WO2017214782A1 - 拉丝磷化剂、金属件及其表面皮膜化处理方法 - Google Patents

拉丝磷化剂、金属件及其表面皮膜化处理方法 Download PDF

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WO2017214782A1
WO2017214782A1 PCT/CN2016/085511 CN2016085511W WO2017214782A1 WO 2017214782 A1 WO2017214782 A1 WO 2017214782A1 CN 2016085511 W CN2016085511 W CN 2016085511W WO 2017214782 A1 WO2017214782 A1 WO 2017214782A1
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parts
film
wire drawing
metal
phosphating agent
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PCT/CN2016/085511
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English (en)
French (fr)
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王饶玲
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深圳市恒兆智科技有限公司
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Priority to PCT/CN2016/085511 priority Critical patent/WO2017214782A1/zh
Publication of WO2017214782A1 publication Critical patent/WO2017214782A1/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
    • C23C22/07—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 containing phosphates
    • C23C22/08—Orthophosphates
    • C23C22/12—Orthophosphates containing zinc cations
    • C23C22/13—Orthophosphates containing zinc cations containing also nitrate or nitrite anions

Definitions

  • the present invention relates to the technical field of metal surface treatment, and in particular to a wire phosphating agent, a metal member and a surface filming treatment method thereof.
  • the surface treatment technology of the workpiece is usually applied.
  • the surface treatment of aluminum, iron and their alloys goes deep into all walks of life.
  • most of the work needs to be pretreated before surface treatment, for example, cleaning, decontamination and degreasing, and metal parts for some applications need to be filmed.
  • the filming treatment generally uses a film agent to pretreat the metal member to form a film layer on the surface of the metal member for subsequent surface treatment, thereby increasing the bonding force and corrosion resistance of the subsequent film.
  • a film agent to pretreat the metal member to form a film layer on the surface of the metal member for subsequent surface treatment, thereby increasing the bonding force and corrosion resistance of the subsequent film.
  • the surface film of the existing metal parts is insufficient in adhesion and lubricity.
  • a wire phosphating agent having a fine structure, strong adhesion, and good lubricity, and a metal film surface treatment method and a metal member obtained by the film treatment are provided.
  • a wire phosphating agent for forming a film on a surface of a metal member comprising 1000 parts by weight of the following components by weight: 15-30 parts of phosphoric acid, 10-20 parts of zinc oxide, 30- 60 parts of a nitric acid solution and a balance of water having a mass concentration of 40-60%.
  • a metal member surface filming treatment method comprising the steps of: formulating the above-mentioned drawing phosphating solution 1J; dissolving the drawing phosphating agent in water to prepare a film agent solution, and immersing the metal piece in the film agent solution In the control solution, the total acidity of the solution is 40-50 pt. After the predetermined daytime treatment, the metal parts are washed and dried. And a metal member having a surface having a film formed by a surface treatment method of a metal member as described above.
  • the above-mentioned wire phosphating agent forms a film layer with a fine structure and strong adhesion, and can form a deep blue film with good lubricity on the surface of the metal member, thereby preventing generation in the pipe drawing, spinning, cold forging, and the like. Mold damage and workpiece strain and breakage.
  • Embodiments of the present invention provide a wire phosphating agent for surface pretreatment of a metal member, which comprises, by weight of 1000 parts by weight, the following components by weight: 15-30 parts of phosphoric acid, 10-20 parts of oxidation Zinc, 30-60 parts of nitric acid solution and balance water, the concentration of the nitric acid solution is 40-60%.
  • the parts by weight of the phosphoric acid are preferably 20-25 parts.
  • the zinc oxide is preferably from 1 2 to 18 parts by weight.
  • the parts by weight of the nitric acid solution are preferably 40 to 50 parts by weight.
  • the mass concentration of the nitric acid solution is preferably 40-60%, more preferably 45%.
  • the total acidity of the coating agent is 35-55 pt.
  • a preferable film forming effect is achieved by controlling the balance of the respective distribution ratios. For example, when the phosphoric acid content is low, the film formation is too slow and too thin, and even film formation is not possible. On the contrary, if the reaction is too fast, the film formation is too fast, the formed film is dissolved again, and the film is not strong enough, so the phosphoric acid is preferred in this embodiment. Parts by weight. Among them, the role of zinc oxide and phosphoric acid is to provide a main phosphate film. The nitric acid solution promotes film formation.
  • the film formed by the wire phosphating agent has a fine structure and strong adhesion, and can form a deep blue film with good lubricity on the surface of the metal member, which can prevent the pipe, the wire, and the cold. Forging and other aspects cause mold damage and workpiece strain and breakage.
