US20140150247A1 - Polyamide-imide coated substrate - Google Patents

Polyamide-imide coated substrate Download PDF

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Publication number
US20140150247A1
US20140150247A1 US14/130,915 US201214130915A US2014150247A1 US 20140150247 A1 US20140150247 A1 US 20140150247A1 US 201214130915 A US201214130915 A US 201214130915A US 2014150247 A1 US2014150247 A1 US 2014150247A1
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United States
Prior art keywords
steel
steel substrate
substrate according
polyamide
layer
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Abandoned
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US14/130,915
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English (en)
Inventor
Jose Reyes Flores Ramirez
Magali Audrey Valeria Wainer
Fouzia Hannour
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tata Steel Nederland Technology BV
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Tata Steel Nederland Technology BV
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Application filed by Tata Steel Nederland Technology BV filed Critical Tata Steel Nederland Technology BV
Assigned to TATA STEEL NEDERLAND TECHNOLOGY B.V. reassignment TATA STEEL NEDERLAND TECHNOLOGY B.V. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: FLORES RAMIREZ, JOSE REYES, HANNOUR, FOUZIA, WAINER, Magali Audrey Valeria
Publication of US20140150247A1 publication Critical patent/US20140150247A1/en
Abandoned legal-status Critical Current

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Classifications

    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/14—Polyamide-imides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
    • C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less

