CN110809640A - Black phosphating agent, metal piece and surface phosphating method thereof - Google Patents

Black phosphating agent, metal piece and surface phosphating method thereof Download PDF

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Publication number
CN110809640A
CN110809640A CN201780092849.8A CN201780092849A CN110809640A CN 110809640 A CN110809640 A CN 110809640A CN 201780092849 A CN201780092849 A CN 201780092849A CN 110809640 A CN110809640 A CN 110809640A
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China
Prior art keywords
parts
phosphating
black
weight
phosphating agent
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CN201780092849.8A
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Chinese (zh)
Inventor
方招娣
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Shenzhen Mayor Hongtai Technology Co Ltd
Shenzhen Changhongtai Technology Co Ltd
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Shenzhen Mayor Hongtai Technology Co Ltd
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Publication of CN110809640A publication Critical patent/CN110809640A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/40Chemical 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 molybdates, tungstates or vanadates
    • C23C22/42Chemical 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 molybdates, tungstates or vanadates containing also phosphates

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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

The black phosphating agent is used for forming a film on the surface of a metal piece and comprises the following components in parts by weight in 1000 parts: 30-50 parts of manganese dihydrogen phosphate, 40-60 parts of zinc nitrate, 2-5 parts of nickel nitrate, 1-4 parts of acetic acid, 1-4 parts of ammonium citrate, 0.5-2 parts of bismuth molybdate and the balance of water. The film formed by the black phosphating agent is compact and uniform, has good toughness, large thickness, high corrosion resistance and less sediment, and is suitable for corrosion resistant treatment of the surface of steel.

