WO2022110339A1 - 钢片钝化工艺、钝化钢片以及均温板 - Google Patents

钢片钝化工艺、钝化钢片以及均温板 Download PDF

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Publication number
WO2022110339A1
WO2022110339A1 PCT/CN2020/136357 CN2020136357W WO2022110339A1 WO 2022110339 A1 WO2022110339 A1 WO 2022110339A1 CN 2020136357 W CN2020136357 W CN 2020136357W WO 2022110339 A1 WO2022110339 A1 WO 2022110339A1
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Prior art keywords
steel sheet
passivation
solution
cover plate
pretreated
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PCT/CN2020/136357
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English (en)
French (fr)
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 WO2022110339A1 publication Critical patent/WO2022110339A1/zh

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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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/50—Treatment of iron or alloys based thereon
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/78—Pretreatment of the material to be coated
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/19—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

Definitions

  • the invention relates to the technical field of heat-dissipating components, in particular to a steel sheet passivation process, a passivation steel sheet prepared by the steel sheet passivation process, and a temperature equalizing plate comprising the passivation 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 or copper alloys, and the material strength and supporting effect are insufficient, making it difficult to ultra-thin.
  • steel 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.
  • 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.
  • the passivated steel sheet prepared by the steel sheet passivation process has a longer service life when used as a cover plate of a soaking plate.
  • a steel sheet passivation process comprising the following steps:
  • the steel sheet is pretreated to obtain a pretreated steel sheet
  • the pretreated steel sheet is immersed in the above-mentioned passivation solution for passivation treatment, cleaned and dried after completion to obtain a passivation steel sheet, wherein the passivation solution comprises 5g/L-10g/L containing Nitrogen or sulfur-containing benzene ring organic matter and 0.5g/L-5g/L inorganic matter, the inorganic matter is silicate, rare earth compound or transition metal compound, the pH of the passivation solution is 4-6 aqueous solution.
  • the nitrogen- or sulfur-containing benzene ring organic compound is benzotriazole, diaminotriazepine or naphthalenesulfonic acid.
  • the silicate is sodium silicate or potassium silicate;
  • the rare earth compound is rare earth nitrate, rare earth hydrochloride or rare earth sulfate;
  • the transition metal compound is transition metal nitrate, transition metal hydrochloride salt or transition metal sulfate.
  • the passivation solution further includes 5g/L-10g/L weak acid and 0.5g/L-2g/L surfactant.
  • the weak acid is sulfosalicylic acid, tannic acid or gallic acid.
  • the surfactant is polyvinyl alcohol, polyethylene glycol 400-1000 or fatty alcohol polyoxyethylene ether.
  • the temperature of the passivation solution is 40°C-70°C
  • the soaking time of the pretreated steel sheet is 5min-70°C 30min.
  • the steel sheet is pretreated to obtain the pretreated steel sheet as follows:
  • 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;
  • 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
  • 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.
  • a passivation steel sheet is prepared by adopting the above-mentioned steel sheet passivation process.
  • a temperature equalizing plate comprising an upper cover plate, a capillary structure and a lower cover plate arranged in sequence, a closed cavity for storing a cooling medium is formed between the upper cover plate and the lower cover plate, and the capillary structure is arranged within the closed cavity;
  • the upper cover plate and/or the lower cover plate are the above-mentioned passivated steel sheets.
  • a plurality of support columns protruding and extending toward the upper cover plate are provided on the inner wall of the lower cover plate close to the upper cover plate.
  • the capillary structure is disposed on the inner wall of the upper cover plate on the side close to the lower cover plate, and the support column abuts against the capillary structure.
  • the capillary structure is formed in the closed cavity by metal wire weaving, metal powder sintering or surface electrochemical deposition.
  • the passivation solution of the above-mentioned steel sheet passivation process contains two types of benzene ring-based organic substances and inorganic substances, and the passivation film formed on the passivation steel sheet prepared by the steel sheet passivation process is composed of carbon chains and inorganic oxides. the composite film.
  • the passivation steel sheet is used as the cover plate of the soaking plate, the passivation film formed on the passivation steel sheet reduces the reaction between the passivation steel sheet and water.
