CN116516335B - High-strength lead frame and preparation method thereof - Google Patents
High-strength lead frame and preparation method thereof Download PDFInfo
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- CN116516335B CN116516335B CN202310387552.1A CN202310387552A CN116516335B CN 116516335 B CN116516335 B CN 116516335B CN 202310387552 A CN202310387552 A CN 202310387552A CN 116516335 B CN116516335 B CN 116516335B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 91
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 82
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 82
- 238000005253 cladding Methods 0.000 claims abstract description 56
- 239000002131 composite material Substances 0.000 claims abstract description 56
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052709 silver Inorganic materials 0.000 claims abstract description 32
- 239000004332 silver Substances 0.000 claims abstract description 32
- 238000007747 plating Methods 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000004372 laser cladding Methods 0.000 claims abstract description 21
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- 239000010949 copper Substances 0.000 claims abstract description 20
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 48
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000853 adhesive Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- BXAGUJYMKLFDEM-UHFFFAOYSA-N [N]1C2=CC=C1C=C(N1)C=C(S)C1=CC([N]1)=CC=C1C=C(N1)C=CC1=C2 Chemical compound [N]1C2=CC=C1C=C(N1)C=C(S)C1=CC([N]1)=CC=C1C=C(N1)C=CC1=C2 BXAGUJYMKLFDEM-UHFFFAOYSA-N 0.000 claims description 8
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 238000007743 anodising Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- XPSMITSOZMLACW-UHFFFAOYSA-N 2-(4-aminophenyl)-n-(benzenesulfonyl)acetamide Chemical compound C1=CC(N)=CC=C1CC(=O)NS(=O)(=O)C1=CC=CC=C1 XPSMITSOZMLACW-UHFFFAOYSA-N 0.000 claims 1
- 239000013384 organic framework Substances 0.000 abstract description 13
- 238000011065 in-situ storage Methods 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 abstract description 6
- 238000003466 welding Methods 0.000 abstract description 6
- -1 sulfhydryl porphyrin Chemical class 0.000 abstract description 5
- GDHNMQIBSKTFPO-UHFFFAOYSA-N lanthanum silver Chemical compound [Ag].[La] GDHNMQIBSKTFPO-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003446 ligand Substances 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 238000007789 sealing Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 13
- 229910052799 carbon Inorganic materials 0.000 description 9
- 230000002195 synergetic effect Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- FTCLAXOKVVLHEG-UHFFFAOYSA-N sodium;3-sulfanylpropane-1-sulfonic acid Chemical compound [Na].OS(=O)(=O)CCCS FTCLAXOKVVLHEG-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000010407 anodic oxide Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- FRTIVUOKBXDGPD-UHFFFAOYSA-M sodium;3-sulfanylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CCCS FRTIVUOKBXDGPD-UHFFFAOYSA-M 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
Abstract
The invention relates to the technical field of lead frames, in particular to a high-strength lead frame and a preparation method thereof, wherein pure copper is used as a matrix of the lead frame, and a micro-nano structure of a uniform array is generated on the surface of a copper sheet through anodic oxidation; the composite carbon nanotube is a silver-lanthanum-based organic framework composite carbon nanotube with sulfhydryl porphyrin as ligand; blending the composite carbon nano tube and polyvinyl alcohol as a binder of the cladding layer; the composite carbon nano tube, tungsten oxide, aluminum and Ni276 mixed materials are used as cladding materials, and the tungsten carbide ceramic reinforced phase with the in-situ authigenic network structure is formed by controlling the mass ratio of the composite carbon nano tube, the tungsten oxide, the aluminum and the Ni276 mixed materials; plating silver after laser cladding, improving the welding benign of the lead frame, introducing composite carbon nano tubes into silver plating solution, improving the binding force of silver and cladding layers, and sealing nano holes in the cladding layers further, thereby improving the corrosion resistance of the generated lead frame.
Description
Technical Field
The invention relates to the technical field of lead frames, in particular to a high-strength lead frame and a preparation method thereof.
Background
Along with the rapid development of social informatization, the electronic industry is an engine of the informatization society, and the electronic component is a foundation for supporting the rapid development of the electronic industry, and in the electronic component, the lead frame is an important carrier of a chip and plays roles of heat dissipation, signal transmission, power distribution and the like while fixing and supporting the chip, so that the service life of the lead frame is closely related to the service life of the electronic component.