  • the embodiment of the present invention further provides a metal film surface filming treatment method, comprising the following steps: preparing a wire phosphating agent as described above; dissolving the wire phosphating agent in water to prepare a film agent solution, the metal The piece is immersed in the film solution to control the total acidity of the film solution to be 35-55 pt. After the predetermined daytime treatment, the metal parts are washed and dried. [0016] When the metal member is immersed in the coating agent solution, the total acidity of the coating agent solution is controlled to be 35-55 pt.
  • the surface treatment enthalpy the temperature of the wire phosphating agent is controlled at 70 ° C - 85 ° C, preferably controlled at about 80 ° C.
  • the metal member is immersed in the film of the 1J solution for 3 to 10 minutes.
  • the total acidity measurement method is as follows: Pipette 10 mL of the drawing phosphating agent test solution into a 250 mL Erlenmeyer flask, and add 2-3 drops of phenolphthalein indicator solution. Use 0.1 single amount of sodium hydroxide standard droplets until the solution is pink, that is, the end point, the number of milliliters of sodium hydroxide standard solution consumed is the total acidity of the bath.
  • Embodiments of the present invention also provide a metal member which is treated by a surface treatment method of a metal member as described above to form a film on the surface of the metal member.
  • the film protects the metal parts and is bright in color.
  • the components are mixed in the following parts by weight (total amount of 1000 parts by weight): 15 parts of phosphoric acid, 10 parts of zinc oxide, 30 parts of nitric acid solution and the balance of water, the concentration of the nitric acid solution is 45%, stirring , evenly mixed, formulated into a filming agent.
  • Treatment method preparing the wire drawing phosphating agent; the metal piece is taken as an example, the iron piece is immersed in the film agent solution, and the total acidity of the film agent solution is controlled to be 35-45 pt, at a temperature of 75 degrees, after 5 After a minute of treatment, the metal parts are washed and dried. During the treatment, a film agent can be added to ensure the effect of the working fluid. The film drying temperature should not be too high, should be controlled at about 80 degrees to prevent cracks in the film.
  • the surface of the workpiece was observed, and the surface of the iron piece was found to be dark blue, the color was uniform, and the film was fine, and the nail was able to draw an obvious imprint, and the thickness of the phosphating film was about 8-20 ⁇ (micrometer). Suitable for iron pipe drawing, spinning, cold forging, etc.
  • the components are mixed in the following parts by weight (total amount of 1000 parts by weight): 20 parts of phosphoric acid, 15 parts of zinc oxide, 40 parts of nitric acid solution and the balance of water, the concentration of the nitric acid solution is 45%, stirring , evenly mixed, formulated into a filming agent.
  • Treatment method preparing the wire drawing phosphating agent; the metal piece is taken as an example, the iron piece is immersed in the film agent solution, and the total acidity of the film agent solution is controlled to be 40-50 pt, at a temperature of 80 degrees, after 5 After a minute of treatment, the metal parts are washed and dried. During the treatment, a film agent can be added to ensure the effect of the working fluid. The film drying temperature should not be too high, should be controlled at about 80 degrees to prevent cracks in the film layer.
  • the surface of the workpiece is observed, and the surface of the iron piece is found to be dark blue, the color is uniform, and the film is fine, and the nail can be used to draw an obvious imprint.
  • the thickness of the phosphate film is about 10-25 ⁇ , suitable for For iron pipe drawing, spinning, cold forging, etc.
  • the components are mixed in the following parts by weight (total amount of 1000 parts by weight): 30 parts of phosphoric acid, 20 parts of zinc oxide, 50 parts of nitric acid solution and the balance of water, the concentration of the nitric acid solution is 50%, stirring , evenly mixed, formulated into a filming agent.
  • Treatment method preparing the wire phosphating agent; the metal piece is taken as an example, the iron piece is immersed in the film agent solution, and the total acidity of the film agent solution is controlled to be 40-55 pt, at 80 degrees temperature, after 5 After a minute of treatment, the metal parts are washed and dried. During the treatment, a film agent can be added to ensure the effect of the working fluid. The film drying temperature should not be too high, should be controlled at about 80 degrees to prevent cracks in the film.
  • the surface of the workpiece is observed, and the surface of the iron piece is found to be dark blue, the color is uniform, and the film is fine, and the nail can be used to draw a clear imprint.
  • the thickness of the phosphating film is about 15-30 ⁇ , suitable for For iron pipe drawing, spinning, cold forging, etc.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