  • the chemical steel sheet will not accelerate the reaction between steel and water due to the formation of galvanic cells between copper and steel, so that the service life of the passivated steel sheet can be extended by about 2 times to 7 times.
  • the passivation film of the passivation steel sheet prepared by the passivation process of the steel sheet has compactness, good bonding force and strong corrosion resistance, and the thickness of the passivation film is between 10 nm and 100 nm, so that the steel sheet will not be damaged. increase in thickness.
  • FIG. 1 is a flow chart of a steel sheet passivation process according to an embodiment.
  • FIG. 2 is a specific flow chart of S20 of the steel sheet passivation process 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.
  • FIG. 5 is a schematic diagram of the explosion structure of the vapor chamber shown in FIG. 3 .
  • a steel sheet passivation 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 purpose of the activation treatment is to improve the surface activity of the steel sheet and ensure the bonding force between the passivation 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 passivation is long.
  • the temperature of the activation treatment may be 20°C or 25°C.
  • the cleaning operation is to rinse with pure water, and the pretreated steel sheet obtained after rinsing is quickly immersed in a passivation solution for the next reaction.
  • the pH of the passivation solution is an aqueous solution of 4-6.
  • the passivation solution includes 5g/L-10g/L nitrogen-containing or sulfur-containing benzene ring organics, 0.5g/L-5g/L inorganic substances and 5g/L -10g/L weak acid.
  • the inorganic substances are silicates, rare earth compounds or transition metal compounds.
  • passivation treatment is to form a passivation film on the surface of the steel sheet, thereby obtaining a passivated steel sheet.
  • the passivation solution includes two types of benzene ring-based organic substances and inorganic substances, so that the passivation film formed on the passivation steel sheet is a composite film layer including carbon chains and inorganic oxides.
  • Inorganic substances are not only used as auxiliary film-forming substances, but also as pore fillers to enhance the compactness of passivation films.
  • Nitrogen-containing or sulfur-containing benzene ring organics can be adsorbed on the surface of the steel sheet or form an organic film on the surface in the form of chelation. The concentration is too high and the solubility is poor. When the concentration is too low, the film-forming reaction is slow.
  • the dosage is 5g/L -10g/L is suitable, and it is difficult to form a composite film after the surface of the steel sheet is occupied by an inorganic film.
  • the passivation film formed on the passivation steel sheet reduces the reaction between the passivation steel sheet and water, and the surface is covered with the copper layer. Compared with steel sheet, this passivated steel sheet will not accelerate the reaction between steel and water due to the formation of galvanic cells between copper and steel, so that the service life of this passivated steel sheet can be extended by about 2 times to 7 times.
  • the passivation film of the passivation steel sheet prepared by the above-mentioned passivation process of the steel sheet has compactness, good bonding force and strong corrosion resistance, and the thickness of the passivation film is between 10 nm and 100 nm, so that the thickness of the steel sheet is not caused. increase.
  • the nitrogen- or sulfur-containing benzene ring organic compound is benzotriazole, diaminotriazepine or naphthalenesulfonic acid.
  • the above organic molecules all have highly electronegative elements such as nitrogen or sulfur, and have strong surface activity and adsorption capacity. It can be adsorbed on the surface of the steel sheet or form an organic film on the surface in the form of chelation.
  • inorganic substances are substances that can be dissolved in a passivation solution with a pH of 4-6.
  • the silicate can be sodium silicate or potassium silicate;
  • the rare earth compound can be rare earth nitrate, rare earth hydrochloride or rare earth sulfate;
  • the transition metal compound can be transition metal nitrate, transition metal hydrochloride or transition metal metal sulfate.
  • the passivation solution further includes 5g/L-10g/L weak acid and 0.5g/L-2g/L surfactant.
  • the weak acid can be sulfosalicylic acid, tannic acid or gallic acid, and the above weak acids are all hydroxycarboxylic acids with a benzene ring and have strong coordination ability.
  • the surfactant can be polyvinyl alcohol, polyethylene glycol 400-1000 or fatty alcohol polyoxyethylene ether. These surfactants are all non-ionic surfactants with strong wetting and dispersing properties.
  • the fatty alcohol polyoxyethylene may be lauryl polyoxyethylene ether.
  • the temperature of the passivation solution is 40°C-70°C, and the soaking time of the pretreated steel sheet is 5min-30min.
  • the invention also discloses a passivation steel sheet prepared by adopting the above-mentioned steel sheet passivation process.