In order to achieve the interconnectivity between the chip and the lead frame, the lead frame has good weldability, so in practical application, how to improve the strength, the wear resistance and the corrosion resistance of the lead frame while keeping the good weldability of the lead frame is an important research point in the field.
Disclosure of Invention
The invention aims to provide a high-strength lead frame and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a method of making a high strength lead frame comprising the steps of:
s1: taking the copper sheet as a substrate of the lead frame, cleaning, polishing and anodizing the substrate after cleaning in sequence to obtain a pretreated substrate;
s2: preparing a binder by using composite carbon nano tubes and polyvinyl alcohol;
s3: mixing the composite carbon nano tube, tungsten oxide, aluminum and Ni276, and drying to obtain a cladding material;
s4: coating cladding material on the surface of the pretreated substrate by using an adhesive, and carrying out laser cladding to obtain a cladding lead frame;
s5: and (3) putting the cladding lead frame into silver plating solution for silver plating treatment to obtain the high-strength lead frame.
Further, the working conditions of the anodic oxidation are as follows: the current density is 0.6-0.8A/dm 2 The temperature is 65-75deg.C, and the time is 20-30min; the electrolyte used for anodic oxidation comprises the following components: deionized water is used as a solvent, wherein 35g/L of sodium hydroxide, 145g/L of sodium chloride and 2g/L of polyethylene glycol are used.
According to the invention, pure copper is used as a substrate of the lead frame, and a micro-nano structure of a uniform array is generated on the surface of the copper sheet through anodic oxidation by controlling the technological parameters of anodic oxidation, so that the bonding strength of the copper sheet and the cladding layer is improved, and the tensile strength and the corrosion resistance of the generated lead frame are improved.
Further, the preparation of the composite carbon nanotube comprises the following steps:
1) Mixing polyvinylpyrrolidone and methanol, adding carboxylated carbon nanotubes, and performing ultrasonic dispersion to obtain a carbon nanotube suspension;
2) Mixing lanthanum nitrate, silver nitrate and methanol, adding the suspension of the carbon nano tube, adding mercaptoporphyrin and methanol, stirring for 1-2h, standing for 20-22h, centrifuging, washing and drying to obtain the composite carbon nano tube.
Further, the mass ratio of lanthanum nitrate, silver nitrate, sulfhydryl porphyrin and carboxylated carbon nano tube is 1:1:5:1.
the composite carbon nanotube is a silver-lanthanum-based organic framework composite carbon nanotube with sulfhydryl porphyrin as a ligand, wherein the introduction of the bimetal organic framework plays a role of a light absorber and improves the laser efficiency; after laser, the in-situ synthesized porous carbon of the bimetal organic framework is favorable for absorbing gas, and the in-situ synthesized porous carbon of the bimetal organic framework is welded with tungsten carbide and carbon nano tubes to obtain a synergistic effect, so that the complexity of a conductive network of a cladding layer is improved, and the wear resistance and the conductivity of the generated lead frame are greatly improved.
Further, the adhesive comprises the following components in parts by weight: 0.1-0.5 part of composite carbon nano tube, 20-25 parts of polyvinyl alcohol and 75-80 parts of deionized water.
In the laser cladding, in the prior art, in order to improve the adhesive force between cladding materials and a matrix, polyvinyl alcohol is generally used as a binder, but gas is generally generated after the laser cladding to cause the generation of holes on the surface of the cladding; after laser, the in-situ synthesized porous carbon of the bimetal organic framework is favorable for absorbing gas, and the in-situ synthesized porous carbon of the bimetal organic framework is used for welding the carbon nano tube to obtain a synergistic effect, so that the conductivity of the cladding layer is improved.
Further, the mass ratio of the composite carbon nano tube, tungsten oxide, aluminum and Ni276 in the cladding material is 1:6:3:1.
the melted Ni276 has good fluidity, is beneficial to reducing the melting speed of the carbon nano tube, improves the flatness of the generated cladding layer, and improves the wear resistance of the cladding layer.
Further, the working conditions of laser cladding are as follows: argon is used as protective gas, the gas flow is 25L/min, the defocusing amount is 220mm, the spot diameter is 2mm, the scanning speed is 18mm/s, and the laser power is 1600W.
Further, the silver plating treatment conditions are as follows: the temperature is 18-25deg.C, and the current density is 0.4-0.6A/dm 2 The time is 20-30min, and the silver plating solution comprises the following components: deionized water is used as a solvent, wherein the silver nitrate is 20g/L, the composite carbon nano tube is 0.5g/L, and the 3-mercapto-1-propanesulfonic acid sodium is 2g/L.