Description

Black phosphating agent, metal piece and surface phosphating method thereof
Black phosphating agent, metal piece and surface phosphating method thereof
[0001] The invention relates to the technical field of metal surface treatment, in particular to a black phosphating agent, a metal piece and a surface phosphating method thereof.
Background
[0002] In order to improve the surface properties or appearance of the product, the surface of the workpiece is usually treated. For example, surface treatment processes for aluminum, iron, and alloys thereof are in great variety of industries. Furthermore, most work requires pretreatment, such as cleaning, degreasing and decontamination, before surface treatment, and some uses require phosphating of the metal parts.
[0003] Phosphating generally adopts a phosphating agent to pretreat a metal piece so as to form a passivation layer on the surface of the metal piece, so that subsequent surface treatment is performed, and the bonding force, the corrosion resistance, the lubricating property and the like of a subsequent film are increased. For example, screw fasteners and the like need to be rustproof for a long time without being sprayed, and are often phosphated for high corrosion resistance. However, most of the existing phosphatizing agents have complex process, much precipitation, high energy consumption and poor corrosion resistance.
Technical problem
[0004] In view of the above, a black phosphating agent with a dense, uniform and firm film layer, good toughness, large thickness and strong corrosion resistance, a surface phosphating method of a metal part and the metal part prepared by phosphating are provided. Solution to the problem
Technical solution
[0005] A black phosphating agent is used for forming a coating on the surface of a metal piece and comprises the following components in parts by weight in 1000 parts: 30-50 parts of manganese dihydrogen phosphate, 40-60 parts of zinc nitrate, 2-5 parts of nickel nitrate, 1-4 parts of acetic acid, 1-4 parts of ammonium citrate, 0.5-2 parts of bismuth molybdate and the balance of water.
[0006] A surface phosphating method for a metal piece comprises the following steps: preparation of the Black phosphating agent as described above
(ii) a And (3) immersing the metal piece into a phosphating solution, washing with water and drying after a preset time interval of treatment.
[0007] And a metal material having a coating film formed by the metal material surface phosphating method.
Advantageous effects of the invention
[0008] The black phosphating agent is prepared by compounding manganese dihydrogen phosphate, zinc nitrate and various additives, and the formed film has the characteristics of compact crystallization, large film thickness, high hardness, strong corrosion resistance and the like. The black phosphating agent can be widely applied to the corrosion prevention and lubrication of metals.
Modes for carrying out the invention
[0009] The present invention will be described in detail with reference to specific examples.
[0010] The embodiment of the invention provides a black phosphating agent for forming a coating on the surface of a metal piece, which comprises the following components in parts by weight in 1000 parts by weight: 30-50 parts of manganese dihydrogen phosphate, 40-60 parts of zinc nitrate, 2-5 parts of nickel nitrate, 1-4 parts of acetic acid, 1-4 parts of ammonium citrate, 0.5-2 parts of bismuth molybdate and the balance of water.
[0011] Specifically, the weight part of the manganese dihydrogen phosphate is preferably 35 to 45 parts. The weight portion of the zinc nitrate is preferably 45 to 55 portions. The weight portion of the nickel nitrate is 3-4. The weight part of the acetic acid is preferably 2 to 3 parts. The weight portion of the bismuth molybdate is 1-2 portions. The weight portion of the ammonium citrate is 2-3 portions.
[0012] In the black phosphating agent, the better film forming effect is achieved by controlling the proportion balance of the components. Wherein the ammonium citrate and acetic acid stabilize the pH of the bath solution and promote film formation. Manganese dihydrogen phosphate and zinc nitrate are main film forming components. The nickel nitrate and the bismuth molybdate enable the film to be fine and uniform, so that the corrosion resistance and the wear resistance of the phosphating film can be improved.
[0013] In the embodiment, the black phosphating film has large thickness and few pores, and the phosphating grains are dense and granular and can be widely applied to corrosion prevention of steel. The black phosphating agent is prepared by compounding manganese dihydrogen phosphate, zinc nitrate and various additives. The metal workpiece is immersed in the acidic treating liquid prepared from the phosphating liquid, and the metal interacts with acid and salt to generate a water-insoluble protective black film layer on the surface of the workpiece. The film has compact crystallization, and has the characteristics of large film thickness, high hardness, strong corrosion resistance and the like.
[0014] The embodiment of the invention also provides a metal piece surface phosphating method, which comprises the following steps: preparing the black phosphating agent; dissolving a black phosphating agent in water to prepare phosphating solution, immersing the metal piece into the phosphating solution, performing treatment for a preset time, washing with water, and drying.