  • the above passivation steel sheet can be applied in various fields, and the passivation layer greatly improves the corrosion resistance and service life of the passivation steel sheet.
  • the present invention also discloses a uniform temperature plate 100 in an embodiment, including 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 for storing the cooling medium is formed, and the capillary structure 20 is arranged in the closed cavity 40 .
  • the upper cover plate 10 and/or the lower cover plate 30 are the above-mentioned passivated steel sheets.
  • the passivation layer of the passivation steel sheet can avoid the generation of non-condensable gas during the use of the passivation steel sheet as the upper cover plate 10 and the lower cover plate 30 of the uniform temperature plate 100, and the passivation layer also greatly improves the passivation. Corrosion resistance and service life of steel sheets.
  • the inner wall of the upper cover 10 is flat, and the inner wall of the lower cover 30 close to the upper cover 10 is provided with a plurality of support columns 32 that protrude and extend from the upper cover 10 .
  • the support columns 32 disposed on the lower cover 30 may be arranged in an array.
  • the capillary structure 20 is disposed on the inner wall of the upper cover plate 10 .
  • the capillary structure 20 is disposed on the inner wall of the upper cover plate 10 on the side close to the lower cover plate 30 , and the support column 32 abuts against the capillary structure 20 .
  • the material of the capillary structure 20 is copper or copper alloy.
  • the capillary structure 20 may be formed in the closed cavity 40 by wire weaving, metal powder sintering, surface electrochemical deposition, or 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 80°C for 30 minutes, and then rinse it off with pure water immediately.
  • the degreasing solution consists of 20g/L sodium hydroxide, 20g/L sodium carbonate and 4mL/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;
  • Passivation treatment soak the activated stainless steel cover in a passivation solution at 45°C for 10 minutes, wash it with pure water and put it in an oven at 80°C to dry for 20 minutes to form a passivation film on the surface of the stainless steel cover , to obtain a passivation stainless steel cover plate, the composition of the passivation solution is 5g/L benzotriazole, 5g/L sodium silicate, 10g/L sulfosalicylic acid and 0.5g/L polyvinyl alcohol , the pH of the passivation solution is 4.
  • Embodiment 2 S10 and S20 are the same as those in Embodiment 1.
  • Passivation treatment soak the activated stainless steel cover in a passivation solution at 70°C for 30 minutes, wash it with pure water, and put it in an oven at 80°C to dry for 20 minutes to form a passivation film on the surface of the stainless steel cover , to obtain a passivation stainless steel cover plate, the composition of the passivation solution is 7g/L benzotriazole, 0.5g/L cerium nitrate, 5g/L sulfosalicylic acid and 2g/L polyvinyl alcohol, The pH of the passivation solution is 6.
  • Embodiment 3 S10 and S20 are the same as those in Embodiment 1.
  • Passivation treatment Soak the activated stainless steel cover in a passivation solution at 45°C for 10 minutes, wash it with pure water, and put it into an oven at 80°C to dry for 15 minutes to form a passivation film on the surface of the stainless steel cover , to obtain a passivation stainless steel cover plate, the composition of the passivation solution is 10g/L of benzotriazole, 3g/L of zinc sulfate, 8g/L of sulfosalicylic acid and 1g/L of polyvinyl alcohol, passivation The pH of the solution was 4.8.
  • the binding force test of the passive film and the steel sheet and the pitting corrosion resistance test are carried out on the passivation stainless steel cover plate of the above-mentioned embodiment 1-3
  • the bonding force between the passivation film and the steel sheet was evaluated by the combination of the cathode test and the corrosion resistance test.
  • the passivated stainless steel cover plates prepared in Examples 1-3 were placed in 5% sodium hydroxide solution as Cathode, stainless steel is the anode, the operating temperature is 90°, and the current of 10A/dm 2 is used for 15min electrolytic treatment.
  • the passive film with poor adhesion will peel off and fall off from the steel sheet after treatment, resulting in subsequent pitting corrosion resistance. A blue dot appears quickly during the test (usually within 5 minutes).
  • the pitting corrosion resistance test uses a mixture of potassium ferricyanide (10g/L) and sodium chloride (20g/L), drop the solution on the surface of the sample to be tested with a dropper, and collect the time when the color becomes completely transparent as A characterization of pitting resistance.
  • the composite passivation film greatly improves the corrosion resistance of the steel sheet, so that the iron element that is easily eroded by water vapor is completely covered, which is beneficial to inhibit the iron-water reaction and the interaction between iron and copper.
  • the galvanic cell reacts, thereby increasing the service life of the vapor chamber.
  • the service life of the passivated stainless steel cover prepared in Examples 1-3 can be extended by about 2 to 7 times.