一种拉丝磷化剂，其用于金属件表面预处理，能在金属件表面上生成具有良好润滑性的深蓝色的皮膜，以1000重量份计，包括如下重量份数的成分：15-30份磷酸、10-20份的氧化锌、30-60份硝酸溶液和余量水，硝酸溶液的质量浓度为40-60%。还公开了一种通过拉丝磷化剂对金属件的表面皮膜化处理方法，以及通过表面皮膜化处理方法得到的金属件。

Description

拉丝磷化剂、 金属件及其表面皮膜化处理方法 技术领域
[0001] 本发明涉及金属表面处理技术领域， 具体涉及一种拉丝磷化剂、 金属件及其表 面皮膜化处理方法。
背景技术
[0002] 为提高产品表面性能或者外观， 通常对工件表面处理技术。 例如， 铝、 铁及其 合金的表面处理工艺深入各行各业中。 而且， 大多数工作在进行表面处理前还 需要经过预处理， 例如， 进行清洗， 除污除油， 某些用途的金属件还需要进行 皮膜化处理。
[0003] 皮膜化处理一般采用皮膜剂对金属件进行预处理， 以在金属件表面形成膜层， 以便进行后续的表面处理， 增加后续膜的结合力和防腐力。 例如， 对金属件进 行抽管、 抽丝、 冷锻处理之前， 需要在金属件表面形成皮膜， 以在工件处理吋 对其表面进行保护润滑。 然而， 现有的金属件表面皮膜在附着力和润滑性方面 表现不足。
技术问题
[0004] 有鉴于此， 提供一种结构细致、 附着力牢固和润滑性好的拉丝磷化剂， 以及金 属件表面皮膜化处理方法和经过皮膜化处理后制得的金属件。
问题的解决方案
技术解决方案
[0005] 一种拉丝磷化剂， 用于在金属件表面形成皮膜， 以 1000重量份计， 其包括如下 重量份数的成分： 15-30份磷酸， 10-20份的氧化锌， 30-60份硝酸溶液和余量水 ， 该硝酸溶液的质量浓度为 40-60%。
[0006] 一种金属件表面皮膜化处理方法， 其包括下列步骤： 配制如上所述的拉丝磷化 齐 1J ; 将拉丝磷化剂溶于水中配制成皮膜剂溶液， 将金属件浸入皮膜剂溶液中， 控制皮膜剂溶液的总酸度为 40-50pt， 经过预定吋间处理后， 水洗金属件， 干燥 [0007] 以及， 一种金属件， 其表面具有通过如上所述的金属件表面皮膜化处理方法形 成的皮膜。
发明的有益效果
有益效果
[0008] 上述拉丝磷化剂形成的膜层结构细致， 附着力牢固， 能在金属件表面上生成具 有良好润滑性的深蓝色的皮膜， 能防止在抽管、 抽丝、 冷锻等方面产生模具损 伤和工件拉伤和断裂。
[0009]
本发明的实施方式
[0010] 以下将结合具体实施例对本发明进行详细说明。
[0011] 本发明实施例提供一种拉丝磷化剂， 用于金属件表面预处理， 以 1000重量份计 ， 其包括如下重量份数的成分： 15-30份磷酸， 10-20份的氧化锌， 30-60份硝酸 溶液和余量水， 该硝酸溶液的质量浓度为 40-60%。
[0012] 具体地， 所述磷酸的重量份数优选为 20-25份。 所述氧化锌的重量份数优选为 1 2-18份。 所述硝酸溶液的重量份数优选为 40-50份。 所述硝酸溶液的质量浓度优 选为 40-60%， 更优选为 45%。 所述皮膜剂的总酸度为 35-55pt。
[0013] 在上述拉丝磷化剂中， 通过控制各成分配比平衡， 以达到较佳成膜效果。 例如 ， 当磷酸含量低， 成膜则过慢过薄， 甚至不能成膜， 反之则反应过快导致成膜 过快， 刚成的膜又会被溶解， 膜不够牢固， 所以本实施例优选磷酸的重量份数 。 其中， 氧化锌和磷酸的作用在于提供主要磷化膜。 硝酸溶液促进成膜。
[0014] 本实施例中， 拉丝磷化剂形成的皮膜结构细致， 附着力牢固， 能在金属件表面 上生成具有良好润滑性的深蓝色的皮膜， 能防止在在抽管、 抽丝、 冷锻等方面 产生模具损伤和工件拉伤和断裂。