The invention has the beneficial effects that:
the invention provides a high-strength lead frame and a preparation method thereof, wherein the lead frame with high strength, good corrosion resistance, high wear resistance and good weldability is prepared by sequentially carrying out anodic oxidation, laser cladding and electroplating silver plating on a copper sheet.
According to the invention, pure copper is used as a substrate of the lead frame, and a micro-nano structure of a uniform array is generated on the surface of the copper sheet through anodic oxidation by controlling the technological parameters of anodic oxidation, so that the bonding strength of the copper sheet and the cladding layer is improved, and the tensile strength of the generated lead frame is improved.
In the laser cladding, in the prior art, in order to improve the adhesion of cladding materials and a matrix, polyvinyl alcohol is generally used as a binder, but gas is generally generated after the laser cladding to cause the generation of holes on the surface of the cladding; after laser, the in-situ synthesized porous carbon of the bimetal organic framework is favorable for absorbing gas, and the in-situ synthesized porous carbon of the bimetal organic framework is used for welding the carbon nano tube to obtain a synergistic effect, so that the conductivity of the cladding layer is improved.
According to the invention, the composite carbon nano tube, tungsten oxide and aluminum are mixed as cladding materials, the tungsten carbide ceramic reinforced phase with an in-situ authigene network structure is formed by controlling the mass ratio of the composite carbon nano tube, the composite carbon nano tube is a silver lanthanum-based organic framework composite carbon nano tube with sulfhydryl porphyrin as a ligand, and the in-situ synthesized porous carbon welding tungsten carbide of the bimetal organic framework obtains a synergistic effect while playing a role in improving the laser efficiency by a light absorber, so that the complexity of a conductive network of a cladding layer is improved, and the wear resistance and the conductivity of a generated lead frame are greatly improved; the melted Ni276 has good fluidity, is beneficial to reducing the melting speed of the carbon nano tube, improves the flatness of the generated cladding layer, and improves the wear resistance of the cladding layer.
Plating silver after laser cladding, improving the welding benign of the lead frame, introducing composite carbon nano tubes into silver plating solution, improving the binding force of silver and cladding layers, and sealing nano holes in the cladding layers further, thereby improving the corrosion resistance of the generated lead frame.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely in connection with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, if directional indications such as up, down, left, right, front, and rear … … are involved in the embodiment of the present invention, the directional indications are merely used to explain a relative positional relationship, a movement condition, and the like between a certain posture such as the respective components, and if the certain posture is changed, the directional indications are changed accordingly. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The following description of the embodiments of the present invention will be presented in further detail with reference to the examples, which should be understood as being merely illustrative of the present invention and not limiting.
Example 1: a method of making a high strength lead frame comprising the steps of:
s1: taking the copper sheet as a substrate of the lead frame, cleaning, polishing and anodizing the substrate after cleaning in sequence to obtain a pretreated substrate;
the anodic oxidation working conditions are as follows: the current density was 0.6A/dm 2 At a temperature of 65 DEG CThe time is 30min; the electrolyte used for anodic oxidation comprises the following components: deionized water is used as a solvent, wherein 35g/L of sodium hydroxide, 145g/L of sodium chloride and 2g/L of polyethylene glycol are used;
the preparation of the composite carbon nano tube comprises the following steps:
1) Mixing 0.5g of polyvinylpyrrolidone and 100mL of methanol, adding 0.5g of carboxylated carbon nanotubes, and performing ultrasonic dispersion to obtain a carbon nanotube suspension;
2) Mixing 0.1g of lanthanum nitrate, 0.1g of silver nitrate and 10mL of methanol, adding the suspension of the carbon nano tube, adding 0.5g of mercaptoporphyrin and 10mL of methanol, stirring for 1h, standing for 20h, centrifuging, washing and drying to obtain the composite carbon nano tube;
s2: preparing a binder by using composite carbon nano tubes and polyvinyl alcohol;
the adhesive comprises the following components in parts by weight: 0.1 part of composite carbon nano tube, 20 parts of polyvinyl alcohol and 80 parts of deionized water;
s3: mixing the composite carbon nano tube, tungsten oxide, aluminum and Ni276, and drying to obtain a cladding material;
the mass ratio of the composite carbon nano tube, tungsten oxide, aluminum and Ni276 in the cladding material is 1:6:3:1, a step of;
s4: coating cladding material on the surface of the pretreated substrate by using an adhesive, and carrying out laser cladding to obtain a cladding lead frame;
the working conditions of laser cladding are as follows: argon is used as protective gas, the gas flow is 25L/min, the defocusing amount is 220mm, the spot diameter is 2mm, the scanning speed is 18mm/s, and the laser power is 1600W;
s5: placing the cladding lead frame into silver plating solution for silver plating treatment to obtain a high-strength lead frame;
the silver plating treatment working conditions are as follows: the temperature was 18℃and the current density was 0.4A/dm 2 The time is 20min, and the silver plating solution comprises the following components: deionized water is used as a solvent, wherein the silver nitrate is 20g/L, the composite carbon nano tube is 0.5g/L, and the 3-mercapto-1-propanesulfonic acid sodium is 2g/L.