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Abstract

一种钢片钝化工艺以及采用钝化钢片制造的均温板，所述钝化工艺包括如下步骤：提供钢片；对所述钢片进行预处理，得到预处理钢片；将所述预处理钢片浸泡在钝化液中进行钝化处理，完成后清洗干净并干燥得到钝化钢片。上述钢片钝化工艺的钝化液中包含苯环类有机物和无机物两类物质，通过该钢片钝化工艺制备得到的钝化钢片上形成的钝化膜为包含碳链和无机氧化物的复合膜层。该钝化钢片在用作均热板的盖板时，钝化钢片上形成的钝化膜降低了钝化钢片与水的反应，与表面覆盖铜层的钢片相比，这种钝化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，从而使得这种钝化钢片使用寿命可以延长约2倍-7倍。

Description

钢片钝化工艺、钝化钢片以及均温板 技术领域
本发明涉及散热器件技术领域，尤其涉及一种钢片钝化工艺、该钢片钝化工艺制备得到的钝化钢片以及包括该钝化钢片的均温板。
 背景技术
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。
 技术问题
传统的均温板的上盖板和下盖板多为铜或铜合金，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。
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。
 技术解决方案
基于此，有必要提供一种钢片钝化工艺，通过该钢片钝化工艺制备得到的钝化钢片用作均热板的盖板时具有更长的使用寿命。
此外，还有必要提供一种该钢片钝化工艺制备得到的钝化钢片以及包括该钝化钢片的均温板。
一种钢片钝化工艺，包括如下步骤：
提供钢片；
对所述钢片进行预处理，得到预处理钢片；以及
将所述预处理钢片浸泡在上述的钝化液中进行钝化处理，完成后清洗干净并干燥，得到钝化钢片，其中，所述钝化液包括5g/L-10g/L的含氮或含硫的苯环类有机物和0.5g/L-5g/L的无机物，所述无机物为硅酸盐、稀土化合物或过渡金属化合物，所述钝化液的pH为4-6的水溶液。
优选的，所述含氮或含硫的苯环类有机物为苯并三氮唑、二氨基三氮杂茂或萘磺酸。
优选的，所述硅酸盐为硅酸钠或硅酸钾；所述稀土化合物为稀土硝酸盐、稀土盐酸盐或稀土硫酸盐；所述过渡金属化合物为过渡金属硝酸盐、过渡金属盐酸盐或过渡金属硫酸盐。
优选的，所述钝化液还包括5g/L-10g/L的弱酸和0.5g/L-2g/L的表面活性剂。
优选的，所述弱酸为磺基水杨酸、单宁酸或没食子酸。
优选的，所述表面活性剂为聚乙烯醇、聚乙二醇400-1000或脂肪醇聚氧乙烯醚。
优选的，将所述预处理钢片浸泡在钝化液中进行钝化处理的操作中，所述钝化液的温度为40℃-70℃，所述预处理钢片的浸泡时间为5min-30min。
优选的，对所述钢片进行预处理，得到预处理钢片的操作为：
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；
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
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。
 