[0015] 本发明实施例还提供一种金属件表面皮膜化处理方法， 其包括下列步骤： 配制 如上所述的拉丝磷化剂； 将拉丝磷化剂溶于水中配制成皮膜剂溶液， 将金属件 浸入皮膜剂溶液中， 控制皮膜剂溶液的总酸度为 35-55pt， 经过预定吋间处理后 ， 水洗金属件， 干燥。 [0016] 在金属件浸入皮膜剂溶液吋， 控制皮膜剂溶液的总酸度为 35-55pt。 表面处理吋 ， 拉丝磷化剂温度控制在 70°C-85°C， 优选为控制在 80度左右。 金属件浸入皮膜 齐 1J溶液的吋间优选为 3-10分钟。 总酸度计量方式为： 用移液管吸取 10mL拉丝磷 化剂试液于 250mL锥形烧瓶中， 加 2-3滴酚酞指示液。 用 0.1单量的氢氧化钠标准 液滴定至溶液呈粉红色， 即为终点， 所消耗氢氧化钠标准液毫升数即为该槽液 的总酸度。
[0017] 本发明实施例还提供一种金属件， 其通过如上所述的金属件表面皮膜化处理方 法进行处理， 在金属件表面形成皮膜。 皮膜可对金属件进行保护， 且色泽光亮 。 以下通过具体实例说明本发明实施例的拉丝磷化剂及其处理方法等方面。
[0018] 实施例 1
[0019] 按照下列重量份数混合各成分 （总量为 1000重量份） ： 15份磷酸， 10份的氧化 锌， 30份硝酸溶液和余量水， 该硝酸溶液的质量浓度为 45%， 搅拌， 混合均匀 ， 配制成皮膜剂。
[0020] 处理方法： 配制好拉丝磷化剂； 金属件以铁件为例， 将铁件浸入皮膜剂溶液中 ， 控制皮膜剂溶液的总酸度为 35-45pt， 在 75度温度下， 经过 5分钟处理后， 水洗 金属件， 干燥。 在处理过程中， 可及吋添加皮膜剂， 以保证工作液的效果。 皮 膜干燥温度不宜过高， 应控制在 80度左右， 防止膜层出现裂痕。
[0021] 经过上述皮膜剂溶液处理后， 观察工件表面， 发现铁件表面呈深蓝色， 颜色均 匀， 皮膜细致， 用指甲能画出明显的印迹， 磷化膜厚度约为 8-20μηι (微米） ， 适合于铁件抽管、 抽丝、 冷锻等。
[0022] 实施例 2
[0023] 按照下列重量份数混合各成分 （总量为 1000重量份） ： 20份磷酸， 15份的氧化 锌， 40份硝酸溶液和余量水， 该硝酸溶液的质量浓度为 45%， 搅拌， 混合均匀 ， 配制成皮膜剂。
[0024] 处理方法： 配制好拉丝磷化剂； 金属件以铁件为例， 将铁件浸入皮膜剂溶液中 ， 控制皮膜剂溶液的总酸度为 40-50pt， 在 80度温度下， 经过 5分钟处理后， 水洗 金属件， 干燥。 在处理过程中， 可及吋添加皮膜剂， 以保证工作液的效果。 皮 膜干燥温度不宜过高， 应控制在 80度左右， 防止膜层出现裂痕。 [0025] 经过上述皮膜剂溶液处理后， 观察工件表面， 发现铁件表面表面呈深蓝色， 颜 色均匀， 皮膜细致， 用指甲能画出明显的印迹， 磷化膜厚度约为 10-25μηι， 适合 于铁件抽管、 抽丝、 冷锻等。
[0026] 实施例 3
[0027] 按照下列重量份数混合各成分 （总量为 1000重量份） ： 30份磷酸， 20份的氧化 锌， 50份硝酸溶液和余量水， 该硝酸溶液的质量浓度为 50%， 搅拌， 混合均匀 ， 配制成皮膜剂。
[0028] 处理方法： 配制好拉丝磷化剂； 金属件以铁件为例， 将铁件浸入皮膜剂溶液中 ， 控制皮膜剂溶液的总酸度为 40-55pt， 在 80度温度下， 经过 5分钟处理后， 水洗 金属件， 干燥。 在处理过程中， 可及吋添加皮膜剂， 以保证工作液的效果。 皮 膜干燥温度不宜过高， 应控制在 80度左右， 防止膜层出现裂痕。
[0029] 经过上述皮膜剂溶液处理后， 观察工件表面， 发现铁件表面表面呈深蓝色， 颜 色均匀， 皮膜细致， 用指甲能画出明显的印迹， 磷化膜厚度约为 15-30μηι， 适合 于铁件抽管、 抽丝、 冷锻等。
[0030] 需要说明的是， 本发明并不局限于上述实施方式， 根据本发明的创造精神， 本 领域技术人员还可以做出其他变化， 这些依据本发明的创造精神所做的变化， 都应包含在本发明所要求保护的范围之内。