Example 2: a method of making a high strength lead frame comprising the steps of:
s1: taking the copper sheet as a substrate of the lead frame, cleaning, polishing and anodizing the substrate after cleaning in sequence to obtain a pretreated substrate;
the anodic oxidation working conditions are as follows: the current density was 0.7A/dm 2 The temperature is 70 ℃ and the time is 25min; the electrolyte used for anodic oxidation comprises the following components: deionized water is used as a solvent, wherein 35g/L of sodium hydroxide, 145g/L of sodium chloride and 2g/L of polyethylene glycol are used;
the preparation of the composite carbon nano tube comprises the following steps:
1) Mixing 0.5g of polyvinylpyrrolidone and 100mL of methanol, adding 0.5g of carboxylated carbon nanotubes, and performing ultrasonic dispersion to obtain a carbon nanotube suspension;
2) Mixing 0.1g of lanthanum nitrate, 0.1g of silver nitrate and 10mL of methanol, adding the suspension of the carbon nano tube, adding 0.5g of mercaptoporphyrin and 10mL of methanol, stirring for 1.5h, standing for 21h, centrifuging, washing and drying to obtain the composite carbon nano tube;
s2: preparing a binder by using composite carbon nano tubes and polyvinyl alcohol;
the adhesive comprises the following components in parts by weight: 0.3 part of composite carbon nano tube, 24 parts of polyvinyl alcohol and 78 parts of deionized water;
s3: mixing the composite carbon nano tube, tungsten oxide, aluminum and Ni276, and drying to obtain a cladding material;
the mass ratio of the composite carbon nano tube, tungsten oxide, aluminum and Ni276 in the cladding material is 1:6:3:1, a step of;
s4: coating cladding material on the surface of the pretreated substrate by using an adhesive, and carrying out laser cladding to obtain a cladding lead frame;
the working conditions of laser cladding are as follows: argon is used as protective gas, the gas flow is 25L/min, the defocusing amount is 220mm, the spot diameter is 2mm, the scanning speed is 18mm/s, and the laser power is 1600W;
s5: placing the cladding lead frame into silver plating solution for silver plating treatment to obtain a high-strength lead frame;
the silver plating treatment working conditions are as follows: the temperature was 20℃and the current density was 0.5A/dm 2 The time is 25min, and the silver plating solution comprises the following components: deionized water is used as a solvent,wherein, 20g/L of silver nitrate, 0.5g/L of composite carbon nano tube and 2g/L of 3-mercapto-1-propane sodium sulfonate.
Example 3: a method of making a high strength lead frame comprising the steps of:
s1: taking the copper sheet as a substrate of the lead frame, cleaning, polishing and anodizing the substrate after cleaning in sequence to obtain a pretreated substrate;
the anodic oxidation working conditions are as follows: the current density was 0.8A/dm 2 The temperature is 75 ℃ and the time is 30min; the electrolyte used for anodic oxidation comprises the following components: deionized water is used as a solvent, wherein 35g/L of sodium hydroxide, 145g/L of sodium chloride and 2g/L of polyethylene glycol are used;
the preparation of the composite carbon nano tube comprises the following steps:
1) Mixing 0.5g of polyvinylpyrrolidone and 100mL of methanol, adding 0.5g of carboxylated carbon nanotubes, and performing ultrasonic dispersion to obtain a carbon nanotube suspension;
2) Mixing 0.1g of lanthanum nitrate, 0.1g of silver nitrate and 10mL of methanol, adding the suspension of the carbon nano tube, adding 0.5g of mercaptoporphyrin and 10mL of methanol, stirring for 2 hours, standing for 22 hours, centrifuging, washing and drying to obtain the composite carbon nano tube;
s2: preparing a binder by using composite carbon nano tubes and polyvinyl alcohol;
the adhesive comprises the following components in parts by weight: 0.5 part of composite carbon nano tube, 25 parts of polyvinyl alcohol and 80 parts of deionized water;
s3: mixing the composite carbon nano tube, tungsten oxide, aluminum and Ni276, and drying to obtain a cladding material;
the mass ratio of the composite carbon nano tube, tungsten oxide, aluminum and Ni276 in the cladding material is 1:6:3:1, a step of;
s4: coating cladding material on the surface of the pretreated substrate by using an adhesive, and carrying out laser cladding to obtain a cladding lead frame;
the working conditions of laser cladding are as follows: argon is used as protective gas, the gas flow is 25L/min, the defocusing amount is 220mm, the spot diameter is 2mm, the scanning speed is 18mm/s, and the laser power is 1600W;
s5: placing the cladding lead frame into silver plating solution for silver plating treatment to obtain a high-strength lead frame;
the silver plating treatment working conditions are as follows: the temperature was 25℃and the current density was 0.6A/dm 2 The time is 30min, and the silver plating solution comprises the following components: deionized water is used as a solvent, wherein the silver nitrate is 20g/L, the composite carbon nano tube is 0.5g/L, and the 3-mercapto-1-propanesulfonic acid sodium is 2g/L.
