CN114231789B - Processing technology of copper strip for LED - Google Patents

Processing technology of copper strip for LED Download PDF

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Publication number
CN114231789B
CN114231789B CN202111562095.2A CN202111562095A CN114231789B CN 114231789 B CN114231789 B CN 114231789B CN 202111562095 A CN202111562095 A CN 202111562095A CN 114231789 B CN114231789 B CN 114231789B
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copper strip
copper
rolling
raw material
carrying
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CN114231789A (en
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谭智泉
陈积为
刘军德
易外庚
罗智涛
何长勇
岳俊江
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Qingyuan Chujiang High Precision Copper Strip Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • C22C9/04Alloys based on copper with zinc as the next major constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23PMETAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The invention discloses a processing technology of a copper strip for an LED, which comprises the following steps of: the method comprises the steps of preparing a raw material A (copper is 98-99.9%, iron is 0.001-0.03%, lead is 0.001-0.03%, and the balance is zinc) and a raw material B (copper is 80-90%, iron is 0.001-0.03%, lead is 0.001-0.03%, mixed rare earth metal is 0.001-0.03%, and the balance is zinc), and processing the raw material A and the raw material B through smelting, surface milling, rough rolling, edge cutting, annealing, surface grinding, finish rolling, passivation and slitting to obtain the copper strip for the LED.

Description

Processing technology of copper strip for LED
Technical Field
The invention relates to the field of processing technologies of copper strips for LEDs, in particular to a processing technology of a copper strip for LEDs.
Background
An LED is a commonly used light emitting device, which emits light by energy released by recombination of electrons and holes, and has a wide application in the field of illumination, and a light emitting diode can efficiently convert electric energy into light energy, and has a wide application in modern society, such as illumination, flat panel display, medical devices, and the like, and such an electronic component appears as early as 1962, and can only emit red light with low luminosity at the early stage, and then other versions of monochromatic light are developed, and the light emitted so far has been spread over visible light, infrared light and ultraviolet light, and the luminosity is also improved to a considerable luminosity. The led is also used as an indicator light, a display panel, etc. in the first place, and with the continuous progress of the technology, the led has been widely used for displays and lighting.
In the prior art, the copper strip for the LED is generally made of copper as a main material and zinc as an auxiliary material, and because the outdoor LED belongs to the conditions of long-term illumination and outdoor environment in the using process, the copper strip for the LED is easy to have a relatively fast oxidation reaction, so that the strength and the oxidation resistance of the copper strip for the LED can be rapidly reduced, the LED is easy to have potential safety hazards such as poor contact, the practicability of the copper strip for the LED is reduced, and therefore, the processing technology of the copper strip for the LED is needed.
Disclosure of Invention
The invention aims to provide a processing technology of a copper strip for an LED (light emitting diode), which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a processing technology of a copper strip for an LED comprises the following steps:
firstly, preparing a raw material A (98-99.9 percent of copper, 0.001-0.03 percent of iron, 0.001-0.03 percent of lead and the balance of zinc) and a raw material B (80-90 percent of copper, 0.001-0.03 percent of iron, 0.001-0.03 percent of lead, 0.001-0.03 percent of mixed rare earth metal and the balance of zinc);
step two, smelting: putting a raw material A into a smelting furnace for smelting, then adding a raw material B according to the weight ratio of A: B of 1 to 6 for smelting, smelting at the temperature of 1100-1200 ℃ for 2-3 hours, removing slag after the raw materials A and B are fully dissolved, then pouring and leading out in a gravity pouring mode, circularly cooling a poured product in a water cooling circulation mode in the leading-out process, and forming a cast blank copper coil with the thickness of 10mm after cooling is finished;
step three, milling the surface: selecting a vibration grinding machine and high-frequency porcelain to treat the surface of the cast blank copper coil, and adding polishing solution, wherein the cast blank copper coil ratio to the polishing solution is 100: polishing for 40 minutes, flushing water for cleaning, ensuring surface finish, ensuring uniform tolerance of the cast blank copper coil, and performing surface milling and deslagging treatment on the cast blank copper coil by using a numerical control milling machine to obtain a copper coil with the thickness of 4.5 mm;
