12%), the composite rate reaches 100%, the tantalum-aluminum composite plate strip for the capacitor is good in electric conduction and heat conduction performance, stable and reliable in quality, capable of being widely applied to the fields of capacitors, mobile phone radiators and the like, and remarkable in economic benefit. The invention has the advantages of simple production process, energy saving, environmental protection, high product composite strength, high composite rate and the like.
Drawings
FIG. 1 is an SEM image of a tantalum-aluminum composite cross-section of a tantalum-aluminum composite strip of example 1;
FIG. 2 is an SEM image of a tantalum-aluminum composite cross-section of a tantalum-aluminum composite strip of example 2;
fig. 3 is an SEM image of a tantalum-aluminum composite cross-section of a tantalum-aluminum composite strip of example 3.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The embodiment provides a production method of a tantalum-aluminum composite plate strip for a capacitor, which comprises the following steps:
step one, after the tantalum plate strip is pretreated, the surface of the tantalum plate strip is electroplated with silver, and a tantalum plate strip blank with a silver coating is obtained. Wherein the pretreatment comprises acid-base cleaning, electrolytic activation and hydrogen heating reduction treatment.
The specific process is as follows: firstly, carrying out alkali washing on a tantalum plate belt with the thickness of 0.3mm, then carrying out acid washing, loading voltage while carrying out acid washing by taking the tantalum plate belt as an anode and a tank body of an electrolytic tank as a cathode, carrying out electrolytic activation on the tantalum plate belt, and finally carrying out hydrogen heating reduction treatment. Then, the tantalum plate strip after pretreatment was immersed in a silver plating solution for electroplating to obtain a tantalum plate strip blank having a silver plating layer of 0.003mm thickness. The silver plating solution is a solution of silver nitrate, potassium cyanide and brightener.
Wherein, in the alkali washing treatment, a NaOH solution with the mass concentration of 15% is adopted. In the acid washing treatment, 25 percent of H by mass is adopted2SO4And (3) solution. In the electrolytic activation, the applied voltage was 6V.
In the silver plating solution, the concentration of silver nitrate is 35g/L, the concentration of potassium cyanide is 55g/L, and the concentration of brightener is 35 g/L. In the silver electroplating process, the voltage is 380V, the current is 500A, and the current density is 0.2A/dm2The temperature of silver plating was 280 ℃.
And step two, performing hot rolling compounding on the tantalum plate strip blank on the silver plating side and an aluminum plate base material with the thickness of 8 mm. In the hot rolling compounding process, the hot rolling compounding temperature is 250 ℃, the rolling speed is 6m/min, and the first pass processing rate of the hot rolling compounding is 25%. Obtaining the tantalum-aluminum composite plate strip with the total thickness of 6.225 mm.
Scanning electron microscope characterization is carried out on the tantalum-aluminum composite plate strip, and an SEM image of the tantalum-aluminum composite plate strip is shown in figure 1. In FIG. 1, tantalum is shown on the left, aluminum on the right, and an intermetallic compound is shown in the middle. As can be seen from the figure, good metallurgical recombination is realized between the tantalum layer and the aluminum layer of the tantalum-aluminum composite plate. The composite strength of the tantalum-aluminum is 65 MPa.
And step three, sequentially carrying out annealing and cold rolling process treatment on the tantalum-aluminum composite plate strip obtained in the step two. Wherein, in the annealing process, the temperature of the annealing treatment is 350 ℃, and the time of the annealing treatment is 15 h. In the cold rolling process, the cold rolling temperature is 150 ℃, the cold rolling speed is 100m/min, and the first time reduction rate of the cold rolling is 20 percent.
And (3) annealing and cold rolling to obtain the tantalum-aluminum composite plate strip with the thickness of 2.0mm for the capacitor. The tantalum in the tantalum-aluminum composite plate strip for the capacitor can account for 2% of the total volume. The elongation of the tantalum-aluminum composite plate strip for the capacitor is 12 percent, the composite strength is 12N/mm, and the conductivity is 4.5 multiplied by 107S/m, tensile strength 235 MPa.
Example 2
The embodiment provides a production method of a tantalum-aluminum composite plate strip for a capacitor, which comprises the following steps:
step one, after the tantalum plate strip is pretreated, the surface of the tantalum plate strip is electroplated with silver, and a tantalum plate strip blank with a silver coating is obtained. Wherein the pretreatment comprises acid-base cleaning, electrolytic activation and hydrogen heating reduction treatment.
The specific process is as follows: firstly, carrying out alkali washing on a tantalum plate belt with the thickness of 0.5mm, then carrying out acid washing, loading voltage while carrying out acid washing by taking the tantalum plate belt as an anode and a tank body of an electrolytic tank as a cathode, carrying out electrolytic activation on the tantalum plate belt, and finally carrying out hydrogen heating reduction treatment. Then, the tantalum plate strip after pretreatment was immersed in a silver plating solution for electroplating to obtain a tantalum plate strip blank having a silver plating layer of 0.004mm thickness. The silver plating solution is a solution of silver nitrate, potassium cyanide and brightener.