一种钝化钢片，采用上述的钢片钝化工艺制备得到。
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用于存储冷却介质的封闭腔体，所述毛细结构设置在所述封闭腔体内；
所述上盖板和/或所述下盖板为上述的钝化钢片。
优选的，所述下盖板靠近所述上盖板的内壁上设有向所述上盖板凸出延伸的多个支撑柱。
优选的，所述毛细结构设置在所述上盖板靠近所述下盖板一侧的内壁上，所述支撑柱与所述毛细结构相抵接。
优选的，所述毛细结构通过金属丝编织、金属粉烧结或表面电化学沉积形成于所述封闭腔体内。
 有益效果
上述钢片钝化工艺的钝化液中包含苯环类有机物和无机物两类物质，通过该钢片钝化工艺制备得到的钝化钢片上形成的钝化膜为包含碳链和无机氧化物的复合膜层。该钝化钢片在用作均热板的盖板时，钝化钢片上形成的钝化膜降低了钝化钢片与水的反应，与表面覆盖铜层的钢片相比，这种钝化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，从而使得这种钝化钢片使用寿命可以延长约2倍-7倍。
此外，通过该钢片钝化工艺制备得到的钝化钢片的钝化膜致密、结合力好、耐蚀性强，并且钝化膜的厚度在10nm-100nm之间，从而不会造成钢片厚度的增加。
 附图说明
图1为一实施方式的钢片钝化工艺的流程图。
图2为如图1所示的钢片钝化工艺的S20的具体流程图。
图3为一实施方式的均温板的立体结构示意图。
图4为如图3所示的均温板的A-A向的剖面结构示意图。
图5为如图3所示的均温板的爆炸结构示意图。
 本发明的实施方式
下面结合附图和实施方式对本发明作进一步说明。
如图1所示的一实施方式的一种钢片钝化工艺，包括如下步骤：
S10、提供钢片。
优选的，钢片为不锈钢片。
具体来说，钢片的厚度可以为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。
S20、对S10得到的钢片进行预处理，得到预处理钢片。
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。
结合图2，具体来说，S20为：
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。
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。
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。
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。
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。
S21中，清洗干净的操作为采用纯水清洗干净。
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。
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。
酸洗处理的目的为去除钢片表面的氧化皮。
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℃。
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。
S22中，清洗干净的操作为采用纯水清洗干净。
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预处理钢片。
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。
活化处理的目的为提高钢片表面活性，保证钝化层和钢片的结合力。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%），尤其当酸洗和钝化之间停留时间较长时。
具体来说，活化处理的温度可以为20℃或25℃。
S23中，清洗干净的操作为采用纯水冲洗干净，冲洗干净后得到的预处理钢片快速浸泡到钝化液中以进行下一步反应。
S30、将S20得到的预处理钢片浸泡在钝化液中进行钝化处理，完成后清洗干净并干燥，得到钝化钢片。
钝化液的pH为4-6的水溶液，钝化液包括5g/L-10g/L的含氮或含硫的苯环类有机物、0.5g/L-5g/L的无机物以及5g/L-10g/L的弱酸。
无机物为硅酸盐、稀土化合物或过渡金属化合物。
钝化处理的目的为在钢片表面形成一层钝化膜，从而得到钝化钢片。
本实施方式中，钝化液包括苯环类有机物和无机物两类物质，从而使得钝化钢片上形成的钝化膜为包含碳链和无机氧化物的复合膜层。无机物不仅作为辅助成膜物质，还作为填孔剂来增强钝化膜的致密性。含氮或含硫的苯环类有机物，可吸附于钢片表面或以螯合的形式在表面形成一层有机膜，浓度过高溶解性差，过低时成膜反应慢，用量在5g/L-10g/L为宜，钢片表面被无机膜占据后难以形成复合膜。
上述钢片钝化工艺制得的钝化钢片在用作均热板的盖板时，钝化钢片上形成的钝化膜降低了钝化钢片与水的反应，与表面覆盖铜层的钢片相比，这种钝化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，从而使得这种钝化钢片使用寿命可以延长约2倍-7倍。
此外，上述钢片钝化工艺制得的钝化钢片的钝化膜致密、结合力好、耐蚀性强，并且钝化膜的厚度在10nm-100nm之间，从而不会造成钢片厚度的增加。
优选的，含氮或含硫的苯环类有机物为苯并三氮唑、二氨基三氮杂茂或萘磺酸。上述有机物分子均具有氮或硫等电负性大的元素，拥有较强的表面活性和吸附能力。可吸附于钢片表面或以螯合的形式在表面形成一层有机膜。
