WO2022088216A1 - Chemical nickel-plating process for steel sheet, phosphorus-nickel-plated steel sheet and vapor chamber - Google Patents

Chemical nickel-plating process for steel sheet, phosphorus-nickel-plated steel sheet and vapor chamber Download PDF

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Publication number
WO2022088216A1
WO2022088216A1 PCT/CN2020/126623 CN2020126623W WO2022088216A1 WO 2022088216 A1 WO2022088216 A1 WO 2022088216A1 CN 2020126623 W CN2020126623 W CN 2020126623W WO 2022088216 A1 WO2022088216 A1 WO 2022088216A1
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Prior art keywords
nickel
steel sheet
phosphorus
nickel plating
electroless nickel
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PCT/CN2020/126623
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French (fr)
Chinese (zh)
Inventor
陈晓杰
徐莎莎
石一卉
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瑞声声学科技(深圳)有限公司
瑞声科技（南京）有限公司
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Publication of WO2022088216A1 publication Critical patent/WO2022088216A1/en

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1646—Characteristics of the product obtained
    • C23C18/165—Multilayered product
    • C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • 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
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • 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
    • C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D15/00—Heat-exchange apparatus with the intermediate heat-transfer medium in closed tubes passing into or through the conduit walls ; Heat-exchange apparatus employing intermediate heat-transfer medium or bodies
    • F28D15/02—Heat-exchange apparatus with the intermediate heat-transfer medium in closed tubes passing into or through the conduit walls ; Heat-exchange apparatus employing intermediate heat-transfer medium or bodies in which the medium condenses and evaporates, e.g. heat pipes
    • F28D15/04—Heat-exchange apparatus with the intermediate heat-transfer medium in closed tubes passing into or through the conduit walls ; Heat-exchange apparatus employing intermediate heat-transfer medium or bodies in which the medium condenses and evaporates, e.g. heat pipes with tubes having a capillary structure

Definitions

  • the present application relates to the technical field of heat-dissipating components, and in particular, to an electroless nickel plating process for steel sheets, a phosphorus-nickel-plated steel sheet prepared by the electroless nickel-plating process for steel sheets, and a soaking plate including the phosphorus-nickel-plated steel sheet.
  • the vapor chamber is a two-dimensional heat conduction device. After absorbing heat, the liquid at the bottom of the vacuum chamber of the vapor chamber evaporates and diffuses into the vacuum chamber, conducts the heat to the top, and then condenses into liquid and returns to the bottom.
  • This kind of evaporation and condensation process similar to the refrigerator air conditioner circulates rapidly in the vacuum chamber to achieve a relatively high heat dissipation efficiency.
  • the upper cover and lower cover of the traditional vapor chamber are mostly copper and copper alloys, and the material strength and support effect are lacking, making it difficult to ultra-thin.
  • steel is used as a high-strength support material for the vapor chamber, non-condensable gas will be generated during use, which cannot be used directly. It needs to be chemically or physically covered on the inside of the cover plate.
  • the traditional solution is to improve the above problems by covering the surface of the steel with a copper layer, but due to the formation of galvanic cells between the copper and the steel, the reaction between the steel and the water is accelerated, thereby reducing the service life of the steel.
  • a process for electroless nickel plating of steel sheet comprising the following steps:
  • the steel sheet is pretreated to obtain a pretreated steel sheet
  • the pretreated steel sheet is electroplated with nickel, a nickel layer is formed on the nickel-plated steel sheet, and the nickel-plated steel sheet is obtained after cleaning;
  • the nickel-plated steel sheet is immersed in the above-mentioned electroless nickel plating solution for electroless nickel-plating treatment, a phosphorus-nickel layer is formed on the nickel layer, and the phosphorus-nickel-plated steel sheet is obtained after cleaning and drying.
  • a phosphorus-nickel-plated steel sheet is prepared by adopting the above-mentioned chemical nickel-plating process for the steel sheet.
  • a temperature equalizing plate comprising an upper cover plate, a capillary structure and a lower cover plate arranged in sequence, a closed cavity is formed between the upper cover plate and the lower cover plate, and the capillary structure is arranged in the closed cavity ;
  • the upper cover plate and/or the lower cover plate is the above-mentioned phosphorus nickel-plated steel sheet.
  • the above-mentioned electroless nickel plating process for the steel sheet can form a high phosphorus phosphorus-nickel layer on the nickel layer of the nickel-plated steel sheet, thereby obtaining a phosphorus-nickel-plated steel sheet.
  • the phosphorus-nickel-plated steel sheet is used as the cover plate of the soaking plate, the phosphorus-nickel layer reduces the reaction of the phosphorus-nickel-plated steel sheet with water.
  • the phosphorus-nickel-plated steel sheet has The reaction between steel and water will not be accelerated due to the formation of galvanic cells between copper and steel, so that the service life of the phosphorus-nickel-plated steel sheet can be extended by about 3 times to 5 times.
  • the bonding force between the steel sheet, the nickel layer and the phosphorus-nickel layer is good, and the total thickness can be no more than 10 ⁇ m, so that the thickness of the steel sheet will not be caused. increase.
  • lactic acid, succinic acid, citrate and acetic acid in the electroless nickel plating solution take into account both buffering and complexation, and when the concentration is too low, the plating speed is slow, the stability of the electroless nickel plating solution is poor, and the electroless nickel plating solution is easy to produce.
  • the nickel compound precipitates and accelerates the decomposition of the electroless nickel plating solution. When the concentration is too high, the complexing ability is too strong and the reaction efficiency is low.
  • FIG. 1 is a flow chart of an electroless nickel plating process for a steel sheet according to an embodiment.
  • FIG. 2 is a specific flow chart of S20 of the electroless nickel plating process on the steel sheet shown in FIG. 1 .
  • FIG. 3 is a schematic three-dimensional structure diagram of a vapor chamber according to an embodiment.
  • FIG. 4 is a schematic view of the cross-sectional structure of the vapor chamber shown in FIG. 3 along the A-A direction.
  • a steel sheet electroless nickel plating process of an embodiment as shown in FIG. 1 includes the following steps:
  • S10. Provide steel sheets.
  • the steel sheet is a stainless steel sheet.
  • the thickness of the steel sheet may be 0.05mm-0.4mm.
  • the steel sheet may be an ordinary steel sheet, or may be a steel sheet with an etched structure obtained after etching treatment.
  • pretreatment usually includes operations such as degreasing treatment, pickling treatment, and activation treatment.
  • S20 is:
  • the degreasing liquid includes 10g/L-50g/L sodium hydroxide, 10g/L-50g/L sodium carbonate and 1mL/L-5mL/L OP emulsifier.
  • degreasing treatment is to remove oil stains on the surface of the steel sheet and make the surface of the steel sheet completely hydrophilic.
  • the OP emulsifier in the degreasing solution acts as a surfactant to improve its dispersibility and wettability, which is beneficial to enhance the degreasing ability. When it is too low, the effect is not good, and when it is too high, it is easy to remain on the surface and difficult to clean.
  • the cleaning operation is to use pure water to clean.
  • the pickling solution includes 20%-30% hydrochloric acid and 3g/L-5g/L rhodin in volume fraction.
  • pickling treatment is to remove the oxide scale on the surface of the steel sheet.
  • Hydrochloric acid has a strong ability to remove stainless steel oxide scale.
  • concentration is too low, it takes a long time and the efficiency is low.
  • concentration is too high, the surface will be corroded, and the corrosion will be accelerated when the temperature is too high. Therefore, the temperature of the pickling treatment is not suitable. higher than 40°C.
  • an appropriate amount of corrosion inhibitor such as rhodin can be added to it. If the content of the inhibitor is too low or too high, the pickling efficiency will be affected.
  • the cleaning operation is to use pure water to clean.
  • the activation solution includes hydrochloric acid with a volume fraction of 10%-20% and acetic acid with a volume fraction of 5g/L-10g/L.
  • the temperature of the activation solution is 20°C-25°C.
  • the purpose of the activation treatment is to improve the surface activity of the steel sheet and ensure the bonding force between the electroless nickel plating layer and the steel sheet.
  • the acidity of the activation solution should not be too high and the time should not be too long, because the oxide layer is no longer or very thin after pickling. Too high acidity or too long time will lead to over-corrosion and affect the performance of the steel sheet. It is best to keep it at a lower concentration ( ⁇ 20%) and supplemented with a certain amount of acetic acid to reduce the corrosion of chloride ions, but the concentration should not be too low ( ⁇ 10%) to ensure the effect, especially when the residence time between pickling and electroless nickel plating is long.
  • the temperature of the activation treatment may be 20°C or 25°C.
  • the cleaning operation is to use pure water to rinse, and the nickel-plated steel sheet obtained after the rinse is quickly immersed in an electroplating solution for electroplating nickel to carry out the next reaction.
  • the operation of nickel electroplating is to form a thin layer of nickel on the surface of the pretreated steel sheet by impacting nickel, on the one hand to improve the bonding force of the high phosphorus phosphorus-nickel layer formed by electroless plating, and on the other hand to improve the surface of the steel sheet. Reactivity of electroless plating.
  • the cathode is the pretreated steel sheet
  • the anode is an electrolytic nickel plate
  • the cathode current density is 5A/dm 2 -10A/dm 2
  • the electroplating solution includes 200g/L-250g /L nickel chloride and 100mL/L-120mL/L hydrochloric acid
  • the plating time is 30s-1min.
  • the current density used for impact nickel should be higher than that of general nickel plating (2-5 times), the purpose is to quickly deposit a thin nickel layer with good bonding force.
  • the mass ratio of nickel chloride and hydrochloric acid in the electroplating solution is controlled to be 1.5-2.2:1.