Claims

权利要求书
[权利要求 1] 一种拉丝磷化剂， 用于在金属件表面形成皮膜， 其特征在于， 以 1000 重量份计， 包括如下重量份数的成分： 15-30份磷酸， 10-20份的氧化 锌， 30-60份硝酸溶液和余量水， 该硝酸溶液的质量浓度为 40-60%。
[权利要求 2] 如权利要求 1所述的拉丝磷化剂， 其特征在于， 所述磷酸的重量份数 为 20-25份。
[权利要求 3] 如权利要求 1所述的拉丝磷化剂， 其特征在于， 所述氧化锌的重量份 数为 12-18份。
[权利要求 4] 如权利要求 1所述的拉丝磷化剂， 其特征在于， 所述硝酸溶液的重量 份数为 40-50份。
[权利要求 5] 如权利要求 1所述的拉丝磷化剂， 其特征在于， 所述硝酸溶液的质量 浓度为 45-55%。
[权利要求 6] 如权利要求 1所述的拉丝磷化剂， 其特征在于， 所述皮膜剂的总酸度 为 40-50pt。
[权利要求 7] —种金属件表面皮膜化处理方法， 其包括下列步骤： 配制如权利要求
1-6任一项所述的拉丝磷化剂； 将拉丝磷化剂溶于水中配制成皮膜剂 溶液将金属件浸入皮膜剂溶液中， 控制皮膜剂溶液的总酸度为 40-50p t， 经过预定吋间处理后， 水洗金属件， 干燥。
[权利要求 8] —种金属件， 其特征在于， 所述金属件表面通过如权利要求 7所述的 金属件表面皮膜化处理方法形成有皮膜。
[权利要求 9] 如权利要求 9所述的金属件， 其特征在于， 所述金属件为铁件。
PCT/CN2016/085511 2016-06-12 2016-06-12 拉丝磷化剂、金属件及其表面皮膜化处理方法 WO2017214782A1 (zh)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB496866A (en) * 1937-06-01 1938-12-07 Metallgesellschaft Ag Process for improving the working of metals by processes such as drawing, not involving the use of cutting tools
US3520737A (en) * 1965-12-22 1970-07-14 Amchem Prod Processes for the production of zinc phosphate coatings
US3681148A (en) * 1967-03-10 1972-08-01 Collardin Gmbh Gerhard Process for the application of thin,continuous phosphate layers on metal surfaces
CN102418094A (zh) * 2011-11-16 2012-04-18 南京派诺金属表面处理技术有限公司 冷成型加工用低温磷化浓缩液及冷成型加工用低温磷化工艺

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB496866A (en) * 1937-06-01 1938-12-07 Metallgesellschaft Ag Process for improving the working of metals by processes such as drawing, not involving the use of cutting tools
US3520737A (en) * 1965-12-22 1970-07-14 Amchem Prod Processes for the production of zinc phosphate coatings
US3681148A (en) * 1967-03-10 1972-08-01 Collardin Gmbh Gerhard Process for the application of thin,continuous phosphate layers on metal surfaces
CN102418094A (zh) * 2011-11-16 2012-04-18 南京派诺金属表面处理技术有限公司 冷成型加工用低温磷化浓缩液及冷成型加工用低温磷化工艺

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