Comparative example 1: in the control group of example 3, no anodic oxidation was performed, and the other steps were normal.
Comparative example 2: using example 3 as a control group and polyvinyl alcohol as a binder, the other procedures were normal.
Comparative example 3: taking example 3 as a control group, the mass ratio of the composite carbon nano tube, the tungsten oxide, the aluminum and the Ni276 is 0.5:6:3:1, other processes are normal.
Comparative example 4: with example 3 as a control group, no Ni276 was added to the clad material, and the other procedures were normal.
Comparative example 5: with example 3 as a control group, the composite carbon nanotubes were replaced with carbon nanotubes, and the other procedures were normal.
Comparative example 6: in the case of example 3 as a control group, no composite carbon nanotubes were added to the silver plating solution, and the other steps were normal.
In examples and comparative examples, the copper sheet had a thickness of 2mm, the anodic oxide layer had a thickness of 50 μm, and the cladding layer had a thickness of 1mm.
The sources of the raw materials are as follows:
copper sheet (purity 99.9%, thickness 2 mm); polyethylene glycol P103719, polyvinylpyrrolidone P110611, lanthanum nitrate L106046, silver nitrate S196951, sodium 3-mercapto-1-propanesulfonate S432236, tungsten oxide T103857, aluminum A434751: ala Ding Shiji; ni276ERNICRMO-4: hebei Beda welding materials Co., ltd; mercaptoporphyrin (AR): green Si; carboxylated carbon nanotubes 153724: shanghai Uygur autonomous Raman Agents Co., ltd; sodium hydroxide, sodium chloride, methanol, analytically pure: national drug group reagent.
Performance test:
tensile strength: a universal force testing machine is adopted, the stretching speed is 2mm/min at 25 ℃, and the length is 20mm multiplied by 2mm; abrasion resistance: with reference to ASTM standard No. G99-95, the friction pair is in a ball-disc contact movement mode, the speed is 0.30m/s, and the normal load is 14N; conductivity: using a digital four-probe tester to test the conductivity; salt spray resistance: referring to GB/T1771-2007, the temperature is 35 ℃, the pH is 6.8, and the concentration of sodium chloride is 55g/L; the results obtained are shown in the following table;
the invention provides a high-strength lead frame and a preparation method thereof, wherein the lead frame with high strength, good corrosion resistance, high wear resistance and good weldability is prepared by sequentially carrying out anodic oxidation, laser cladding and electroplating silver plating on a copper sheet.
Comparing example 3 with comparative example 1, the invention uses pure copper as the substrate of the lead frame, and by controlling the anodic oxidation process parameters, a micro-nano structure of uniform array is generated on the surface of the copper sheet through anodic oxidation, and the bonding strength of the copper sheet and the cladding layer is improved, thereby improving the tensile strength of the generated lead frame.
As is clear from comparison between example 3 and comparative example 2, in the laser cladding, in the prior art, in order to improve adhesion between the cladding material and the substrate, polyvinyl alcohol is generally used as a binder, but after laser cladding, gas is generally generated to cause generation of holes on the surface of the cladding layer.
As can be seen from comparing example 3 with comparative example 3, the invention uses composite carbon nanotube, tungsten oxide and aluminum mixture as cladding material, and the weight ratio is controlled to make the tungsten carbide ceramic reinforced phase with in-situ self-generated network structure.