  • the mass ratio of nickel chloride and hydrochloric acid is between 1.5 and 2.2. If the acidity is not enough, there will be problems with the adhesion of the coating. If the content of the main salt is too low, the coating speed may be slow and the coating may be uneven.
  • the cleaning operation is to rinse with pure water at 70°C-80°C.
  • Electroless nickel plating solution includes 20g/L-30g/L nickel salt, 20g/L-30g/L hypophosphite, 20g/L-25g/L lactic acid, 5g/L-10g/L succinic acid, 0.5g/L-2g/L citrate and 5mL/L-10mL/L acetic acid, the pH of electroless nickel plating solution is 4.4-4.8.
  • the above-mentioned electroless nickel plating solution can be used for electroless nickel plating of nickel-plated steel sheets, and its purpose is to form a high-phosphorus high-phosphorus phosphorus-nickel layer on the nickel layer of nickel-plated steel sheets, thereby obtaining phosphorus-nickel-plated steel sheets.
  • the phosphorus-nickel layer reduces the reaction of the phosphorus-nickel-plated steel sheet with water.
  • the phosphorus-nickel-plated steel sheet has The reaction between steel and water will not be accelerated due to the formation of galvanic cells between copper and steel, so that the service life of the phosphorus-nickel-plated steel sheet can be extended by about 3 times to 5 times.
  • the bonding force between the steel sheet, the nickel layer and the phosphorus-nickel layer is good, and the total thickness can be no more than 10 ⁇ m, so that the thickness of the steel sheet will not be increased. .
  • lactic acid, succinic acid, citrate and acetic acid in the electroless nickel plating solution take into account both buffering and complexation, and when the concentration is too low, the plating speed is slow, the stability of the electroless nickel plating solution is poor, and the electroless nickel plating solution is easy to produce.
  • the nickel compound precipitates and accelerates the decomposition of the electroless nickel plating solution. When the concentration is too high, the complexing ability is too strong and the reaction efficiency is low.
  • nickel salts, hypophosphites and citrates are all substances that can be dissolved in the passivation solution at pH 4-6.
  • the nickel salt can be nickel sulfate or nickel acetate.
  • the hypophosphite can be sodium hypophosphite or potassium hypophosphite.
  • the citrate can be sodium citrate or potassium citrate.
  • the electroless nickel plating solution further includes 0.1 mg/L-0.4 mg/L of ammonium molybdate, 0.5 mg/L-1 mg/L of tellurium oxide and 1 mg/L-2 mg/L of copper sulfate.
  • ammonium molybdate, tellurium oxide and copper sulfate can improve the stability of the plating solution and the efficiency of electroless plating.
  • the stability effect is not good when the concentration is low, and the reactivity is affected when the concentration is high.
  • the pH of the electroless nickel plating solution is adjusted to 4.4-4.8 by ammonia water.
  • the electroless nickel plating solution further includes 0.2g/L-1g/L of wetting agent.
  • the humectant may be dihexyl sulfosuccinate sodium salt.
  • the purpose of adding wetting agent is to reduce the surface tension of the solution and reduce the pores, and 0.21g/L-1g/L can satisfy the effect.
  • the electroless nickel plating solution further includes a combination of additives.
  • the combined additive may be selected from at least two of benzenesulfonic acid, sodium allylsulfonate, propargyl alcohol ethoxylate, N,N-diethylpropargylamine, and sulfosalicylic acid.
  • the function of the combined additive is to adsorb on the surface of the nickel-plated steel sheet during the electroless plating process to reduce the roughness of the coating, in order to achieve the effect of high corrosion resistance.
  • the temperature of the electroless nickel-plating solution is 86°C-90°C, and the soaking time of the nickel-plated steel sheet is 60min-90min.
  • the molar ratio of nickel ions and hypophosphite ions in the electroless nickel plating solution is controlled to be 0.3-0.45:1, which is mainly It is to ensure the stability of electroless nickel plating solution and high plating speed.
  • the present application also discloses a phosphor-nickel-plated steel sheet prepared by using the above-mentioned chemical nickel-plating process for the steel sheet.
  • the above-mentioned phosphorus-nickel-plated steel sheet can be applied in various fields, and the electroless nickel-plated layer greatly improves the corrosion resistance and service life of the phosphorus-nickel-plated steel sheet.
  • the present application also discloses an embodiment of a uniform temperature plate 100 , which includes an upper cover plate 10 , a capillary structure 20 and a lower cover plate 30 arranged in sequence, and between the upper cover plate 10 and the lower cover plate 30 A closed cavity 40 is formed, and the capillary structure 20 is disposed in the closed cavity 40 .
  • the upper cover plate 10 and/or the lower cover plate 30 are the above-mentioned phosphorus nickel-plated steel sheets.
  • the electroless nickel plating layer of the phosphorus-nickel-plated steel sheet can avoid the non-condensable gas generated by the phosphorus-nickel-plated steel sheet as the upper cover plate 10 and the lower cover plate 30 of the vaporizing plate 100 during use. Improves corrosion resistance and service life of phosphorus-nickel-plated steel sheets.
  • the inner wall of the upper cover plate 10 is flat, and the inner wall of the lower cover plate 30 is provided with a plurality of support columns 32 .
  • the capillary structure 20 is disposed on the inner wall of the upper cover plate 10 .
  • the material of the capillary structure 20 is copper or copper alloy.
  • the capillary structure 20 can be obtained by means of metal wire weaving, metal powder sintering, surface electrochemical deposition, and the like.
  • the temperature equalizing plate 100 of this embodiment is assembled by welding the upper cover plate 10 and the lower cover plate 30 together.
  • a stainless steel cover plate is obtained by etching a stainless steel sheet with a thickness of 0.05-0.4 mm.
  • Degreasing Soak the stainless steel cover in a degreasing solution at 70°C for 30 minutes, and then rinse it off with pure water immediately.
  • the degreasing solution consists of 20g/L sodium hydroxide, 30g/L sodium carbonate and 3mL/L L's OP emulsifier;
  • Pickling soak the degreasing stainless steel cover in the pickling solution for 1 min at room temperature, and then immediately clean it with pure water.
  • the components of the pickling solution are 20% hydrochloric acid and 3g/L Ding;
  • Activation soak the acid-washed stainless steel cover in the activation solution for 30s at room temperature, take it out, rinse it quickly, and immediately put it into the tank for the next step.
  • the activation solution is 10% hydrochloric acid and 5g/L hydrochloric acid. acetic acid;
  • electroplating nickel (impact nickel) treatment the activated stainless steel cover plate is used as the cathode, the electrolytic nickel plate with a purity of 99.99% is used as the anode, the cathode current density is 8A/dm 2 , and the electroplating solution includes 240g/L nickel chloride and 120mL/L of hydrochloric acid, the electroplating time is 30s, and the nickel-plated stainless steel cover plate is obtained after the electroplating is completed.
  • Electroless nickel plating treatment Soak the nickel-plated stainless steel cover in an electroless nickel plating solution at 86°C for 90 minutes, wash it with pure water, and place it in an oven at 120°C to dry for 20 minutes, forming a high layer on the nickel-plated stainless steel cover.
  • the phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate.
  • the composition of electroless nickel plating solution is nickel sulfate 25g/L, sodium hypophosphite 20g/L, lactic acid 24g/L, succinic acid 10g/L, sodium citrate 1g/L, acetic acid 8mL/L, ammonium molybdate 0.24mg/L L, tellurium oxide 1mg/L, copper sulfate 2mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, benzenesulfonic acid 50mg/L, sodium allyl sulfonate 20mg/L, propynyl alcohol ethyl Oxygen compound 20mg/L, the pH value of the solution was adjusted to 4.6 with ammonia water.
  • Embodiment 2 S10, S20 and S30 are the same as those in Embodiment 1.
  • Electroless nickel plating treatment Soak the nickel-plated stainless steel cover in an electroless nickel plating solution at 86°C for 90 minutes, wash it with pure water, and place it in an oven at 120°C to dry for 20 minutes, forming a high layer on the nickel-plated stainless steel cover.
  • the phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate.
  • the composition of electroless nickel plating solution is nickel sulfate 25g/L, sodium hypophosphite 24g/L, lactic acid 22g/L, succinic acid 12g/L, sodium citrate 1g/L, acetic acid 8mL/L, ammonium molybdate 0.24mg/L L, tellurium oxide 1mg/L, copper sulfate 2mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, allyl sodium sulfonate 30mg/L, propynyl alcohol ethoxylate 20mg/L, N,N-diethylpropargylamine 5mg/L, the pH value of the solution was adjusted to 4.6 with ammonia water.
  • Embodiment 3 S10, S20 and S30 are the same as those in Embodiment 1.
  • Electroless nickel plating treatment Soak the nickel-plated stainless steel cover in an electroless nickel plating solution at 86°C for 90 minutes, wash it with pure water, and place it in an oven at 120°C to dry for 20 minutes, forming a high layer of nickel-plated stainless steel cover. The phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate.
  • the composition of electroless nickel plating solution is nickel sulfate 26g/L, sodium hypophosphite 22g/L, lactic acid 24g/L, succinic acid 10g/L, sodium citrate 1.5g/L, acetic acid 8mL/L, ammonium molybdate 0.2mg /L, tellurium oxide 1mg/L, copper sulfate 2mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, allyl sodium sulfonate 30mg/L, propargyl alcohol ethoxylate 10mg/L , N,N-diethylpropargylamine 15mg/L, and the pH value of the solution was adjusted to 4.6 with ammonia water.
  • Embodiment 4 S10, S20 and S30 are the same as those in Embodiment 1.
  • Electroless nickel plating treatment Soak the nickel-plated stainless steel cover plate in an electroless nickel plating solution at 90°C for 60 minutes, wash it with pure water, and put it in an oven at 120°C to dry for 20 minutes. A layer of high-grade nickel-plated stainless steel cover plate is formed. The phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate.