step four, rough rolling: heating the cast blank copper coil at the high temperature of 1000 ℃, then carrying out rough rolling, and rolling into a copper strip with the thickness of about 2.3cm to generate the copper strip meeting the tolerance requirement of the next procedure;
step five, cutting edges: cutting edges of the roughly rolled copper strip, trimming edges of the copper strip which are cracked in the rolling process, and then rolling;
step six, annealing: annealing the rough rolled casting blank copper coil, keeping the temperature in a push rod furnace at 700 ℃ for 6h for annealing, and cooling by circulating water;
step seven, grinding the flour: cleaning the surface of the annealed copper strip, and carrying out acid washing on the copper strip by using dilute sulfuric acid in a water washing area at the speed of 70m/min, wherein the acid concentration is 3-5 ℃, red spots generated on the surface of the copper strip can be washed away by acid liquor in a water washing pool, and dark red spots are brushed away by iron fine hair during water washing;
step eight, finish rolling: carrying out five-pass finish rolling on a 2.3mm copper strip to obtain a finished copper strip with the thickness of 0.3mm, rolling the 2.3mm copper strip to 1.3mm in the first pass, rolling the 1.3mm copper strip to 1mm in the second pass, carrying out heat preservation for 6h annealing in a push rod furnace at the temperature of 700 ℃, cooling with circulating water, carrying out acid pickling on the copper strip at the speed of 70m/min by using dilute sulfuric acid, rolling the 1mm copper strip to 0.5mm in the third and fourth passes, carrying out heat preservation for 5.5h annealing in a hood-type furnace at the temperature of 460 ℃, cooling to 85 ℃, discharging, carrying out acid pickling on the copper strip at the speed of 70m/min by using dilute sulfuric acid, rolling the 0.5mm copper strip to a finished product with the thickness of 0.3mm in the fifth pass, and carrying out acid pickling on the copper strip at the speed of 65m/min by using dilute sulfuric acid;
step nine, passivation: heating a copper strip to about 35 ℃ by using a hydrogen peroxide type polishing agent MS0308-1 and water distribution of 1-3, soaking for 1-3 minutes to form a uniform tan oxidation film on the surface of the copper strip, washing the polishing solution remained on the surface of the copper strip completely to prevent the liquid medicine from polluting the next procedure, using 5-8% of dilute sulfuric acid stripping solution, putting the polished copper strip into the soaking solution for a few seconds, completely removing the tan oxidation film to achieve a light-emitting effect, washing the stripping solution remained on the surface of the copper strip completely, using 0.2-0.3% of sodium carbonate solution as a neutralizing solution, neutralizing at normal temperature for 1-3 minutes, washing the neutralizing solution remained on the surface of the copper strip completely, placing the polished copper strip into a passivation solution MS0407, soaking at normal temperature for 5 minutes, and washing the neutralizing solution remained on the surface of the copper strip by flowing tap water of a user to be dry;
step ten, slitting: and cutting and winding the finished copper strip according to the specified size.
Preferably, the mixed rare earth metal is a metal prepared by extracting an oxide or chloride mixed with lanthanum, cerium, praseodymium and neodymium and a small amount of samarium, europium and gadolinium from rare earth ore through molten salt electrolysis, wherein the total amount of rare earth is more than 98 percent, and the cerium is more than 48 percent.
Preferably, the annealing treatment is carried out using a combustion ammonia gas containing 2% of H2 and an incomplete combustion furnace gas containing 2 to 5% of H2 and CO, and in the case of using steam, the accumulated water in the steam line must be vented for the main energy, and in order to prevent the generation of water flow on the alloy surface during cooling, the incomplete combustion furnace gas is used for protection during cooling, and in the case of decomposing ammonia gas, combustion is used to reduce the hydrogen content, and water vapor is completely removed, and in the case of using ammonia gas, oxygen must be removed to prevent explosion, and vacuum and the introduction of nitrogen or argon may be used in combination.
Preferably, 0.2-0.3% sodium carbonate solution is used as the neutralizing solution in the ninth step, and the neutralizing solution is neutralized for 1-3 minutes at normal temperature, so that the process prevents acidic membrane stripping solution from entering into weak alkaline passivation solution to cause the passivation solution to lose passivation performance.