[0015] The metal piece was immersed in a phosphating solution. Surface treatment time, and the temperature of the black phosphating agent is controlled to be 60-80 ℃. The metal pieces are preferably immersed in the phosphating solution for 15-25 minutes. Preferably, the metal workpiece is degreased and pickled before the metal part is immersed in the phosphating solution, and after the metal part is immersed in the phosphating solution, the metal part can be further immersed in an antirust agent or an antirust oil to increase the corrosion resistance of the metal part. [0016] The embodiment of the invention also provides a metal part, which is treated by the metal part surface phosphating method to form a film on the surface of the metal part. The film can protect and lubricate the metal piece, and has strong corrosion resistance.
[0017] The black phosphating agent and the treatment method thereof according to the embodiment of the invention are described below by specific examples.
[0018] Example 1
[0019] Mixing the following components in parts by weight (the total amount is 1000 parts by weight): 30 parts of manganese dihydrogen phosphate, 40 parts of zinc nitrate, 2 parts of nickel nitrate, 1 part of acetic acid, 1 part of ammonium citrate, 0.5 part of bismuth molybdate and the balance of water, stirring and uniformly mixing to prepare the phosphating agent.
[0020] The phosphating treatment method comprises the following steps: preparing a black phosphating agent according to the method; taking an iron piece as an example, the iron piece is immersed into a phosphating solution, the phosphating solution is controlled at the temperature of 80 ℃ for 25 minutes, and then the iron piece is washed and dried. In the treatment process, the phosphating agent can be added to the water to ensure the effect of the working solution.
[0021] After the phosphating solution is treated, the surface of the workpiece is observed, a black film layer is found on the surface of the workpiece, the color is uniform, the film is fine, and the corrosion resistance of the workpiece is tested by a copper sulfate dropping experiment, so that the workpiece does not change the color within more than 1 minute.
[0022] Example 2
[0023] Mixing the following components in parts by weight (the total amount is 1000 parts by weight): 38 parts of manganese dihydrogen phosphate, 48 parts of zinc nitrate, 3 parts of nickel nitrate, 2 parts of acetic acid, 2 parts of ammonium citrate, 1 part of bismuth molybdate and the balance of water, stirring, and uniformly mixing to prepare the phosphating agent.
[0024] The phosphating treatment method comprises the following steps: preparing a black phosphating agent according to the method; taking an iron piece as an example, the iron piece is immersed into a phosphating solution, the phosphating solution is controlled at the temperature of 80 ℃ for 25 minutes, and then the iron piece is washed and dried. In the treatment process, the phosphating agent can be added to the water to ensure the effect of the working solution.
[0025] After the phosphating solution is treated, the surface of the workpiece is observed, a black film layer is found on the surface of the workpiece, the color is uniform, the film is fine, and the corrosion resistance of the workpiece is tested by a copper sulfate dropping experiment, so that the workpiece does not change the color within more than 3 minutes.
[0026] Example 3
[0027] Mixing the following components in parts by weight (the total amount is 1000 parts by weight): 45 parts of manganese dihydrogen phosphate, 53 parts of zinc nitrate, 4 parts of nickel nitrate, 3 parts of acetic acid, 3 parts of ammonium citrate, 1.5 parts of bismuth molybdate and the balance of water, stirring and uniformly mixing to prepare the phosphating agent.
[0028] The phosphating treatment method comprises the following steps: preparing a black phosphating agent according to the method; taking an iron piece as an example, the iron piece is immersed into a phosphating solution, the phosphating solution is controlled at the temperature of 70 ℃, and after 20 minutes of treatment, the iron piece is washed and dried. In the treatment process, the phosphating agent can be added to the water to ensure the effect of the working solution.
[0029] After the phosphating solution is treated, the surface of the workpiece is observed, a black film layer is found on the surface of the workpiece, the color is uniform, the film is fine, and the corrosion resistance of the workpiece is tested by a copper sulfate dropping experiment, so that the workpiece does not change the color after more than 5 minutes.
[0030] Example 4
[0031] Mixing the following components in parts by weight (the total amount is 1000 parts by weight): 50 parts of manganese dihydrogen phosphate, 60 parts of zinc nitrate, 5 parts of nickel nitrate, 4 parts of acetic acid, 4 parts of ammonium citrate, 2 parts of bismuth molybdate and the balance of water, stirring, and uniformly mixing to prepare the phosphating agent.
[0032] The phosphating treatment method comprises the following steps: preparing a black phosphating agent according to the method; taking an iron piece as an example, the iron piece is immersed into a phosphating solution, the phosphating solution is controlled at the temperature of 70 ℃ for 15 minutes, and then the iron piece is washed and dried. In the treatment process, the phosphating agent can be added to the water to ensure the effect of the working solution.
[0033] After the phosphating solution is treated, the surface of the workpiece is observed, a black film layer is found on the surface of the workpiece, the color is uniform, the film is fine, and the corrosion resistance of the workpiece is tested by a copper sulfate dropping experiment, so that the workpiece does not change the color after more than 5 minutes.
[0034] It should be noted that the present invention is not limited to the above-mentioned embodiments, and other changes and modifications can be made by those skilled in the art according to the spirit of the present invention, and these changes and modifications are included in the scope of the present invention as claimed.