  • the composition of electroless nickel plating solution is nickel acetate 24g/L, sodium hypophosphite 20g/L, lactic acid 22g/L, succinic acid 10g/L, sodium citrate 1g/L, acetic acid 8mL/L, ammonium molybdate 0.18mg/L L, tellurium oxide 1mg/L, copper sulfate 2mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, sulfosalicylic acid 30mg/L, propargyl alcohol ethoxylate 20mg/L, benzene Sulfonic acid was 10 mg/L, and the pH value of the solution was adjusted to 4.4 with ammonia water.
  • Embodiment 5 S10, S20 and S30 are the same as those in Embodiment 1.
  • Electroless nickel plating treatment Soak the nickel-plated stainless steel cover in an electroless nickel plating solution at 88°C for 70 minutes, rinse with pure water, and place it in an oven at 120°C to dry for 20 minutes. A layer of high layer is formed on the nickel-plated stainless steel cover. The phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate.
  • the composition of electroless nickel plating solution is nickel sulfate 28g/L, sodium hypophosphite 30g/L, lactic acid 25g/L, succinic acid 10g/L, sodium citrate 2g/L, acetic acid 6mL/L, ammonium molybdate 0.3mg/L L, tellurium oxide 1mg/L, copper sulfate 1.5mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, sulfosalicylic acid 30mg/L, N,N-diethylpropynamide 10mg /L, benzenesulfonic acid 20mg/L, and the pH value of the solution was adjusted to 4.8 with ammonia water.
  • Coating adhesion The cathode test method is used to characterize the coating adhesion.
  • the coated steel sheet is placed in a 5% sodium hydroxide solution as the cathode, and the stainless steel is used as the anode.
  • the operating temperature is 90° and 10A is used. /dm 2 current for 15min electrolytic treatment, the coating with poor adhesion will form many bubbles after treatment and separate from the steel sheet.
  • Coating thickness and phosphorus content The coating thickness and phosphorus content of the phosphorus-plated nickel stainless steel cover plates prepared in Examples 1-5 were measured by an X-ray fluorescence film thickness meter. The specific test results are shown in the following standard 1.
  • the thickness of the plating layer of the phosphorus-nickel-plated stainless steel cover plates prepared in Examples 1 to 5 is all less than 10 ⁇ m, and the phosphorus content of the plating layer is between 11% and 14%.
  • Example 1 Put the phosphorus-nickel-plated stainless steel cover plates prepared in Example 1-Example 5 together with the untreated stainless steel cover plate into a 100 °C aging test box, and by tracking and measuring the temperature difference between the two ends of the stainless steel cover plate, it can be simulated. The performance difference between the two in a normal environment.
  • the temperature difference between the phosphorus-nickel-plated stainless steel cover plates prepared in Examples 1 to 5 can be kept within 10°C after 96h, and the temperature difference from the untreated stainless steel cover plates (after 24h-30h is greater than 10°C) ), the service life can be increased by more than 3 times.

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Abstract

The present application provides a chemical nickel-plating process for a steel sheet, a phosphorus-nickel-plated steel sheet and a vapor chamber. The chemical nickel-plating process for a steel sheet comprises the following steps: providing a steel sheet; pretreating the steel sheet to obtain a pretreated steel sheet; electroplating the pretreated steel sheet with nickel to form a nickel layer on a pretreated steel sheet, and cleaning same to obtain a nickel-plated steel sheet; and soaking the nickel-plated steel sheet in a chemical nickel-plating solution for a chemical nickel-plating treatment to form a phosphorus-nickel layer on the nickel layer, and washing the phosphorus-nickel layer clean and drying the phosphorus-nickel layer to obtain a phosphorus-nickel-plated steel sheet. In the chemical nickel-plating process for a steel sheet, a high-phosphorus-content phosphorus-nickel layer can be formed on the nickel layer of the nickel-plated steel sheet to thereby obtain the phosphorus-nickel-plated steel sheet. When the phosphorus-nickel-plated steel sheet is used as a cover plate of the vapor chamber, the phosphorus-nickel layer reduces the reaction between the phosphorus-nickel-plated steel sheet and water, and compared with a steel sheet clad with a copper layer on the surface thereof. Even though a primary cell is formed between the copper and the steel, the phosphorus-nickel-plated steel sheet does not accelerate the reaction between the steel and water, such that the service life of the phosphorus-nickel-plated steel sheet can be prolonged by about 3-5 times.

Description

钢片化学镀镍工艺、镀磷镍钢片以及均温板Electroless nickel plating process for steel sheet, phosphorus nickel-plated steel sheet and vapor chamber 技术领域technical field
本申请涉及散热器件技术领域，尤其涉及一种钢片化学镀镍工艺、该钢片化学镀镍工艺制备得到的镀磷镍钢片以及包括该镀磷镍钢片的均温板。The present application relates to the technical field of heat-dissipating components, and in particular, to an electroless nickel plating process for steel sheets, a phosphorus-nickel-plated steel sheet prepared by the electroless nickel-plating process for steel sheets, and a soaking plate including the phosphorus-nickel-plated steel sheet.
背景技术Background technique
均温板是一种二维热传导器件，均温板的真空腔底部的液体在吸收热量后，蒸发扩散至真空腔内，将热量传导至顶部，随后冷凝为液体回到底部。这种类似冰箱空调的蒸发、冷凝过程在真空腔内快速循环，实现了相当高的散热效率。The vapor chamber is a two-dimensional heat conduction device. After absorbing heat, the liquid at the bottom of the vacuum chamber of the vapor chamber evaporates and diffuses into the vacuum chamber, conducts the heat to the top, and then condenses into liquid and returns to the bottom. This kind of evaporation and condensation process similar to the refrigerator air conditioner circulates rapidly in the vacuum chamber to achieve a relatively high heat dissipation efficiency.
技术问题technical problem
传统的均温板的上盖板和下盖板多为铜和铜合金，材料强度和支撑效果欠缺，难以超薄化。而钢材作为高强度的支撑材料用于均温板在使用过程中会产生非凝结性气体，无法直接使用，需要在盖板内侧进行化学或物理覆盖。The upper cover and lower cover of the traditional vapor chamber are mostly copper and copper alloys, and the material strength and support effect are lacking, making it difficult to ultra-thin. However, when steel is used as a high-strength support material for the vapor chamber, non-condensable gas will be generated during use, which cannot be used directly. It needs to be chemically or physically covered on the inside of the cover plate.
传统的解决方案是通过在钢材的表面覆盖铜层来改善上述问题，但由于铜和钢材之间会形成原电池而加速钢材与水的反应，从而降低了钢材的使用寿命。The traditional solution is to improve the above problems by covering the surface of the steel with a copper layer, but due to the formation of galvanic cells between the copper and the steel, the reaction between the steel and the water is accelerated, thereby reducing the service life of the steel.
技术解决方案technical solutions
基于此，有必要提供一种钢片化学镀镍工艺，通过该钢片化学镀镍工艺制备得到的镀磷镍钢片用作均热板的盖板时具有更长的使用寿命。Based on this, it is necessary to provide an electroless nickel plating process for steel sheets, and the phosphorus-nickel-plated steel sheets prepared by the electroless nickel plating process for steel sheets have longer service life when used as a cover plate of a soaking plate.
此外，还有必要提供一种该钢片化学镀镍工艺制备得到的镀磷镍钢片以及包括该镀磷镍钢片的均温板。In addition, it is also necessary to provide a phosphorus-nickel-plated steel sheet prepared by the electroless nickel-plating process of the steel sheet, and a soaking plate including the phosphorus-nickel-plated steel sheet.
一种钢片化学镀镍工艺，包括如下步骤：A process for electroless nickel plating of steel sheet, comprising the following steps:
提供钢片；provide steel sheets;
对所述钢片进行预处理，得到预处理钢片；The steel sheet is pretreated to obtain a pretreated steel sheet;
对所述预处理钢片进行电镀镍，在所述镀镍钢片上形成镍层，清洗干净后得到镀镍钢片；以及The pretreated steel sheet is electroplated with nickel, a nickel layer is formed on the nickel-plated steel sheet, and the nickel-plated steel sheet is obtained after cleaning; and
将所述镀镍钢片浸泡在上述的化学镀镍液中进行化学镀镍处理，在所述镍层上形成磷镍层，清洗干净并干燥后得到镀磷镍钢片。The nickel-plated steel sheet is immersed in the above-mentioned electroless nickel plating solution for electroless nickel-plating treatment, a phosphorus-nickel layer is formed on the nickel layer, and the phosphorus-nickel-plated steel sheet is obtained after cleaning and drying.
一种镀磷镍钢片，采用上述的钢片化学镀镍工艺制备得到。A phosphorus-nickel-plated steel sheet is prepared by adopting the above-mentioned chemical nickel-plating process for the steel sheet.
一种均温板，包括依次设置的上盖板、毛细结构和下盖板，所述上盖板和所述下盖板之间形成封闭腔体，所述毛细结构设置在所述封闭腔体内；A temperature equalizing plate, comprising an upper cover plate, a capillary structure and a lower cover plate arranged in sequence, a closed cavity is formed between the upper cover plate and the lower cover plate, and the capillary structure is arranged in the closed cavity ;
所述上盖板和/或所述下盖板为上述的镀磷镍钢片。The upper cover plate and/or the lower cover plate is the above-mentioned phosphorus nickel-plated steel sheet.