显而易见的，无机物为可以溶解在pH为4-6的钝化液中的物质。
优选的，硅酸盐可以为硅酸钠或硅酸钾；稀土化合物可以为稀土硝酸盐、稀土盐酸盐或稀土硫酸盐；过渡金属化合物可以为过渡金属硝酸盐、过渡金属盐酸盐或过渡金属硫酸盐。
优选的，钝化液还包括5g/L-10g/L的弱酸和0.5g/L-2g/L的表面活性剂。
弱酸和表面活性剂的添加，更有利于钝化膜的形成。
更优选的，弱酸可以为磺基水杨酸、单宁酸或没食子酸，上述弱酸均是带有苯环的羟基羧酸，具有较强的配位能力。表面活性剂可以为聚乙烯醇、聚乙二醇400-1000或脂肪醇聚氧乙烯醚，这些表面活性剂皆为非离子型表面活性剂，具有较强的润湿性和分散性。
脂肪醇聚氧乙烯可以为月桂醇聚氧乙烯醚。
为了使得形成的钝化膜的性质更好，S30中，钝化液的温度为40℃-70℃，预处理钢片的浸泡时间为5min-30min。
S30中，清洗干净并干燥的操作为纯水洗净后放入80℃-100℃的烘箱中干燥10min-20min。
本发明还公开了一种采用上述的钢片钝化工艺制备得到钝化钢片。
上述钝化钢片可以应用于多种领域，钝化层大大提高了钝化钢片的耐腐蚀性和使用寿命。
下面仅以该钝化钢片应用于均温板领域为例进行介绍。
结合图3和图4，本发明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之间形成用于存储冷却介质的封闭腔体40，毛细结构20设置在封闭腔体40内。
上盖板10和/或下盖板30为上述的钝化钢片。
钝化钢片的钝化层可以避免钝化钢片作为均温板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，此外钝化层还大大提高了钝化钢片的耐腐蚀性和使用寿命。
具体来说，结合图3-图5，上盖板10的内壁为平面，下盖板30靠近上盖板10的内壁上设有向上盖板10凸出延伸的多个支撑柱32。优选的，设置在下盖板30上的支撑柱32可以呈阵列排布。
具体来说，毛细结构20设置在上盖板10的内壁。具体的，毛细结构20设置在上盖板10靠近下盖板30一侧的内壁上，支撑柱32与毛细结构20相抵接。
优选的，毛细结构20的材料为铜或者铜合金。
具体来说，毛细结构20可通过金属丝编织、金属粉烧结、表面电化学沉积等形成于封闭腔体40内。
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。
以下为具体实施例。
实施例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。
S20、依次对不锈钢盖板进行除油处理、酸洗处理和活化处理。
除油：将不锈钢盖板放入80℃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、20g/L的碳酸钠和4mL/L的OP乳化剂；
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；
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；
S30、钝化处理：将活化后的不锈钢盖板放入45℃的钝化液中浸泡10min，纯水洗净后放入80℃烘箱中干燥20min，在不锈钢盖板表面形成一层钝化膜，得到钝化不锈钢盖板，钝化液的成分为5g/L的苯并三氮唑、5g/L的硅酸钠、10g/L的磺基水杨酸和0.5g/L的聚乙烯醇，钝化液的pH值为4。
实施例2
实施例2中，S10和S20与实施例1一致。
S30、钝化处理：将活化后的不锈钢盖板放入70℃的钝化液中浸泡30min，纯水洗净后放入80℃烘箱中干燥20min，在不锈钢盖板表面形成一层钝化膜，得到钝化不锈钢盖板，钝化液的成分为7g/L的苯并三氮唑、0.5g/L的硝酸铈、5g/L的磺基水杨酸和2g/L的聚乙烯醇，钝化液的pH值为6。
实施例3
实施例3中，S10和S20与实施例1一致。
S30、钝化处理：将活化后的不锈钢盖板放入45℃的钝化液中浸泡10min，纯水洗净后放入80℃烘箱中干燥15min，在不锈钢盖板表面形成一层钝化膜，得到钝化不锈钢盖板，钝化液的成分为10g/L的苯并三氮唑、3g/L的硫酸锌、8g/L的磺基水杨酸和1g/L的聚乙烯醇，钝化液的pH值为4.8。
对上述实施例1-3的钝化不锈钢盖板进行钝化膜与钢片的结合力测试以及耐点蚀性能测试
钝化膜与钢片之间的结合力是通过阴极试验和耐蚀性测试联合进行评估的，将实施例1-3制得的钝化不锈钢盖板放在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，结合力差的钝化膜在处理后会与钢片剥离、脱落，导致在后续的耐点蚀测试中迅速出现蓝点（一般在5min以内）。
耐点蚀性能测试采用的是铁氰化钾（10g/L）和氯化钠（20g/L）的混合液，用滴管将溶液滴在待测样品表面，收集颜色完全变透明的时间作为耐点蚀性能的一种表征。
Figure 618221dest_path_image001
由表1可以看出，实施例1-3制得的钝化不锈钢盖板中，钝化膜在上述电解处理后并未出现脱落现象，且通过了耐点蚀测试，说明钝化膜与钢片结合紧密。
由表1可以看出，复合钝化膜大幅提升了钢片的耐蚀性，使易受水蒸气侵蚀的铁元素被完全覆盖，有利于抑制铁-水反应以及铁-铜之间所引发的原电池反应，从而提高均温板的使用寿命。与未处理过的不锈钢盖板相比，实施例1-3制得的钝化不锈钢盖板的使用寿命可以延长约2倍-7倍。
以上所述的仅是本发明的实施方式，在此应当指出，对于本领域的普通技术人员来说，在不脱离本发明创造构思的前提下，还可以做出改进，但这些均属于本发明的保护范围。