Definitions

  • the present invention relates to a steel substrate comprising a corrosion protective coating and to a method for making the same.
  • the present invention further relates to the use of the steel substrate in forming operations to form a part.
  • Galvanized steel is used in applications where rust resistance is needed, for instance, in the automotive industry where the zinc layer reduces the onset of rust at exposed edges and surfaces.
  • galvanised steel substrates are first provided with a phosphate coating (2-5 ⁇ m) to enhance paint adhesion, by enhancing paint adhesion such phosphate coatings indirectly enhance corrosion resistance.
  • the application of the phosphate coating comprises the steps of dissolving metal phosphate salts in a solution of phosphoric acid and immersing the steel substrate in the solution for 4-6 minutes.
  • the automotive manufacturer needs to clean the galvanised steel substrate, such that it is free from oil, grease, lubricants and rust. This is not trivial and increases manufacturing costs.
  • the use of phosphoric acid also introduces environmental and safety issues related to the handling and disposal of such solutions.
  • Organic coatings are often provided on the phosphate coating by electrophoretic deposition, which is a process that uses electrical current to deposit paint onto a suitable substrate.
  • the electro-(organic)-coating typically has a thickness between 7 and 20 ⁇ m and acts as a primer for the application of additional paint layers.
  • the use of electrophoretic deposition to apply organic coatings increases the cost of manufacturing automotive parts due to the high voltages that are required to apply such coatings.
  • the first aspect of the invention relates to a steel substrate suitable for forming operations comprising a corrosion protective coating wherein the corrosion protective coating comprises a layer of polyamide-imide having a dry film thickness between 1 and 10 ⁇ m.
  • the layer of polyamide-imide (PAI) having a thickness between 1 and 10 ⁇ m exhibits improved corrosion resistance, humidity barrier properties, friction and adhesion properties relative to coating systems based on a phosphate layer and an electrophoretic layer, which have a layer thickness of approximately 2 ⁇ m and 20 ⁇ m respectively.
  • the present invention therefore offers automotive manufacturers a significant advantage both in terms of cost and processing and materials handling since a single layer of polyamide-imide can be applied in a single pass to replace both the phosphate layer and the electrophoretic layer.
  • the inventors have found that the thickness of the layer of polyamide-imide should be at most 10 ⁇ m since with higher thicknesses the layer may delaminate from the steel substrate.
  • Another advantage of the present invention is that anti-corrosion pigments need not be provided to obtain the improvements in corrosion resistance.
  • the layer of polyamide-imide has a dry film thickness between 3 and 5 ⁇ m.
  • PAI layers having a thickness between 3 and 5 ⁇ m exhibit excellent performance in respect of barrier, adhesion and corrosion resistance properties that can be provided at reduced cost relative to other thicker coatings.
  • the layer of polyamide-imide has a dry film thickness between 2 and 5 ⁇ m since further cost savings can be made by providing 2 ⁇ m thick PAI layers.
  • lubricant is typically required when forming galvanised steel strips, and in certain instances, it may also be necessary to provide the galvanised steel strips with texture to improve lubricant retention at the steel strip surface.
  • providing texture can be detrimental to both the formability of the galvanised steel strip and the appearance of such formed and painted steel parts.
  • Another consequence of providing texture is that the friction coefficient will increase relative to galvanised steel strips without texture.
  • the layer of polyamide-imide is lubricating, which means an additional step of providing a lubricant and/or texture during subsequent forming and/or stamping operations is not required.
  • the steel substrate is selected from the group consisting of carbon steel, low carbon steel, high strength steel, advanced high strength steel, boron steel, nickel chromium steel, electrical steel, tin-plated steel, nickel-plated steel and electro-coated chromium steel.
  • the second aspect of the invention relates to a method of manufacturing a steel substrate comprising a corrosion protective coating according to the first aspect of the invention which comprises the steps of:
  • Amines used in accordance with the invention include ammonia, hydroxyl amines such as 2,2-Butyliminodiethanol and tertiary amines such as trimethylamine, N,N-dimethyl ethylamine,N,N-dimethyl propylamine, triethylamine or the like. Surprisingly, it was found that the use of hydroxyl amines also improved coating performance which may be due to the water solubility and/or hydrogen bonding properties of hydroxyl amines.
  • Other suitable hydroxyl amines include diethylaminoethanol, diisopropanolamine and aminoethylpropanediol.
  • Tertiary hydroxyl amines are preferred although the presence of primary or secondary hydroxyl amines in the curable coating also improves the corrosion resistance properties of the layer of polyamide-imide.
  • the inventors found that hydroxyl amines having a boiling point of at least 160° C., preferably above 240° C. further improved the corrosion protective properties of the layer of polyamideimide.
  • Tertiary hydroxyl amines such as 2,2-Butyliminodiethanol are particularly preferred.
  • the curable coating is cured using near infrared radiation which causes the steel substrate to heat up and transfer heat to the curable coating. This has the advantage that the curable coating can be cured in seconds rather than minutes.
  • the steel substrate according to the first aspect of the invention is used in forming operations to form a part, which include but are not limited to, stamping, blanking and drawing.
  • the forming is carried out without lubricant.
  • the use of the coated steel strip reduces manufacturing costs since additional lubrication is not required during, for instance, deep-drawing or stamping operations.
  • the coated steel strip can also be manufactured in-house at the steel strip supplier. This has a significant advantage for the automotive manufacturer since the number of manufacturing steps required to form the part is reduced.
  • the automotive manufacturer has to apply lubricant on the bare steel strip it has received, form it, clean it, provide a phosphate layer on the steel strip and provide an electro-coating on the phosphate layer before subsequent paint layers can be applied.
  • the present invention avoids the automotive manufacturer having to apply lubricant before forming, removing lubricant after forming and having to provide the phosphate layer and electro-coating.