有益效果beneficial effect
上述钢片化学镀镍工艺可以在镀镍钢片的镍层上形成高磷的磷镍层，从而得到镀磷镍钢片。该镀磷镍钢片在用作均热板的盖板时，磷镍层降低了镀磷镍钢片与水的反应，与表面覆盖铜层的钢片相比，这种镀磷镍钢片不会因为铜和钢材之间形成原电池而加速钢材与水的反应，从而使得这种镀磷镍钢片使用寿命可以延长约3倍-5倍。The above-mentioned electroless nickel plating process for the steel sheet can form a high phosphorus phosphorus-nickel layer on the nickel layer of the nickel-plated steel sheet, thereby obtaining a phosphorus-nickel-plated steel sheet. When the phosphorus-nickel-plated steel sheet is used as the cover plate of the soaking plate, the phosphorus-nickel layer reduces the reaction of the phosphorus-nickel-plated steel sheet with water. Compared with the steel sheet covered with a copper layer, the phosphorus-nickel-plated steel sheet has The reaction between steel and water will not be accelerated due to the formation of galvanic cells between copper and steel, so that the service life of the phosphorus-nickel-plated steel sheet can be extended by about 3 times to 5 times.
此外，通过该钢片化学镀镍工艺制备得到的镀磷镍钢片中，钢片、镍层和磷镍层之间的结合力好，总厚度可以不超过10μm，从而不会造成钢片厚度的增加。In addition, in the phosphorus-nickel-plated steel sheet prepared by the chemical nickel-plating process of the steel sheet, the bonding force between the steel sheet, the nickel layer and the phosphorus-nickel layer is good, and the total thickness can be no more than 10 μm, so that the thickness of the steel sheet will not be caused. increase.
进一步的，化学镀镍液中的乳酸、丁二酸、柠檬酸盐和乙酸兼顾缓冲和络合作用，浓度过低时镀速较慢、化学镀镍液稳定性差，化学镀镍液中易产生镍化合物沉淀、加速化学镀镍液分解，浓度过高时络合能力太强，反应效率低。Further, lactic acid, succinic acid, citrate and acetic acid in the electroless nickel plating solution take into account both buffering and complexation, and when the concentration is too low, the plating speed is slow, the stability of the electroless nickel plating solution is poor, and the electroless nickel plating solution is easy to produce. The nickel compound precipitates and accelerates the decomposition of the electroless nickel plating solution. When the concentration is too high, the complexing ability is too strong and the reaction efficiency is low.
附图说明Description of drawings
图1为一实施方式的钢片化学镀镍工艺的流程图。FIG. 1 is a flow chart of an electroless nickel plating process for a steel sheet according to an embodiment.
图2为如图1所示的钢片化学镀镍工艺的S20的具体流程图。FIG. 2 is a specific flow chart of S20 of the electroless nickel plating process on the steel sheet shown in FIG. 1 .
图3为一实施方式的均温板的立体结构示意图。FIG. 3 is a schematic three-dimensional structure diagram of a vapor chamber according to an embodiment.
图4为如图3所示的均温板的A-A向的剖面结构示意图。FIG. 4 is a schematic view of the cross-sectional structure of the vapor chamber shown in FIG. 3 along the A-A direction.
本发明的实施方式Embodiments of the present invention
下面结合附图和实施方式对本申请作进一步说明。The present application will be further described below with reference to the accompanying drawings and embodiments.
如图1所示的一实施方式的一种钢片化学镀镍工艺，包括如下步骤：A steel sheet electroless nickel plating process of an embodiment as shown in FIG. 1 includes the following steps:
S10、提供钢片。S10. Provide steel sheets.
优选的，钢片为不锈钢片。Preferably, the steel sheet is a stainless steel sheet.
具体来说，钢片的厚度可以为0.05mm-0.4mm。Specifically, the thickness of the steel sheet may be 0.05mm-0.4mm.
本实施方式中，钢片可以为普通的钢片，也可以为经过蚀刻处理后得到的具有蚀刻结构的钢片。In this embodiment, the steel sheet may be an ordinary steel sheet, or may be a steel sheet with an etched structure obtained after etching treatment.
S20、对S10得到的钢片进行预处理，得到预处理钢片。S20, preprocessing the steel sheet obtained in S10 to obtain a pretreated steel sheet.
一般来说，预处理通常包括除油处理、酸洗处理、活化处理等操作。Generally speaking, pretreatment usually includes operations such as degreasing treatment, pickling treatment, and activation treatment.
结合图2，具体来说，S20为：With reference to Figure 2, specifically, S20 is:
S21、将钢片浸泡在温度为70℃-80℃的除油液中20min-30min进行除油处理，完成后清洗干净得到第一预处理钢片。S21. Soak the steel sheet in a degreasing solution with a temperature of 70°C-80°C for 20min-30min to perform degreasing treatment, and clean it after completion to obtain a first pretreated steel sheet.
优选的，除油液包括10g/L-50g/L的氢氧化钠、10g/L-50g/L的碳酸钠以及1mL/L-5mL/L的OP乳化剂。Preferably, the degreasing liquid includes 10g/L-50g/L sodium hydroxide, 10g/L-50g/L sodium carbonate and 1mL/L-5mL/L OP emulsifier.
除油处理的目的为去除钢片表面油污，使钢片表面完全亲水。The purpose of degreasing treatment is to remove oil stains on the surface of the steel sheet and make the surface of the steel sheet completely hydrophilic.
除油液中的氢氧化钠和碳酸钠浓度过低时脱脂力度不够，难以将油污完全去除，影响形成的膜层的均匀性和结合力，导致表面发花、焊接不良等缺陷，浓度过高时润湿性差，且会对钢片造成损伤。When the concentration of sodium hydroxide and sodium carbonate in the degreasing solution is too low, the degreasing strength is insufficient, and it is difficult to completely remove the oil stain, which affects the uniformity and bonding force of the formed film layer, resulting in defects such as surface blooming and poor welding, and the concentration is too high. When the wettability is poor, it will cause damage to the steel sheet.
除油液中的OP乳化剂作为表面活性剂，提高其分散性和润湿性，有利于增强脱脂能力，过低时效果不佳，过高时易残留表面难以清洗。The OP emulsifier in the degreasing solution acts as a surfactant to improve its dispersibility and wettability, which is beneficial to enhance the degreasing ability. When it is too low, the effect is not good, and when it is too high, it is easy to remain on the surface and difficult to clean.
S21中，清洗干净的操作为采用纯水清洗干净。In S21, the cleaning operation is to use pure water to clean.
S22、将S21得到的第一预处理钢片浸泡在温度为20℃-40℃的酸洗液中1min-2min进行酸洗处理，完成后清洗干净得到第二预处理钢片。S22, soaking the first pretreated steel sheet obtained in S21 in a pickling solution with a temperature of 20°C-40°C for 1 min-2min for pickling treatment, and cleaning after completion to obtain a second pretreated steel sheet.
优选的，酸洗液包括体积分数为20%-30%的盐酸和3g/L-5g/L的若丁。Preferably, the pickling solution includes 20%-30% hydrochloric acid and 3g/L-5g/L rhodin in volume fraction.
酸洗处理的目的为去除钢片表面的氧化皮。The purpose of pickling treatment is to remove the oxide scale on the surface of the steel sheet.
盐酸对不锈钢氧化皮的清除能力较强，浓度过低时所需时间较长，效率低下，浓度过高时会导致表面过腐蚀，温度过高时也会加速腐蚀，因此酸洗处理的温度不宜高于40℃。Hydrochloric acid has a strong ability to remove stainless steel oxide scale. When the concentration is too low, it takes a long time and the efficiency is low. When the concentration is too high, the surface will be corroded, and the corrosion will be accelerated when the temperature is too high. Therefore, the temperature of the pickling treatment is not suitable. higher than 40°C.
为了避免过腐蚀、抑制酸雾，可在其中加入适量的若丁等缓蚀剂，缓蚀剂含量过低过高都会影响酸洗效率。In order to avoid over-corrosion and inhibit acid mist, an appropriate amount of corrosion inhibitor such as rhodin can be added to it. If the content of the inhibitor is too low or too high, the pickling efficiency will be affected.
S22中，清洗干净的操作为采用纯水清洗干净。In S22, the cleaning operation is to use pure water to clean.
S23、将S22得到的第二预处理钢片浸泡在温度为15℃-30℃的活化液中0.5min-1min进行活化处理，完成后清洗干净得到镀镍钢片。S23, soaking the second pretreated steel sheet obtained in S22 in an activation solution with a temperature of 15°C-30°C for 0.5min-1min for activation treatment, and cleaning after completion to obtain a nickel-plated steel sheet.
优选的，活化液包括体积分数为10%-20%的盐酸和5g/L-10g/L的乙酸。Preferably, the activation solution includes hydrochloric acid with a volume fraction of 10%-20% and acetic acid with a volume fraction of 5g/L-10g/L.
优选的，活化液的温度为20℃-25℃。Preferably, the temperature of the activation solution is 20°C-25°C.
活化处理的目的为提高钢片表面活性，保证化学镀镍层和钢片的结合力。活化液的酸度不宜过高时间不宜过长，因为经过酸洗后氧化层已经没有或很薄，酸度过高或时间过长会导致过腐蚀，影响钢片性能，最好保持在较低浓度（<20%）并辅以一定的乙酸，降低氯离子的侵蚀，但为了保证效果浓度也不宜过低（<10%），尤其当酸洗和化学镀镍之间停留时间较长时。The purpose of the activation treatment is to improve the surface activity of the steel sheet and ensure the bonding force between the electroless nickel plating layer and the steel sheet. The acidity of the activation solution should not be too high and the time should not be too long, because the oxide layer is no longer or very thin after pickling. Too high acidity or too long time will lead to over-corrosion and affect the performance of the steel sheet. It is best to keep it at a lower concentration ( <20%) and supplemented with a certain amount of acetic acid to reduce the corrosion of chloride ions, but the concentration should not be too low (<10%) to ensure the effect, especially when the residence time between pickling and electroless nickel plating is long.
具体来说，活化处理的温度可以为20℃或25℃。Specifically, the temperature of the activation treatment may be 20°C or 25°C.