Wherein, in the alkali washing treatment, a NaOH solution with the mass concentration of 15% is adopted. In the acid washing treatment, 25 percent of H by mass is adopted2SO4And (3) solution. In electrolytic activation, electricity is appliedThe pressure was 6V.
In the solution of silver nitrate and potassium cyanide, the concentration of silver nitrate is 45g/L, the concentration of potassium cyanide is 65g/L, and the concentration of brightener is 38 g/L. In the silver electroplating process, the voltage is 380V, the current is 800A, and the current density is 3A/dm2The temperature of silver plating was 290 ℃.
And step two, carrying out hot rolling compounding on the tantalum plate strip blank on the silver plating side and an aluminum plate base material with the thickness of 10 mm. In the hot rolling compounding process, the hot rolling compounding temperature is 350 ℃, the rolling speed is 8m/min, and the first pass processing rate of the hot rolling compounding is 30%. And obtaining the tantalum-aluminum composite plate strip with the total thickness of 7.35 mm.
Scanning electron microscope characterization is carried out on the tantalum-aluminum composite plate strip, and an SEM image of the tantalum-aluminum composite plate strip is shown in FIG. 2. In FIG. 2, tantalum is shown on the left, aluminum on the right, and an intermetallic compound is shown in the middle. As can be seen from the figure, good metallurgical recombination is realized between the tantalum layer and the aluminum layer of the tantalum-aluminum composite plate. The composite strength of the tantalum-aluminum is 60 MPa.
And step three, sequentially carrying out annealing and cold rolling process treatment on the tantalum-aluminum composite plate strip obtained in the step two. Wherein, in the annealing process, the temperature of the annealing treatment is 400 ℃, and the time of the annealing treatment is 12 h. In the cold rolling process, the cold rolling temperature is 200 ℃, the cold rolling speed is 100m/min, and the first time reduction rate of the cold rolling is 30 percent.
And (3) annealing and cold rolling to obtain the tantalum-aluminum composite plate strip with the thickness of 2.0mm for the capacitor. The tantalum in the tantalum-aluminum composite plate strip for the capacitor can account for 2.5 percent of the total volume. The elongation of the tantalum-aluminum composite plate strip for the capacitor is 13 percent, the composite strength is 13N/mm, and the conductivity is 4.8 multiplied by 107S/m, tensile strength 242 MPa.
Example 3
The embodiment provides a production method of a tantalum-aluminum composite plate strip for a capacitor, which comprises the following steps:
step one, after the tantalum plate strip is pretreated, the surface of the tantalum plate strip is electroplated with silver, and a tantalum plate strip blank with a silver coating is obtained. Wherein the pretreatment comprises acid-base cleaning, electrolytic activation and hydrogen heating reduction treatment.
The specific process is as follows: firstly, carrying out alkali washing on a tantalum plate belt with the thickness of 0.6mm, then carrying out acid washing, loading voltage while carrying out acid washing by taking the tantalum plate belt as an anode and a tank body of an electrolytic tank as a cathode, carrying out electrolytic activation on the tantalum plate belt, and finally carrying out hydrogen heating reduction treatment. Then, the tantalum plate strip after pretreatment was immersed in a silver plating solution for electroplating to obtain a tantalum plate strip blank having a silver plating layer of 0.005mm thickness. The silver plating solution is a solution of silver nitrate, potassium cyanide and brightener.
Wherein, in the alkali washing treatment, a NaOH solution with the mass concentration of 15% is adopted. In the acid washing treatment, 25 percent of H by mass is adopted2SO4And (3) solution. In the electrolytic activation, the applied voltage was 6V.
In the solution of silver nitrate and potassium cyanide, the concentration of silver nitrate is 55g/L, the concentration of potassium cyanide is 75g/L, and the concentration of brightener is 40 g/L. In the silver electroplating process, the voltage is 380V, the current is 1000A, and the current density is 5A/dm2The temperature of silver plating was 300 ℃.
And step two, carrying out hot rolling compounding on the tantalum plate strip blank on the silver plating side and an aluminum plate base material with the thickness of 12 mm. In the hot rolling compounding process, the hot rolling compounding temperature is 450 ℃, the rolling speed is 10m/min, and the first pass processing rate of the hot rolling compounding is 50%. And obtaining the tantalum-aluminum composite plate strip with the total thickness of 6.3 mm.
Scanning electron microscope characterization is carried out on the tantalum-aluminum composite plate strip, and an SEM image of the tantalum-aluminum composite plate strip is shown in FIG. 3. In fig. 3, tantalum is shown on the left, aluminum on the right, and an intermetallic compound is shown in the middle. As can be seen from the figure, good metallurgical recombination is realized between the tantalum layer and the aluminum layer of the tantalum-aluminum composite plate. The composite strength of the tantalum-aluminum is 70 MPa.