  • polyamide amic acid (TORLON® Al-50 from Solvay Advanced Polymers, available as wet powder with a solids content of 35 wt %, is dispersed in a mixture of water (485 g) and dimethyl ethanol amine (50 g). The dispersion is then warmed to a temperature between 60 and 70° C. until the solids dissolve to produce a brown aqueous solution having about 9% by weight polyamide-amic acid.
  • aqueous polyamide-amic acid solution is cooled to room temperature and 0.5 wt % of wetting agent BYK® 380N (from Byk Chemie) is added thereto.
  • This solution is applied on a galvanised steel strip by roller coating at a speed of 150-250 m/min.
  • the applied coating is then cured via near-infrared at s temperature of 260° C. for 5-10 s to remove the aqueous solvent and form a layer of polyamide-imide on the galvanised steel strip surface.
  • C1-C3 are comparative examples in which galvanised steel strips have been provided with titanium phosphate (C1), a layer of acrylic containing chromate pigments (Cr 3 + ) thereon (C2) and polyester paint (C3).
  • Example 2 Other polyamide amic acid solutions were prepared according to the method of Example 1 by replacing dimethyl ethanol amine with 2,2-Butyliminodiethanol (E2), diisopropanolamine (E3) or aminoethylpropanediol (E4). Dimethyl ethanol amine was also replaced by trimethylamine as a further comparative example (C4). These solutions were then applied and cured in accordance with the method of Example 2.
  • the coated steel strip of the invention was subjected to a salt spray test.
  • the salt spray test was performed according to ASTM B117, using a 5% NaCl solution at 35° C., with an overpressure of 2-3.5 mbar (200 to 350 Pascal) to create fog inside the spray chamber.
  • Table 1 shows the corrosion resistance properties of a galvanised steel strip provided with a layer of polyamide-imide (E1-E4) and comparative examples C1-C4. All thicknesses relate to the thickness of the respective layers, i.e. exclusive of the underlying galvanised coating layer. It can be seen from Table 1 that the present invention El offers a significant improvement in corrosion resistance relative to C1-03 with just 2% white rust being observed after 15 days and 5% white rust being observed after 25 days. Similar results are obtained for examples E2-E4. The observed improvement in corrosion resistance properties for E2 relative to El has been attributed to the presence of 2,2-Butyliminodiethanol having a boiling point of 274° C., which is above the temperature required to cure the applied coating.
  • the coated steel strip of the invention was subjected to a cyclic humidity test (DIN-norm 50017, IS06270-2) The following conditions were used: 38° C. with a humidity cycle of 100% for 8 hours and atmospheric humidity for 16 hours.
  • Table 2 shows the humidity barrier properties of the present invention (El) and comparative examples C1-C3.
  • the results show that the layer of polyamide-imide is particularly effective as a humidity barrier since no white rust is observed after 9 weeks and only 2% white is observed after 15 weeks of the cyclic humidity test.
  • white rust can be seen after 3 weeks and between 6 and 15 weeks the amount of white rust significantly increases, particularly with respect to C1 and C2.
  • the coated steel strips were then pulled at a speed of 0.33 mm/s between a flat tool and a cylindrical tool pushed together with a force of 5 kN.
  • the tool material used was DIN 1.3343 and the surface roughness (Ra) of each tool was 0.4 ⁇ m.
  • the tools were cleaned with a tissue soaked in acetone or alcohol.
  • the coated strips were drawn through the tools ten times along a testing distance of 55 mm; after each stroke the tools were released and the strips returned to the original starting position in preparation for the next stroke. All tests were conducted in triplicate at 200 and 80° C. at atmospheric pressure.
  • FIG. 1 shows the coefficient of friction as a function of the number of tooling steps at 20° C.
  • Strip A is a galvanised steel strip that has been provided with a layer of polyamide-imide having a thickness of 6 ⁇ m.
  • Strip B is a cold-rolled steel strip that has been provided with a layer of polyamide-imide having a thickness of 7 ⁇ m.
  • Strips C-D correspond with comparative examples C1-C2 respectively and strip E is a galvanised strip that has been provided with oil as a lubricant.
  • the difference in coefficient of friction between the first tool pass and the tenth tool pass is less than 0.02, i.e. it is substantially constant for both Strip A and Strip B of the invention.
  • the layer of polyamide-imide is smooth enough to have a friction coefficient that satisfies the CoF requirements of the automotive industry (0.13-2.5).
  • the results also show that the layer of polyamide-imide has very good adhesion to the underlying substrate irrespective of whether it is provided on galvanised steel or cold-rolled steel. If this was not the case then the friction coefficient would increase with the number of tool passes. During the LFT no tool damage or tool fouling was observed.
  • the layer of polyamide-imide is also hard enough to resist contact with a metallic tool (at least 10 times). It is this combination of surface characteristics (hard, smooth and adhesive) that allows the coated steel strips of the present invention to be formed without the need of additional lubrication (oil, wax, hard particles).
  • FIG. 2 shows the coefficient of friction as a function of the number of tooling steps at 20° C. and 80° C.
  • Strip A and B are galvanised steel strips that have been provided with a layer of polyamide-imide having a thickness of 6 ⁇ m which were tested for friction respectively at 20° C. and at 80° C.
  • Strips C-D are galvanised strips that have been provided with oil as a lubricant and were tested respectively at 20° C. and at 80° C.
  • the difference in friction coefficient between the first tool pass and the tenth tool pass is less than 0.05 for both strip A and strip B of the invention, i.e. at 20° C. and 80° C.
  • the CoF of the strips with the polyamide-imide layer still satisfy the requirements of the automotive manufacturers.
  • galvanized steel strips with lubricant exhibit a CoF increase of up to 350% from pass 1 to pass 10 at 80° C.
  • FIG. 2 also shows that the adhesion of the polyamide-imide coating to the galvanised steel strip does not degrade with an increase in temperature.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Laminated Bodies (AREA)
US14/130,915 2011-07-07 2012-07-06 Polyamide-imide coated substrate Abandoned US20140150247A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP11005546 2011-07-07
EP11005546.4 2011-07-07
PCT/EP2012/002851 WO2013004394A1 (en) 2011-07-07 2012-07-06 Polyamide-imide coated substrate