S23中，清洗干净的操作为采用纯水冲洗干净，冲洗干净后得到的镀镍钢片快速浸泡到电镀镍的电镀液中以进行下一步反应。In S23, the cleaning operation is to use pure water to rinse, and the nickel-plated steel sheet obtained after the rinse is quickly immersed in an electroplating solution for electroplating nickel to carry out the next reaction.
S30、对S20得到的预处理钢片进行电镀镍，在预处理钢片上形成镍层，清洗干净后得到镀镍钢片。S30, performing nickel electroplating on the pretreated steel sheet obtained in S20, forming a nickel layer on the pretreated steel sheet, and cleaning to obtain a nickel-plated steel sheet.
电镀镍的操作是为了通过冲击镍的方式在预处理钢片表面形成一层薄薄的镍层，一方面提高化学镀形成的高磷的磷镍层的结合力，另一方面提高钢片表面化学镀的反应活性。The operation of nickel electroplating is to form a thin layer of nickel on the surface of the pretreated steel sheet by impacting nickel, on the one hand to improve the bonding force of the high phosphorus phosphorus-nickel layer formed by electroless plating, and on the other hand to improve the surface of the steel sheet. Reactivity of electroless plating.
具体来说，对预处理钢片进行电镀镍的操作中,阴极为预处理钢片，阳极为电解镍板，阴极电流密度5A/dm 2-10A/dm 2，电镀液包括200g/L-250g/L的氯化镍和100mL/L-120mL/L的盐酸，电镀时间为30s-1min。 Specifically, in the operation of electroplating nickel on the pretreated steel sheet, the cathode is the pretreated steel sheet, the anode is an electrolytic nickel plate, the cathode current density is 5A/dm 2 -10A/dm 2 , and the electroplating solution includes 200g/L-250g /L nickel chloride and 100mL/L-120mL/L hydrochloric acid, the plating time is 30s-1min.
冲击镍使用的电流密度应高于一般镀镍（2-5倍），目的是为了快速沉积一层结合力良好的薄镍层。The current density used for impact nickel should be higher than that of general nickel plating (2-5 times), the purpose is to quickly deposit a thin nickel layer with good bonding force.
优选的，对预处理钢片进行电镀镍的操作中,控制电镀液中氯化镍和盐酸的质量比为1.5-2.2：1。Preferably, in the operation of electroplating nickel on the pretreated steel sheet, the mass ratio of nickel chloride and hydrochloric acid in the electroplating solution is controlled to be 1.5-2.2:1.
在生产过程中保证氯化镍和盐酸的质量比在1.5-2.2之间，酸度不够会出现镀层结合力问题，主盐含量过低则可能导致镀速慢、镀层不均匀。In the production process, ensure that the mass ratio of nickel chloride and hydrochloric acid is between 1.5 and 2.2. If the acidity is not enough, there will be problems with the adhesion of the coating. If the content of the main salt is too low, the coating speed may be slow and the coating may be uneven.
S30中，清洗干净的操作为采用70℃-80℃的纯水冲洗干净。In S30, the cleaning operation is to rinse with pure water at 70°C-80°C.
S40、将S30得到的镀镍钢片浸泡在化学镀镍液中进行化学镀镍处理，完成后清洗干净并干燥，得到镀磷镍钢片。S40, soak the nickel-plated steel sheet obtained in S30 in an electroless nickel-plating solution for electroless nickel-plating treatment, clean and dry after completion, to obtain a phosphorus-nickel-plated steel sheet.
化学镀镍液包括20g/L-30g/L的镍盐、20g/L-30g/L的次磷酸盐、20g/L-25g/L的乳酸、5g/L-10g/L的丁二酸、0.5g/L-2g/L的柠檬酸盐以及5mL/L-10mL/L的乙酸，化学镀镍液的pH为4.4-4.8。Electroless nickel plating solution includes 20g/L-30g/L nickel salt, 20g/L-30g/L hypophosphite, 20g/L-25g/L lactic acid, 5g/L-10g/L succinic acid, 0.5g/L-2g/L citrate and 5mL/L-10mL/L acetic acid, the pH of electroless nickel plating solution is 4.4-4.8.
上述化学镀镍液可以用于镀镍钢片的化学镀镍，其目的为在镀镍钢片的镍层上形成一层高磷的高磷的磷镍层，从而得到镀磷镍钢片。The above-mentioned electroless nickel plating solution can be used for electroless nickel plating of nickel-plated steel sheets, and its purpose is to form a high-phosphorus high-phosphorus phosphorus-nickel layer on the nickel layer of nickel-plated steel sheets, thereby obtaining phosphorus-nickel-plated steel sheets.
该镀磷镍钢片在用作均热板的盖板时，磷镍层降低了镀磷镍钢片与水的反应，与表面覆盖铜层的钢片相比，这种镀磷镍钢片不会因为铜和钢材之间形成原电池而加速钢材与水的反应，从而使得这种镀磷镍钢片使用寿命可以延长约3倍-5倍。When the phosphorus-nickel-plated steel sheet is used as the cover plate of the soaking plate, the phosphorus-nickel layer reduces the reaction of the phosphorus-nickel-plated steel sheet with water. Compared with the steel sheet covered with a copper layer, the phosphorus-nickel-plated steel sheet has The reaction between steel and water will not be accelerated due to the formation of galvanic cells between copper and steel, so that the service life of the phosphorus-nickel-plated steel sheet can be extended by about 3 times to 5 times.
此外，通过该化学镀镍液制备得到的镀磷镍钢片中，钢片、镍层和磷镍层之间的结合力好，总厚度可以不超过10μm，从而不会造成钢片厚度的增加。In addition, in the phosphorus-nickel-plated steel sheet prepared by the chemical nickel plating solution, the bonding force between the steel sheet, the nickel layer and the phosphorus-nickel layer is good, and the total thickness can be no more than 10 μm, so that the thickness of the steel sheet will not be increased. .
进一步的，化学镀镍液中的乳酸、丁二酸、柠檬酸盐和乙酸兼顾缓冲和络合作用，浓度过低时镀速较慢、化学镀镍液稳定性差，化学镀镍液中易产生镍化合物沉淀、加速化学镀镍液分解，浓度过高时络合能力太强，反应效率低。Further, lactic acid, succinic acid, citrate and acetic acid in the electroless nickel plating solution take into account both buffering and complexation, and when the concentration is too low, the plating speed is slow, the stability of the electroless nickel plating solution is poor, and the electroless nickel plating solution is easy to produce. The nickel compound precipitates and accelerates the decomposition of the electroless nickel plating solution. When the concentration is too high, the complexing ability is too strong and the reaction efficiency is low.
显而易见的，镍盐、次磷酸盐和柠檬酸盐均为可以溶解在pH为4-6的钝化液中的物质。Obviously, nickel salts, hypophosphites and citrates are all substances that can be dissolved in the passivation solution at pH 4-6.
优选的，镍盐可以为硫酸镍或醋酸镍。Preferably, the nickel salt can be nickel sulfate or nickel acetate.
优选的，次磷酸盐可以为次磷酸钠或次磷酸钾。Preferably, the hypophosphite can be sodium hypophosphite or potassium hypophosphite.
优选的，柠檬酸盐可以为柠檬酸钠或柠檬酸钾。Preferably, the citrate can be sodium citrate or potassium citrate.
优选的，化学镀镍液还包括0.1mg/L-0.4mg/L的钼酸铵、0.5mg/L-1mg/L的氧化碲以及1mg/L-2mg/L的硫酸铜。Preferably, the electroless nickel plating solution further includes 0.1 mg/L-0.4 mg/L of ammonium molybdate, 0.5 mg/L-1 mg/L of tellurium oxide and 1 mg/L-2 mg/L of copper sulfate.
钼酸铵、氧化碲、硫酸铜的加入可提高镀液稳定性和化学镀效率，浓度低时稳定效果不佳，浓度高时影响反应活性。The addition of ammonium molybdate, tellurium oxide and copper sulfate can improve the stability of the plating solution and the efficiency of electroless plating. The stability effect is not good when the concentration is low, and the reactivity is affected when the concentration is high.
本实施方式中，化学镀镍液的pH通过氨水调节至4.4-4.8。In this embodiment, the pH of the electroless nickel plating solution is adjusted to 4.4-4.8 by ammonia water.
优选的，化学镀镍液还包括0.2g/L-1g/L的湿润剂。Preferably, the electroless nickel plating solution further includes 0.2g/L-1g/L of wetting agent.
具体来说，湿润剂可以为磺基丁二酸二己酯钠盐。Specifically, the humectant may be dihexyl sulfosuccinate sodium salt.
加入润湿剂是为了降低溶液表面张力，减少孔隙，0.21g/L-1g/L即可满足效果。The purpose of adding wetting agent is to reduce the surface tension of the solution and reduce the pores, and 0.21g/L-1g/L can satisfy the effect.
优选的，化学镀镍液还包括组合添加剂。Preferably, the electroless nickel plating solution further includes a combination of additives.
组合添加剂可以选自苯磺酸、烯丙基磺酸钠、丙炔醇乙氧基化合物、N,N-二乙基丙炔胺和磺基水杨酸中的至少两种。The combined additive may be selected from at least two of benzenesulfonic acid, sodium allylsulfonate, propargyl alcohol ethoxylate, N,N-diethylpropargylamine, and sulfosalicylic acid.
组合添加剂的作用是在化学镀过程中吸附在镀镍钢片的表面、降低镀层粗糙度，以期达到高耐蚀性的效果。The function of the combined additive is to adsorb on the surface of the nickel-plated steel sheet during the electroless plating process to reduce the roughness of the coating, in order to achieve the effect of high corrosion resistance.