Preferably, the copper strip is turned over during polishing in the ninth step so that the copper strip is fully contacted with the liquid medicine, and a uniform tan oxide film is formed on the surface of the copper strip.
Preferably, in the ninth step, the multiple treatments are all cleaned by flowing water and then dried, so that the influence on the subsequent flow is avoided.
The invention has the technical effects and advantages that:
(1) The invention relates to a processing technology of a copper strip for an LED (light-emitting diode), which adds a certain amount of mixed rare earth metal on the basis of the traditional production of the copper strip, and the diffusion process of copper ions passing through an oxide layer is seriously inhibited due to the addition of the mixed rare earth metal, so that the oxidation speed of a rare earth copper alloy is lower than that of pure copper by multiple times, the oxidation resistance of the copper strip applied to the LED is stronger, the oxidation corrosion efficiency of the LED is reduced, the contact efficiency of the LED is increased, and the service life of the LED is prolonged.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a processing technology of a copper strip for an LED, which comprises the following steps:
firstly, preparing a raw material A (98-99.9 percent of copper, 0.001-0.03 percent of iron, 0.001-0.03 percent of lead and the balance of zinc) and a raw material B (80-90 percent of copper, 0.001-0.03 percent of iron, 0.001-0.03 percent of lead, 0.001-0.03 percent of mixed rare earth metal and the balance of zinc);
step two, smelting: putting a raw material A into a smelting furnace for smelting, then adding a raw material B according to the weight ratio of A: B of 1 to 6 for smelting, smelting at the temperature of 1100-1200 ℃ for 2-3 hours, removing slag after the raw materials A and B are fully dissolved, then pouring and leading out in a gravity pouring mode, circularly cooling a poured product in a water cooling circulation mode in the leading-out process, and forming a cast blank copper coil with the thickness of 10mm after cooling is finished;
step three, milling the surface: selecting a vibration grinding machine and high-frequency porcelain to treat the surface of the cast blank copper coil, and adding polishing solution, wherein the cast blank copper coil ratio to the polishing solution is 100: polishing for 40 minutes, flushing water for cleaning, ensuring surface finish, ensuring uniform tolerance of the cast blank copper coil, and performing surface milling and deslagging treatment on the cast blank copper coil by using a numerical control milling machine to obtain a copper coil with the thickness of 4.5 mm;
step four, rough rolling: heating the cast blank copper coil at the high temperature of 1000 ℃, then carrying out rough rolling, and rolling into a copper strip with the thickness of about 2.3cm to generate the copper strip meeting the tolerance requirement of the next procedure;
step five, cutting edges: cutting edges of the roughly rolled copper strip, trimming the edge cracking caused in the rolling process, and then rolling;
step six, annealing: annealing the rough rolled casting blank copper coil, keeping the temperature in a push rod furnace at 700 ℃ for 6h for annealing, and cooling by circulating water;
step seven, grinding the flour: cleaning the surface of the annealed copper strip, and carrying out acid washing on the copper strip by using dilute sulfuric acid in a water washing area at the speed of 70m/min, wherein the acid concentration is 3-5 ℃, red spots generated on the surface of the copper strip can be washed away by acid liquor in a water washing pool, and dark red spots are brushed away by iron fine hair during water washing;
step eight, finish rolling: carrying out five-pass finish rolling on a 2.3mm copper strip to obtain a finished copper strip with the thickness of 0.3mm, rolling the 2.3mm copper strip to 1.3mm in the first pass, rolling the 1.3mm copper strip to 1mm in the second pass, carrying out heat preservation for 6h annealing in a push rod furnace at the temperature of 700 ℃, cooling with circulating water, carrying out acid pickling on the copper strip at the speed of 70m/min by using dilute sulfuric acid, rolling the 1mm copper strip to 0.5mm in the third and fourth passes, carrying out heat preservation for 5.5h annealing in a hood-type furnace at the temperature of 460 ℃, cooling to 85 ℃, discharging, carrying out acid pickling on the copper strip at the speed of 70m/min by using dilute sulfuric acid, rolling the 0.5mm copper strip to a finished product with the thickness of 0.3mm in the fifth pass, and carrying out acid pickling on the copper strip at the speed of 65m/min by using dilute sulfuric acid;
step nine, passivation: the method comprises the following steps of (1) heating a copper strip to about 35 ℃ by using a hydrogen peroxide type polishing agent MS0308-1 and water distribution of 1;
step ten, slitting: and cutting and winding the finished copper strip according to the specified size.