Comparing example 3 with comparative example 4 shows that the melted Ni276 has good fluidity, which is beneficial to reducing the melting speed of the carbon nanotubes, improving the flatness of the generated cladding layer and improving the wear resistance of the cladding layer.
Comparing example 3 with comparative example 5, it can be seen that the composite carbon nanotube is a silver lanthanum-based organic skeleton composite carbon nanotube using thiol porphyrin as ligand, wherein the introduction of the bimetallic organic skeleton can improve the laser efficiency while playing the role of light absorber; after laser, the in-situ synthesized porous carbon of the bimetal organic framework is favorable for absorbing gas, and the in-situ synthesized porous carbon of the bimetal organic framework is welded with tungsten carbide and carbon nano tubes to obtain a synergistic effect, so that the complexity of a conductive network of a cladding layer is improved, and the wear resistance and the conductivity of the generated lead frame are greatly improved.
Comparing example 3 with comparative example 6, it is known that plating silver plating is performed after laser cladding, improving soldering benign of the lead frame, introducing composite carbon nanotubes into silver plating solution, improving binding force of silver and cladding layer, and further sealing nano holes existing in the cladding layer, thereby improving corrosion resistance of the resulting lead frame.
In conclusion, the high-strength lead frame is prepared and has good application prospect.
The foregoing description is only exemplary embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.
Claims (6)
1. A method of making a high strength lead frame comprising the steps of:
s1: taking the copper sheet as a substrate of the lead frame, cleaning, polishing and anodizing the substrate after cleaning in sequence to obtain a pretreated substrate;
s2: preparing a binder by using composite carbon nano tubes and polyvinyl alcohol;
s3: mixing the composite carbon nano tube, tungsten oxide, aluminum and Ni276, and drying to obtain a cladding material;
s4: coating cladding material on the surface of the pretreated substrate by using an adhesive, and carrying out laser cladding to obtain a cladding lead frame;
s5: placing the cladding lead frame into silver plating solution for silver plating treatment to obtain a high-strength lead frame;
the anodic oxidation working conditions are as follows: the current density is 0.6-0.8A/dm 2 The temperature is 65-75deg.C, and the time is 20-30min;
the mass ratio of the composite carbon nano tube, tungsten oxide, aluminum and Ni276 in the cladding material is 1:6:3:1, a step of;
the silver plating treatment working conditions are as follows: the temperature is 18-25deg.C, and the current density is 0.4-0.6A/dm 2 The time is 20-30min, and the silver plating solution comprises the following components: deionized water is used as a solvent, wherein 20g/L of silver nitrate, 0.5g/L of composite carbon nano tube and 2g/L of 3-mercapto-1-propanesulfonic acid sodium salt are used;
the preparation of the composite carbon nano tube comprises the following steps:
1) Mixing polyvinylpyrrolidone and methanol, adding carboxylated carbon nanotubes, and performing ultrasonic dispersion to obtain a carbon nanotube suspension;
2) Mixing lanthanum nitrate, silver nitrate and methanol, adding the suspension of the carbon nano tube, adding mercaptoporphyrin and methanol, stirring for 1-2h, standing for 20-22h, centrifuging, washing and drying to obtain the composite carbon nano tube.
2. The method for manufacturing a high-strength lead frame according to claim 1, wherein the composition of the electrolyte used for the anodic oxidation is: deionized water is used as a solvent, wherein 35g/L of sodium hydroxide, 145g/L of sodium chloride and 2g/L of polyethylene glycol are used.
3. The method for manufacturing a high-strength lead frame according to claim 1, wherein the composition of the binder is, in parts by mass: 0.1-0.5 part of composite carbon nano tube, 20-25 parts of polyvinyl alcohol and 75-80 parts of deionized water.
4. The method for manufacturing a high-strength lead frame according to claim 1, wherein the working conditions of the laser cladding are: argon is used as protective gas, the gas flow is 25L/min, the defocusing amount is 220mm, the spot diameter is 2mm, the scanning speed is 18mm/s, and the laser power is 1600W.
5. The method for preparing the high-strength lead frame according to claim 1, wherein in the preparation of the composite carbon nanotubes, the mass ratio of lanthanum nitrate, silver nitrate, mercaptoporphyrin and carboxylated carbon nanotubes is 1:1:5:1.
6. a high strength leadframe prepared by the method of any one of claims 1-5.
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