优选的，将镀镍钢片浸泡在化学镀镍液中进行化学镀镍处理的操作中，化学镀镍液的温度为86℃-90℃，镀镍钢片的浸泡时间为60min-90min。Preferably, in the operation of immersing the nickel-plated steel sheet in an electroless nickel-plating solution for electroless nickel-plating treatment, the temperature of the electroless nickel-plating solution is 86°C-90°C, and the soaking time of the nickel-plated steel sheet is 60min-90min.
优选的，将镀镍钢片浸泡在化学镀镍液中进行化学镀镍处理的操作中，控制化学镀镍液中的镍离子和次磷酸根离子的摩尔比为0.3-0.45：1，这主要是为了保证化学镀镍液的稳定性和较高的镀速。Preferably, in the operation of immersing the nickel-plated steel sheet in the electroless nickel plating solution for electroless nickel plating treatment, the molar ratio of nickel ions and hypophosphite ions in the electroless nickel plating solution is controlled to be 0.3-0.45:1, which is mainly It is to ensure the stability of electroless nickel plating solution and high plating speed.
S40中，清洗干净并干燥的操作为纯水洗净后放入80℃-120℃下干燥。In S40, the operation of cleaning and drying is as follows: washing with pure water and then drying at 80°C-120°C.
本申请还公开了一种采用上述的钢片化学镀镍工艺制备得到镀磷镍钢片。The present application also discloses a phosphor-nickel-plated steel sheet prepared by using the above-mentioned chemical nickel-plating process for the steel sheet.
上述镀磷镍钢片可以应用于多种领域，化学镀镍层大大提高了镀磷镍钢片的耐腐蚀性和使用寿命。The above-mentioned phosphorus-nickel-plated steel sheet can be applied in various fields, and the electroless nickel-plated layer greatly improves the corrosion resistance and service life of the phosphorus-nickel-plated steel sheet.
下面仅以该镀磷镍钢片应用于均温板领域为例进行介绍。The following only takes the application of the phosphorus-nickel-plated steel sheet to the field of vapor chamber as an example for introduction.
结合图3和图4，本申请还公开了一实施方式的均温板100，包括依次设置的上盖板10、毛细结构20和下盖板30，上盖板10和下盖板30之间形成封闭腔体40，毛细结构20设置在封闭腔体40内。With reference to FIGS. 3 and 4 , the present application also discloses an embodiment of a uniform temperature plate 100 , which includes an upper cover plate 10 , a capillary structure 20 and a lower cover plate 30 arranged in sequence, and between the upper cover plate 10 and the lower cover plate 30 A closed cavity 40 is formed, and the capillary structure 20 is disposed in the closed cavity 40 .
上盖板10和/或下盖板30为上述的镀磷镍钢片。The upper cover plate 10 and/or the lower cover plate 30 are the above-mentioned phosphorus nickel-plated steel sheets.
镀磷镍钢片的化学镀镍层可以避免镀磷镍钢片作为均温板100的上盖板10和下盖板30在使用过程中会产生非凝结性气体，此外化学镀镍层还大大提高了镀磷镍钢片的耐腐蚀性和使用寿命。The electroless nickel plating layer of the phosphorus-nickel-plated steel sheet can avoid the non-condensable gas generated by the phosphorus-nickel-plated steel sheet as the upper cover plate 10 and the lower cover plate 30 of the vaporizing plate 100 during use. Improves corrosion resistance and service life of phosphorus-nickel-plated steel sheets.
具体来说，结合图3和图4，上盖板10的内壁为平面，下盖板30内壁上设有多个支撑柱32。Specifically, referring to FIGS. 3 and 4 , the inner wall of the upper cover plate 10 is flat, and the inner wall of the lower cover plate 30 is provided with a plurality of support columns 32 .
具体来说，毛细结构20设置在上盖板10的内壁。Specifically, the capillary structure 20 is disposed on the inner wall of the upper cover plate 10 .
优选的，毛细结构20的材料为为铜或者铜合金。Preferably, the material of the capillary structure 20 is copper or copper alloy.
具体来说，毛细结构20可采用金属丝编织、金属粉烧结、表面电化学沉积等方式得到。Specifically, the capillary structure 20 can be obtained by means of metal wire weaving, metal powder sintering, surface electrochemical deposition, and the like.
本实施方式的均温板100，通过将上盖板10和下盖板30焊接在一起后组装得到。The temperature equalizing plate 100 of this embodiment is assembled by welding the upper cover plate 10 and the lower cover plate 30 together.
以下为具体实施例。The following are specific examples.
实施例1Example 1
S10、通过对厚度在0.05-0.4mm之间的不锈钢片进行蚀刻，得到不锈钢盖板。S10, a stainless steel cover plate is obtained by etching a stainless steel sheet with a thickness of 0.05-0.4 mm.
S20、依次对不锈钢盖板进行除油处理、酸洗处理和活化处理。S20, performing degreasing treatment, pickling treatment and activation treatment on the stainless steel cover plate in sequence.
除油：将不锈钢盖板放入70℃的除油液中浸泡30min，而后立即用纯水清洗干净，除油液的成分为20g/L的氢氧化钠、30g/L的碳酸钠和3mL/L的OP乳化剂；Degreasing: Soak the stainless steel cover in a degreasing solution at 70°C for 30 minutes, and then rinse it off with pure water immediately. The degreasing solution consists of 20g/L sodium hydroxide, 30g/L sodium carbonate and 3mL/L L's OP emulsifier;
酸洗：在室温下将除油后的不锈钢盖板放入酸洗液中浸泡1min，而后立即用纯水清洗干净，酸洗液的成分为体积分数为20%的盐酸和3g/L的若丁；Pickling: soak the degreasing stainless steel cover in the pickling solution for 1 min at room temperature, and then immediately clean it with pure water. The components of the pickling solution are 20% hydrochloric acid and 3g/L Ding;
活化：在室温下将酸洗过的不锈钢盖板放入活化液中浸泡30s后取出，快速冲洗干净，立即入槽进行下一步骤，活化液为体积分数为10%的盐酸和5g/L的乙酸；Activation: soak the acid-washed stainless steel cover in the activation solution for 30s at room temperature, take it out, rinse it quickly, and immediately put it into the tank for the next step. The activation solution is 10% hydrochloric acid and 5g/L hydrochloric acid. acetic acid;
S30、电镀镍（冲击镍）处理：以活化后的不锈钢盖板作为阴极，纯度为99.99%的电解镍板为阳极，阴极电流密度8A/dm 2，电镀液包括240g/L的氯化镍和120mL/L的盐酸，电镀时间为30s，电镀完成后得到镀镍不锈钢盖板。 S30, electroplating nickel (impact nickel) treatment: the activated stainless steel cover plate is used as the cathode, the electrolytic nickel plate with a purity of 99.99% is used as the anode, the cathode current density is 8A/dm 2 , and the electroplating solution includes 240g/L nickel chloride and 120mL/L of hydrochloric acid, the electroplating time is 30s, and the nickel-plated stainless steel cover plate is obtained after the electroplating is completed.
S40、化学镀镍处理：将镀镍不锈钢盖板放入86℃的化学镀镍液中浸泡90min，纯水洗净后放入120℃烘箱中干燥20min，在镀镍不锈钢盖板形成一层高磷的磷镍层，得到镀磷镍不锈钢盖板。化学镀镍液的成分为硫酸镍25g/L、次磷酸钠20g/L、乳酸24g/L、丁二酸10g/L、柠檬酸钠1g/L、乙酸8mL/L、钼酸铵0.24mg/L、氧化碲1mg/L、硫酸铜2mg/L、磺基丁二酸二己酯钠盐0.5g/L、苯磺酸50mg/L、烯丙基磺酸钠20mg/L、丙炔醇乙氧基化合物20mg/L，用氨水调节溶液pH值为4.6。S40. Electroless nickel plating treatment: Soak the nickel-plated stainless steel cover in an electroless nickel plating solution at 86°C for 90 minutes, wash it with pure water, and place it in an oven at 120°C to dry for 20 minutes, forming a high layer on the nickel-plated stainless steel cover. The phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate. The composition of electroless nickel plating solution is nickel sulfate 25g/L, sodium hypophosphite 20g/L, lactic acid 24g/L, succinic acid 10g/L, sodium citrate 1g/L, acetic acid 8mL/L, ammonium molybdate 0.24mg/L L, tellurium oxide 1mg/L, copper sulfate 2mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, benzenesulfonic acid 50mg/L, sodium allyl sulfonate 20mg/L, propynyl alcohol ethyl Oxygen compound 20mg/L, the pH value of the solution was adjusted to 4.6 with ammonia water.
实施例2Example 2
实施例2中，S10、S20和S30与实施例1一致。In Embodiment 2, S10, S20 and S30 are the same as those in Embodiment 1.
S40、化学镀镍处理：将镀镍不锈钢盖板放入86℃的化学镀镍液中浸泡90min，纯水洗净后放入120℃烘箱中干燥20min，在镀镍不锈钢盖板形成一层高磷的磷镍层，得到镀磷镍不锈钢盖板。化学镀镍液的成分为硫酸镍25g/L、次磷酸钠24g/L、乳酸22g/L、丁二酸12g/L、柠檬酸钠1g/L、乙酸8mL/L、钼酸铵0.24mg/L、氧化碲1mg/L、硫酸铜2mg/L、磺基丁二酸二己酯钠盐0.5g/L、烯丙基磺酸钠30mg/L、丙炔醇乙氧基化合物20mg/L、N,N-二乙基丙炔胺5mg/L，用氨水调节溶液pH值为4.6。S40. Electroless nickel plating treatment: Soak the nickel-plated stainless steel cover in an electroless nickel plating solution at 86°C for 90 minutes, wash it with pure water, and place it in an oven at 120°C to dry for 20 minutes, forming a high layer on the nickel-plated stainless steel cover. The phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate. The composition of electroless nickel plating solution is nickel sulfate 25g/L, sodium hypophosphite 24g/L, lactic acid 22g/L, succinic acid 12g/L, sodium citrate 1g/L, acetic acid 8mL/L, ammonium molybdate 0.24mg/L L, tellurium oxide 1mg/L, copper sulfate 2mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, allyl sodium sulfonate 30mg/L, propynyl alcohol ethoxylate 20mg/L, N,N-diethylpropargylamine 5mg/L, the pH value of the solution was adjusted to 4.6 with ammonia water.