Claims (13)

  1. 一种钢片钝化工艺，其特征在于，包括如下步骤：
    提供钢片；
    对所述钢片进行预处理，得到预处理钢片；以及
    将所述预处理钢片浸泡在钝化液中进行钝化处理，完成后清洗干净并干燥，得到钝化钢片，其中，所述钝化液包括5g/L-10g/L的含氮或含硫的苯环类有机物和0.5g/L-5g/L的无机物，所述无机物为硅酸盐、稀土化合物或过渡金属化合物，所述钝化液是pH为4-6的水溶液。
  2. 根据权利要求1所述的钢片钝化工艺，其特征在于，所述含氮或含硫的苯环类有机物为苯并三氮唑、二氨基三氮杂茂或萘磺酸。
  3. 根据权利要求1所述的钢片钝化工艺，其特征在于，所述硅酸盐为硅酸钠或硅酸钾；
    所述稀土化合物为稀土硝酸盐、稀土盐酸盐或稀土硫酸盐；
    所述过渡金属化合物为过渡金属硝酸盐、过渡金属盐酸盐或过渡金属硫酸盐。
  4. 根据权利要求1所述的钢片钝化工艺，其特征在于，所述钝化液还包括5g/L-10g/L的弱酸和0.5g/L-2g/L的表面活性剂。
  5. 根据权利要求4所述的钢片钝化工艺，其特征在于，所述弱酸为磺基水杨酸、单宁酸或没食子酸。
  6. 根据权利要求4所述的钢片钝化工艺，其特征在于，所述表面活性剂为聚乙烯醇、聚乙二醇400-1000或脂肪醇聚氧乙烯醚。
  7. 根据权利要求1-6中任意一项所述的钢片钝化工艺，其特征在于，将所述预处理钢片浸泡在钝化液中进行钝化处理的操作中，所述钝化液的温度为40℃-70℃，所述预处理钢片的浸泡时间为5min-30min。
  8. 根据权利要求1-6中任意一项所述的钢片钝化工艺，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：
    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；
    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
    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。
  9. 一种钝化钢片，其特征在于，所述钝化钢片采用如权利要求1-8中任意一项所述的钢片钝化工艺制备得到。
  10. 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用于存储冷却介质的封闭腔体，所述毛细结构设置在所述封闭腔体内；
    所述上盖板和/或所述下盖板为如权利要求9所述的钝化钢片。
  11. 根据权利要求10所述的均温板，其特征在于，所述下盖板靠近所述上盖板的内壁上设有向所述上盖板凸出延伸的多个支撑柱。
  12. 根据权利要求11所述的均温板，其特征在于，所述毛细结构设置在所述上盖板靠近所述下盖板一侧的内壁上，所述支撑柱与所述毛细结构相抵接。
  13. 根据权利要求11或12所述的均温板，其特征在于，所述毛细结构通过金属丝编织、金属粉烧结或表面电化学沉积形成于所述封闭腔体内。
PCT/CN2020/136357 2020-11-27 2020-12-15 钢片钝化工艺、钝化钢片以及均温板 WO2022110339A1 (zh)

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