The mixed rare earth metal is a metal which is prepared by extracting mixed oxides or chlorides of lanthanum, cerium, praseodymium and neodymium and a small amount of samarium, europium and gadolinium from rare earth ore and electrolyzing the mixed oxides or chlorides by molten salt, wherein the total amount of the rare earth is more than 98 percent, and the cerium is more than 48 percent.
The annealing treatment is carried out by using 2% H2-containing combustion ammonia gas and 2-5% H2-and CO-containing incomplete combustion furnace gas for protection, wherein when steam is used, accumulated water in a steam pipeline must be discharged out of main energy for ventilation, in order to prevent water flow on the surface of the alloy during cooling, the incomplete combustion furnace gas is used for protection during cooling, when ammonia gas is used for decomposition, the hydrogen content is reduced by combustion, the water vapor in the ammonia gas is completely removed, and when the ammonia gas is used, oxygen must be removed to prevent explosion, and vacuum and nitrogen or argon introduction can be adopted for matching.
And step nine, 0.2-0.3% sodium carbonate solution is used as a neutralization solution, and the neutralization solution is neutralized for 1-3 minutes at normal temperature, wherein the process is to prevent acidic membrane stripping solution from entering into weak alkaline passivation solution to cause the passivation solution to lose passivation performance.
And in the step nine, turning over the copper strip during polishing to ensure that the copper strip is fully contacted with the liquid medicine, so that a uniform tan oxide film is formed on the surface of the copper strip.
And in the ninth step, the multiple treatments are all cleaned by flowing water and then dried, so that the subsequent processes are prevented from being influenced.
In the first embodiment, the formula proportion 1 of the preparation raw material A used in the preparation process is as follows:
Figure BDA0003420937200000071
the formula proportion 1 of the preparation raw material B used in the preparation process is as follows:
Figure BDA0003420937200000072
in the second embodiment, the formula ratio 2 of the preparation raw material A used in the preparation process is as follows:
Figure BDA0003420937200000073
the formula proportion 2 of the preparation raw material B used in the preparation process is as follows:
Figure BDA0003420937200000074
in the third embodiment, the formula ratio 3 of the preparation raw material A used in the preparation process is as follows:
Figure BDA0003420937200000075
Figure BDA0003420937200000081
the formula proportion 3 of the preparation raw material B used in the preparation process is as follows:
Figure BDA0003420937200000082
in summary, according to the processing technology of the copper strip for the LED provided by the invention, the preparation raw material a and the preparation raw material B are selected as the preparation raw materials of the copper strip, 98% -99.9% of copper, 0.001% -0.03% of iron, 0.001% -0.03% of lead and the balance of zinc are selected as the preparation raw material a, 80% -90% of copper, 0.001% -0.03% of iron, 0.001% -0.03% of lead, 0.001% -0.03% of mixed rare earth metal and the balance of zinc are selected as the preparation raw material B, the structural level of the copper strip can be improved by mixing various raw materials, the mechanical property is enhanced, and quantitative mixed rare earth metal is added, because the diffusion process of copper ions passing through an oxidation layer is seriously inhibited by adding the mixed rare earth metal, the oxidation speed of the rare earth copper alloy is much slower than that of pure copper, so that the copper strip applied to the LED has stronger oxidation resistance, the oxidation corrosion resistance of the LED is reduced, the contact efficiency of the LED is increased, and the service life of the LED is prolonged.
In the description of the present invention, unless otherwise expressly specified or limited, the terms "disposed," "mounted," "connected," and "secured" are to be construed broadly, e.g., as meaning fixedly connected, detachably connected, or integral to; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood in a specific case to those of ordinary skill in the art.