实施例3Example 3
实施例3中，S10、S20和S30与实施例1一致。In Embodiment 3, S10, S20 and S30 are the same as those in Embodiment 1.
S40、化学镀镍处理：将镀镍不锈钢盖板放入86℃的化学镀镍液中浸泡90min，纯水洗净后放入120℃烘箱中干燥20min，在镀镍不锈钢盖板形成一层高磷的磷镍层，得到镀磷镍不锈钢盖板。化学镀镍液的成分为硫酸镍26g/L、次磷酸钠22g/L、乳酸24g/L、丁二酸10g/L、柠檬酸钠1.5g/L、乙酸8mL/L、钼酸铵0.2mg/L、氧化碲1mg/L、硫酸铜2mg/L、磺基丁二酸二己酯钠盐0.5g/L、烯丙基磺酸钠30mg/L、丙炔醇乙氧基化合物10mg/L、N,N-二乙基丙炔胺15mg/L，用氨水调节溶液pH值为4.6。S40. Electroless nickel plating treatment: Soak the nickel-plated stainless steel cover in an electroless nickel plating solution at 86°C for 90 minutes, wash it with pure water, and place it in an oven at 120°C to dry for 20 minutes, forming a high layer of nickel-plated stainless steel cover. The phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate. The composition of electroless nickel plating solution is nickel sulfate 26g/L, sodium hypophosphite 22g/L, lactic acid 24g/L, succinic acid 10g/L, sodium citrate 1.5g/L, acetic acid 8mL/L, ammonium molybdate 0.2mg /L, tellurium oxide 1mg/L, copper sulfate 2mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, allyl sodium sulfonate 30mg/L, propargyl alcohol ethoxylate 10mg/L , N,N-diethylpropargylamine 15mg/L, and the pH value of the solution was adjusted to 4.6 with ammonia water.
实施例4Example 4
实施例4中，S10、S20和S30与实施例1一致。In Embodiment 4, S10, S20 and S30 are the same as those in Embodiment 1.
S40、化学镀镍处理：将镀镍不锈钢盖板放入90℃的化学镀镍液中浸泡60min，纯水洗净后放入120℃烘箱中干燥20min，在镀镍不锈钢盖板形成一层高磷的磷镍层，得到镀磷镍不锈钢盖板。化学镀镍液的成分为醋酸镍24g/L、次磷酸钠20g/L、乳酸22g/L、丁二酸10g/L、柠檬酸钠1g/L、乙酸8mL/L、钼酸铵0.18mg/L、氧化碲1mg/L、硫酸铜2mg/L、磺基丁二酸二己酯钠盐0.5g/L、磺基水杨酸30mg/L、丙炔醇乙氧基化合物20mg/L、苯磺酸10mg/L，用氨水调节溶液pH值为4.4。S40. Electroless nickel plating treatment: Soak the nickel-plated stainless steel cover plate in an electroless nickel plating solution at 90°C for 60 minutes, wash it with pure water, and put it in an oven at 120°C to dry for 20 minutes. A layer of high-grade nickel-plated stainless steel cover plate is formed. The phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate. The composition of electroless nickel plating solution is nickel acetate 24g/L, sodium hypophosphite 20g/L, lactic acid 22g/L, succinic acid 10g/L, sodium citrate 1g/L, acetic acid 8mL/L, ammonium molybdate 0.18mg/L L, tellurium oxide 1mg/L, copper sulfate 2mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, sulfosalicylic acid 30mg/L, propargyl alcohol ethoxylate 20mg/L, benzene Sulfonic acid was 10 mg/L, and the pH value of the solution was adjusted to 4.4 with ammonia water.
实施例5Example 5
实施例5中，S10、S20和S30与实施例1一致。In Embodiment 5, S10, S20 and S30 are the same as those in Embodiment 1.
S40、化学镀镍处理：将镀镍不锈钢盖板放入88℃的化学镀镍液中浸泡70min，纯水洗净后放入120℃烘箱中干燥20min，在镀镍不锈钢盖板形成一层高磷的磷镍层，得到镀磷镍不锈钢盖板。化学镀镍液的成分为硫酸镍28g/L、次磷酸钠30g/L、乳酸25g/L、丁二酸10g/L、柠檬酸钠2g/L、乙酸6mL/L、钼酸铵0.3mg/L、氧化碲1mg/L、硫酸铜1.5mg/L、磺基丁二酸二己酯钠盐0.5g/L、磺基水杨酸30mg/L、N,N-二乙基丙炔胺10mg/L、苯磺酸20mg/L，用氨水调节溶液pH值为4.8。S40. Electroless nickel plating treatment: Soak the nickel-plated stainless steel cover in an electroless nickel plating solution at 88°C for 70 minutes, rinse with pure water, and place it in an oven at 120°C to dry for 20 minutes. A layer of high layer is formed on the nickel-plated stainless steel cover. The phosphorus-nickel layer of phosphorus is obtained to obtain a phosphorus-nickel-plated stainless steel cover plate. The composition of electroless nickel plating solution is nickel sulfate 28g/L, sodium hypophosphite 30g/L, lactic acid 25g/L, succinic acid 10g/L, sodium citrate 2g/L, acetic acid 6mL/L, ammonium molybdate 0.3mg/L L, tellurium oxide 1mg/L, copper sulfate 1.5mg/L, dihexyl sulfosuccinate sodium salt 0.5g/L, sulfosalicylic acid 30mg/L, N,N-diethylpropynamide 10mg /L, benzenesulfonic acid 20mg/L, and the pH value of the solution was adjusted to 4.8 with ammonia water.
以下对上述实施例1-5制得的不锈钢盖板进行了性能测试：The performance test of the stainless steel cover plates prepared in the above-mentioned embodiments 1-5 was carried out below:
1、镀层结合力：镀层结合力的表征采用的是阴极试验法，将镀覆后的钢片放在5%的氢氧化钠溶液中作为阴极，不锈钢为阳极，操作温度为90°，使用10A/dm 2的电流进行15min的电解处理，结合力差的镀层在处理后会形成许多气泡，与钢片分离。 1. Coating adhesion: The cathode test method is used to characterize the coating adhesion. The coated steel sheet is placed in a 5% sodium hydroxide solution as the cathode, and the stainless steel is used as the anode. The operating temperature is 90° and 10A is used. /dm 2 current for 15min electrolytic treatment, the coating with poor adhesion will form many bubbles after treatment and separate from the steel sheet.
实施例1-实施例5制得的镀磷镍不锈钢盖板的磷镍镀层在上述电解处理后并未产生起泡现象，说明该镀层与钢片结合紧密。The phosphorus-nickel coating of the phosphorus-nickel-plated stainless steel cover plates prepared in Example 1-Example 5 did not produce bubbling after the above electrolytic treatment, indicating that the coating was closely combined with the steel sheet.
2、镀层厚度和磷含量：实施例1-实施例5制得的镀磷镍不锈钢盖板的镀层厚度和磷含量是由X射线荧光膜厚仪测量得到，具体测试结果如下标1所示。2. Coating thickness and phosphorus content: The coating thickness and phosphorus content of the phosphorus-plated nickel stainless steel cover plates prepared in Examples 1-5 were measured by an X-ray fluorescence film thickness meter. The specific test results are shown in the following standard 1.
Figure 624196dest_path_image001
Figure 624196dest_path_image001
由上表1可以看出，实施例1-实施例5制得的镀磷镍不锈钢盖板的镀层厚度均低于10μm，且镀层的磷含量在11%-14%之间。It can be seen from the above Table 1 that the thickness of the plating layer of the phosphorus-nickel-plated stainless steel cover plates prepared in Examples 1 to 5 is all less than 10 μm, and the phosphorus content of the plating layer is between 11% and 14%.
3、均温板老化试验：3. Aging test of uniform temperature plate:
将实施例1-实施例5制得的镀磷镍不锈钢盖板和未处理的不锈钢盖板一起放入100℃老化试验箱中，通过跟踪测量不锈钢盖板两端之间的温差，可模拟出常规环境中二者的性能差异。Put the phosphorus-nickel-plated stainless steel cover plates prepared in Example 1-Example 5 together with the untreated stainless steel cover plate into a 100 ℃ aging test box, and by tracking and measuring the temperature difference between the two ends of the stainless steel cover plate, it can be simulated. The performance difference between the two in a normal environment.
通过老化试验测得，实施例1-实施例5制得的镀磷镍不锈钢盖板在96h后温差均能保持在10℃以内，与未处理的不锈钢盖板（24h-30h后温差大于10℃）相比，使用寿命可提升3倍以上。According to the aging test, the temperature difference between the phosphorus-nickel-plated stainless steel cover plates prepared in Examples 1 to 5 can be kept within 10°C after 96h, and the temperature difference from the untreated stainless steel cover plates (after 24h-30h is greater than 10°C) ), the service life can be increased by more than 3 times.
以上所述的仅是本申请的实施方式，在此应当指出，对于本领域的普通技术人员来说，在不脱离本申请创造构思的前提下，还可以做出改进，但这些均属于本申请的保护范围。The above are only the embodiments of the present application. It should be pointed out that for those of ordinary skill in the art, improvements can be made without departing from the creative concept of the present application, but these belong to the present application. scope of protection.