Claims (1)

  1. Claims
    [ claim 1] A black phosphating agent for forming a coating on the surface of a metal part, which is characterized by comprising the following components in parts by weight, based on 1000 parts by weight: 30-50 parts of manganese dihydrogen phosphate, 40-60 parts of zinc nitrate, 2-5 parts of nickel nitrate, 1-4 parts of acetic acid, 1-4 parts of ammonium citrate, 0.5-2 parts of bismuth molybdate and the balance of water.
    [ claim 2] the black phosphating agent according to claim 1, wherein the manganese dihydrogen phosphate is present in an amount of 35 to 45 parts by weight.
    [ claim 3] the black phosphating agent according to claim 1, wherein the zinc nitrate is present in an amount of 45 to 55 parts by weight.
    [ claim 4] the black phosphating agent according to claim 1, wherein the nickel nitrate is present in an amount of 3 to 4 parts by weight.
    [ claim 5] the black phosphating agent according to claim 1, wherein the ammonium citrate is present in an amount of 2 to 3 parts by weight.
    [ claim 6] the black phosphating agent according to claim 1, wherein the acetic acid is present in an amount of 2 to 3 parts by weight.
    [ claim 7] the black phosphating agent according to claim 1, wherein the bismuth molybdate is present in an amount of 1 to 2 parts by weight.
    [ claim 8] A surface phosphating method for a metal piece, which comprises the following steps: formulating the black phosphating agent according to any one of claims 1 to 7; and (3) immersing the metal piece into a phosphating solution, performing treatment within a preset time interval, washing with water, and drying.
    [ claim 9] the method for phosphating the surface of a metal piece according to claim 8, wherein the metal piece is degreased and pickled before being immersed in the phosphating solution, and the phosphating temperature is 60-80 ℃.
    [ claim 10] A metal member, wherein a black coating film is formed on the surface of the metal member by the metal member surface phosphating method according to claim 8.
CN201780092849.8A 2017-07-04 2017-07-04 Black phosphating agent, metal piece and surface phosphating method thereof Withdrawn CN110809640A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3484304A (en) * 1966-10-11 1969-12-16 Hooker Chemical Corp Process and composition for cleaning and coating metal surfaces
CN101200799A (en) * 2006-12-15 2008-06-18 西安工业大学 Medium-low temperature high corrosion resistant black phosphating solution on steel surface
CN104250776A (en) * 2013-06-26 2014-12-31 无锡洛社科技创业有限公司 Phosphatization technology for hot rolling steel plate under normal temperature
CN104250771A (en) * 2013-06-26 2014-12-31 无锡洛社科技创业有限公司 Room temperature phosphating solution of hot rolled steel plate
CN105256297A (en) * 2014-07-17 2016-01-20 烟台盛业钢格板有限公司 High-corrosion-resistance phosphating solution and preparing method thereof
CN106148974A (en) * 2016-09-29 2016-11-23 广州市汇吉科技企业孵化器有限公司 A kind of iron and steel derusting and phosphorating agent

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08325748A (en) * 1995-05-31 1996-12-10 Daido Kagaku Kogyo Kk Surface treating composition for melanizing and treatment

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3484304A (en) * 1966-10-11 1969-12-16 Hooker Chemical Corp Process and composition for cleaning and coating metal surfaces
CN101200799A (en) * 2006-12-15 2008-06-18 西安工业大学 Medium-low temperature high corrosion resistant black phosphating solution on steel surface
CN104250776A (en) * 2013-06-26 2014-12-31 无锡洛社科技创业有限公司 Phosphatization technology for hot rolling steel plate under normal temperature
CN104250771A (en) * 2013-06-26 2014-12-31 无锡洛社科技创业有限公司 Room temperature phosphating solution of hot rolled steel plate
CN105256297A (en) * 2014-07-17 2016-01-20 烟台盛业钢格板有限公司 High-corrosion-resistance phosphating solution and preparing method thereof
CN106148974A (en) * 2016-09-29 2016-11-23 广州市汇吉科技企业孵化器有限公司 A kind of iron and steel derusting and phosphorating agent

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Application publication date: 20200218