The standard parts used by the invention can be purchased from the market, and the special-shaped parts can be customized according to the description of the specification.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (4)

1. A processing technology of a copper strip for an LED is characterized in that the copper strip is prepared by the following steps:
step one, preparing a raw material A and a raw material B, wherein the raw material A comprises 98-99.9% of copper, 0.001-0.03% of iron, 0.001-0.03% of lead and the balance of zinc; the raw material B comprises 80-90% of copper, 0.001-0.03% of iron, 0.001-0.03% of lead, 0.001-0.03% of mixed rare earth metal and the balance of zinc;
step two, smelting: putting a raw material A into a smelting furnace for smelting, then adding a raw material B according to the weight ratio of A: B being 1;
step three, milling the surface: selecting a vibration grinding machine and high-frequency porcelain to treat the surface of the cast blank copper coil, and adding polishing solution, wherein the ratio of the cast blank copper coil to the polishing solution is 100: polishing for 40 minutes, flushing water for cleaning, ensuring surface finish, ensuring uniform tolerance of the cast blank copper coil, and performing surface milling and deslagging treatment on the cast blank copper coil by using a numerical control milling machine to obtain a copper coil with the thickness of 4.5 mm;
step four, rough rolling: heating a copper coil with the thickness of 4.5mm at the high temperature of 1000 ℃, then carrying out rough rolling, and rolling into a copper strip with the thickness of 2.3mm to generate the copper strip meeting the tolerance requirement of the next procedure;
step five, cutting edges: cutting edges of the roughly rolled copper strip, trimming edge cracking caused in the rolling process and then rolling;
step six, annealing: annealing the copper strip after edge cutting, keeping the temperature in a push rod furnace at 700 ℃ for 6h for annealing, and cooling with circulating water;
step seven, grinding the flour: cleaning the surface of the annealed copper strip, and carrying out acid washing on the copper strip by using dilute sulfuric acid in a water washing area at the speed of 70m/min, wherein the acid concentration is 3-5 ℃, red spots generated on the surface of the copper strip are washed away by acid liquor in a water washing pool, and dark red spots are brushed away by iron fine hair during water washing;
step eight, finish rolling: carrying out five-pass finish rolling on a 2.3mm copper strip to obtain a finished copper strip with the thickness of 0.3mm, rolling 2.3mm to 1.3mm in the first pass, rolling 1.3mm to 1mm in the second pass, carrying out heat preservation in a push rod furnace at the temperature of 700 ℃ for 6h for annealing, cooling with circulating water, carrying out acid washing on the copper strip at the speed of 70m/min by adopting dilute sulfuric acid, rolling 1mm to 0.5mm in the third and fourth passes, carrying out heat preservation in a hood-type furnace at the temperature of 460 ℃ for 5.5h for annealing, cooling to 85 ℃ and discharging, carrying out acid washing on the copper strip at the speed of 70m/min by adopting dilute sulfuric acid, rolling 0.5mm copper strip to a 0.3mm finished product in the first pass in the fifth pass, and carrying out acid washing on the copper strip at the speed of 65m/min by adopting dilute sulfuric acid;
step nine, passivation: the method comprises the following steps of (1) heating a copper strip by using a hydrogen peroxide type polishing agent MS0308-1 and water distribution of 1;
step ten, slitting: cutting and winding the finished copper strip according to a specified size;
the mixed rare earth metal is prepared by performing fused salt electrolysis on an oxide or chloride extracted from rare earth ore, wherein the oxide or chloride contains lanthanum, cerium, praseodymium, neodymium and a small amount of samarium, europium and gadolinium.
2. The processing technology of the copper strip for the LED according to claim 1, wherein in the ninth step, 0.2 to 0.3% of sodium carbonate solution is used as a neutralization solution, and the neutralization solution is neutralized for 1 to 3 minutes at normal temperature, so that the acidic membrane stripping solution is prevented from entering a weakly alkaline passivation solution to cause the passivation solution to lose passivation performance.
3. The processing technology of the copper strip for the LED as claimed in claim 1, wherein the copper strip is turned over during polishing in the ninth step so that the copper strip is fully contacted with the chemical solution, and a uniform tan oxide film is formed on the surface of the copper strip.
4. The processing technology of the copper strip for the LED according to claim 1, wherein flowing water is used for cleaning and drying the copper strip between the multiple treatments in the ninth step, so that the subsequent processes are prevented from being affected.
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