Claims (13)

  1. 一种钢片化学镀镍工艺，其特征在于，包括如下步骤：A steel sheet chemical nickel plating process is characterized in that, comprises the following steps:
    提供钢片；provide steel sheets;
    对所述钢片进行预处理，得到预处理钢片；The steel sheet is pretreated to obtain a pretreated steel sheet;
    对所述预处理钢片进行电镀镍，在所述预处理钢片上形成镍层，清洗干净后得到镀镍钢片；以及The pretreated steel sheet is electroplated with nickel, a nickel layer is formed on the pretreated steel sheet, and the nickel-plated steel sheet is obtained after cleaning; and
    将所述镀镍钢片浸泡在化学镀镍液中进行化学镀镍处理，在所述镍层上形成磷镍层，清洗干净并干燥后得到镀磷镍钢片，其中，所述化学镀镍液包括20g/L-30g/L的镍盐、20g/L-30g/L的次磷酸盐、20g/L-25g/L的乳酸、5g/L-10g/L的丁二酸、0.5g/L-2g/L的柠檬酸盐以及5mL/L-10mL/L的乙酸，所述化学镀镍液的pH为4.4-4.8。The nickel-plated steel sheet is immersed in an electroless nickel plating solution for chemical nickel-plating treatment, a phosphorus-nickel layer is formed on the nickel layer, cleaned and dried to obtain a phosphorus-nickel-plated steel sheet, wherein the chemical nickel-plated steel sheet is The liquid includes 20g/L-30g/L nickel salt, 20g/L-30g/L hypophosphite, 20g/L-25g/L lactic acid, 5g/L-10g/L succinic acid, 0.5g/L-10g/L L-2g/L citrate and 5mL/L-10mL/L acetic acid, the pH of the electroless nickel plating solution is 4.4-4.8.
  2. 根据权利要求1所述的钢片化学镀镍工艺，其特征在于，所述镍盐为硫酸镍或醋酸镍；The steel sheet electroless nickel plating process according to claim 1, wherein the nickel salt is nickel sulfate or nickel acetate;
    所述次磷酸盐为次磷酸钠或次磷酸钾；Described hypophosphite is sodium hypophosphite or potassium hypophosphite;
    所述柠檬酸盐为柠檬酸钠或柠檬酸钾。The citrate is sodium citrate or potassium citrate.
  3. 根据权利要求1所述的钢片化学镀镍工艺，其特征在于，所述化学镀镍液还包括0.1mg/L-0.4mg/L的钼酸铵、0.5mg/L-1mg/L的氧化碲以及1mg/L-2mg/L的硫酸铜。The steel sheet electroless nickel plating process according to claim 1, wherein the electroless nickel plating solution further comprises 0.1mg/L-0.4mg/L ammonium molybdate, 0.5mg/L-1mg/L oxidizing agent Tellurium and 1mg/L-2mg/L of copper sulfate.
  4. 根据权利要求3所述的钢片化学镀镍工艺，其特征在于，所述化学镀镍液的pH通过氨水调节至4.4-4.8。The electroless nickel plating process for steel sheets according to claim 3, wherein the pH of the electroless nickel plating solution is adjusted to 4.4-4.8 by ammonia water.
  5. 根据权利要求3所述的钢片化学镀镍工艺，其特征在于，所述化学镀镍液还包括0.2g/L-1g/L的湿润剂。The electroless nickel plating process for steel sheets according to claim 3, wherein the electroless nickel plating solution further comprises a wetting agent of 0.2g/L-1g/L.
  6. 根据权利要求5所述的钢片化学镀镍工艺，其特征在于，所述化学镀镍液还包括组合添加剂，所述组合添加剂选自苯磺酸、烯丙基磺酸钠、丙炔醇乙氧基化合物、N,N-二乙基丙炔胺和磺基水杨酸中的至少两种。The electroless nickel plating process for steel sheets according to claim 5, wherein the electroless nickel plating solution further comprises a combination additive selected from the group consisting of benzenesulfonic acid, sodium allylsulfonate, propargyl alcohol ethyl At least two of an oxy compound, N,N-diethylpropargylamine, and sulfosalicylic acid.
  7. 根据权利要求1-6中任意一项所述的钢片化学镀镍工艺，其特征在于，将所述镀镍钢片浸泡在化学镀镍液中进行化学镀镍处理的操作中，所述化学镀镍液的温度为86℃-90℃，所述镀镍钢片的浸泡时间为60min-90min。The electroless nickel plating process for a steel sheet according to any one of claims 1 to 6, wherein in the operation of immersing the nickel-plated steel sheet in an electroless nickel plating solution for electroless nickel plating, the chemical The temperature of the nickel plating solution is 86°C-90°C, and the soaking time of the nickel-plated steel sheet is 60min-90min.
  8. 根据权利要求1-6中任意一项所述的钢片化学镀镍工艺，其特征在于，将所述镀镍钢片浸泡在所述化学镀镍液中进行化学镀镍处理的操作中，控制所述化学镀镍液中的镍离子和次磷酸根离子的摩尔比为0.3-0.45：1。The electroless nickel plating process for steel sheets according to any one of claims 1 to 6, characterized in that, in the operation of immersing the nickel-plated steel sheets in the electroless nickel plating solution for electroless nickel plating, controlling The molar ratio of nickel ions and hypophosphite ions in the electroless nickel plating solution is 0.3-0.45:1.
  9. 根据权利要求1-6中任意一项所述的钢片化学镀镍工艺，其特征在于，对所述预处理钢片进行电镀镍的操作中,阴极为所述预处理钢片，阳极为电解镍板，阴极电流密度5A/dm 2-10A/dm 2，电镀液包括200g/L-250g/L的氯化镍和100mL/L-120mL/L的盐酸，电镀时间为30s-1min。 The electroless nickel plating process for steel sheets according to any one of claims 1-6, wherein in the operation of electroplating nickel on the pretreated steel sheets, the cathode is the pretreated steel sheet, and the anode is an electrolytic Nickel plate, the cathode current density is 5A/dm 2 -10A/dm 2 , the electroplating solution includes 200g/L-250g/L nickel chloride and 100mL/L-120mL/L hydrochloric acid, and the electroplating time is 30s-1min.
  10. 根据权利要求9所述的钢片化学镀镍工艺，其特征在于，对所述预处理钢片进行电镀镍的操作中,控制所述电镀液中所述氯化镍和所述盐酸的质量比为1.5-2.2：1。The electroless nickel plating process for steel sheets according to claim 9, wherein in the operation of electroplating nickel on the pretreated steel sheets, the mass ratio of the nickel chloride and the hydrochloric acid in the electroplating solution is controlled. 1.5-2.2:1.
  11. 根据权利要求1所述的钢片化学镀镍工艺，其特征在于，对所述钢片进行预处理，得到预处理钢片的操作为：The steel sheet electroless nickel plating process according to claim 1, wherein the steel sheet is pretreated, and the operation of obtaining the pretreated steel sheet is:
    将所述钢片浸泡在温度为70℃-80℃的除油液中20min-30min进行除油处理，完成后清洗干净得到第一预处理钢片，其中，所述除油液包括10g/L-50g/L的氢氧化钠、10g/L-50g/L的碳酸钠以及1mL/L-5mL/L的OP乳化剂；Soak the steel sheet in a degreasing solution with a temperature of 70°C-80°C for 20min-30min to perform degreasing treatment, and clean it after completion to obtain a first pretreated steel sheet, wherein the degreasing solution comprises 10g/L -50g/L sodium hydroxide, 10g/L-50g/L sodium carbonate and 1mL/L-5mL/L OP emulsifier;
    将所述第一预处理钢片浸泡在温度为20℃-40℃的酸洗液中1min-2min进行酸洗处理，完成后清洗干净得到第二预处理钢片，其中，所述酸洗液包括体积分数为20%-30%的盐酸和3g/L-5g/L的若丁；以及The first pretreated steel sheet is immersed in a pickling solution with a temperature of 20°C-40°C for 1min-2min to perform pickling treatment, and after completion, cleaning is performed to obtain a second pretreated steel sheet, wherein the pickling solution Including 20%-30% hydrochloric acid and 3g/L-5g/L rhodine; and
    将所述第二预处理钢片浸泡在温度为15℃-30℃的活化液中0.5min-1min进行活化处理，完成后清洗干净得到所述预处理钢片，其中，所述活化液包括体积分数为10%-20%的盐酸和5g/L-10g/L的乙酸。The second pretreated steel sheet is immersed in an activation solution with a temperature of 15°C-30°C for 0.5min-1min for activation treatment, and after completion, cleaning is performed to obtain the pretreated steel sheet, wherein the activation solution includes a volume of The fractions are 10%-20% hydrochloric acid and 5g/L-10g/L acetic acid.
  12. 一种镀磷镍钢片，其特征在于，所述镀磷镍钢片采用如权利要求1-11中任意一项所述的钢片化学镀镍工艺制备得到。A phosphorus-nickel-coated steel sheet, characterized in that, the phosphorus-nickel-coated steel sheet is prepared by the chemical nickel-plating process for a steel sheet according to any one of claims 1-11.
  13. 一种均温板，其特征在于，包括依次设置的上盖板、毛细结构和下盖板，所述上盖板和所述下盖板之间形成封闭腔体，所述毛细结构设置在所述封闭腔体内；A temperature equalizing plate is characterized in that it comprises an upper cover plate, a capillary structure and a lower cover plate arranged in sequence, a closed cavity is formed between the upper cover plate and the lower cover plate, and the capillary structure is arranged in the inside the closed cavity;
    所述上盖板和/或所述下盖板为如权利要求12所述的镀磷镍钢片。The upper cover plate and/or the lower cover plate is the phosphorus nickel plated steel sheet according to claim 12 .
PCT/CN2020/126623 2020-10-28 2020-11-05 Chemical nickel-plating process for steel sheet, phosphorus-nickel-plated steel sheet and vapor chamber WO2022088216A1 (en)

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