And step three, sequentially carrying out annealing and cold rolling process treatment on the tantalum-aluminum composite plate strip obtained in the step two. Wherein, in the annealing process, the temperature of the annealing treatment is 450 ℃, and the time of the annealing treatment is 8 h. In the cold rolling process, the cold rolling temperature is 250 ℃, the cold rolling speed is 100m/min, and the first time reduction rate of the cold rolling is 20 percent.
And (3) annealing and cold rolling to obtain the tantalum-aluminum composite plate strip with the thickness of 2.0mm for the capacitor. The tantalum in the tantalum-aluminum composite plate strip for the capacitor can account for 3% of the total volume. The elongation of the tantalum-aluminum composite plate strip for the capacitor is 13%, the composite strength is 14N/mm, and the tantalum-aluminum composite plate strip is conductiveThe ratio was 4.9X 107S/m, tensile strength 245 MPa.
Claims (9)
1. A production method of a tantalum-aluminum composite plate strip for a capacitor is characterized by comprising the following steps:
after the tantalum plate belt is pretreated, electroplating silver on one side surface of the tantalum plate belt to obtain a tantalum plate belt blank with a silver coating;
the specific process of the pretreatment is as follows: firstly carrying out alkali washing on the tantalum plate strip, then carrying out acid washing, loading voltage while carrying out acid washing by taking the tantalum plate strip as an anode and taking a tank body of an electrolytic tank as a cathode, carrying out electrolytic activation on the tantalum plate strip, and finally carrying out hydrogen heating reduction treatment
Step two, carrying out hot rolling compounding on the tantalum plate strip blank on the silver-plated side and an aluminum plate base material to obtain a tantalum-aluminum composite plate strip;
in the hot rolling compounding process, the temperature of hot rolling compounding is 250-450 ℃, the rolling speed is 5-10 m/min, and the first pass processing rate of hot rolling compounding is 25-50%;
thirdly, obtaining the tantalum-aluminum composite plate strip for the capacitor after the tantalum-aluminum composite plate strip is subjected to a heat treatment process;
the heat treatment process sequentially comprises an annealing process and a cold rolling process;
in the annealing process, the temperature of the annealing treatment is 350-450 ℃, and the time of the annealing treatment is 8-15 h;
in the cold rolling process, the cold rolling temperature is 150-250 ℃, the cold rolling speed is 100m/min, and the first time working rate of the cold rolling is 20-35%.
2. The method for producing the tantalum-aluminum composite plate strip for the capacitor as claimed in claim 1, wherein:
in the first step, the silver electroplating process comprises the following steps: and immersing the pretreated tantalum plate strip into silver plating solution for electroplating, wherein the silver plating solution is a solution comprising silver nitrate and potassium cyanide.
3. The production method of the tantalum-aluminum composite plate strip for the capacitor as claimed in claim 1 or 2, wherein:
wherein, in the first step, in the silver electroplating process, the voltage is 380V, the current is 500-1000A, and the current density is 0.2A/dm2～5A/dm2The temperature of silver plating is 280-300 ℃.
4. The production method of the tantalum-aluminum composite plate strip for the capacitor as claimed in claim 1 or 2, wherein:
in the first step, in the silver electroplating process, the concentration of silver nitrate in the silver plating solution is 35-55 g/L, and the concentration of potassium cyanide in the silver plating solution is 55-75 g/L.
5. The production method of the tantalum-aluminum composite plate strip for the capacitor as claimed in claim 1 or 2, wherein:
in the first step, in the silver electroplating process, the silver plating solution further comprises a brightening agent, and the concentration of the brightening agent is 35-40 g/L.
6. The method for producing the tantalum-aluminum composite plate strip for the capacitor as claimed in claim 1, wherein:
in the first step, the thickness of the tantalum plate strip is 0.3-0.6 mm, and the thickness of the silver coating layer on one side of the tantalum plate strip is 2-6 microns;
in the second step, the thickness of the aluminum plate base material is 8-12 mm;
in the third step, the thickness of the obtained tantalum-aluminum composite plate strip for the capacitor is 2.0 mm.
7. The method for producing the tantalum-aluminum composite plate strip for the capacitor as claimed in claim 1, wherein:
in the first step, the pretreatment comprises acid-base cleaning, electrolytic activation and hydrogen heating reduction treatment.
8. The method for producing the tantalum-aluminum composite plate strip for the capacitor as claimed in claim 1, wherein:
wherein, in the alkali washing treatment, a NaOH solution with the mass concentration of 15% is adopted;
in the acid washing treatment, 25 percent of H by mass is adopted2SO4And (3) solution.
9. The method for producing the tantalum-aluminum composite plate strip for the capacitor as claimed in claim 1, wherein:
wherein, in the electrolytic activation, the loading voltage is 6V.
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