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US (1) US20140150247A1 (enrdf_load_stackoverflow)
EP (1) EP2729540B1 (enrdf_load_stackoverflow)
AU (1) AU2012280627B2 (enrdf_load_stackoverflow)
IN (1) IN2014CN00762A (enrdf_load_stackoverflow)
WO (1) WO2013004394A1 (enrdf_load_stackoverflow)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150072091A1 (en) * 2012-04-11 2015-03-12 Seb S.A. Primer Compositions for Non-Stick Coatings and Method for Manufacturing Same
US9404187B2 (en) 2011-07-07 2016-08-02 Tata Steel Nederland Technology B.V. Coated steel substrate and method for making the same
CN108699685A (zh) * 2016-03-07 2018-10-23 塔塔钢铁英国有限公司 用于电池壳的钢片的制造方法和根据所述方法制作的电池壳
US20190277439A1 (en) * 2014-11-10 2019-09-12 Sanoh Industrial Co., Ltd. Coated metal pipe for vehicle piping
WO2021094404A1 (en) * 2019-11-13 2021-05-20 Tata Steel Ijmuiden B.V. Method for producing a part of steel or aluminium
US20220357650A1 (en) * 2021-05-07 2022-11-10 Entegris, Inc. Metal plating with lubricant
US11574764B2 (en) * 2015-01-22 2023-02-07 Alps Electric Co., Ltd. Dust core, method for manufacturing dust core, electric/electronic component including dust core, and electric/electronic device equipped with electric/electronic component
WO2023144709A1 (en) 2022-01-25 2023-08-03 Tata Steel Limited Preparation and application of polyimide intermediates for anti-corrosion coating on metal surfaces

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111925726B (zh) * 2020-08-20 2022-04-29 绵阳麦思威尔科技有限公司 一种海上风机及钢管桩用改性重防腐涂料及其制备方法

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US20140141275A1 (en) * 2011-07-07 2014-05-22 Tata Steel Nederland Technology B.V. Coated steel substrate and method for making the same

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US4330598A (en) * 1980-06-09 1982-05-18 Inland Steel Company Reduction of loss of zinc by vaporization when heating zinc-aluminum coatings on a ferrous metal base
US4508692A (en) * 1982-01-18 1985-04-02 Exxon Research & Engineering Co. Process for the selective removal of hydrogen sulfide from gaseous mixtures with strongly basic tertiary amino compounds
US20040137378A1 (en) * 2001-11-05 2004-07-15 Yoshiki Sugeta Agent for forming coating for narrowing patterns and method for forming fine pattern using the same
US20060151106A1 (en) * 2003-06-02 2006-07-13 Katsufumi Hiraishi Method for producing laminate
US20140141275A1 (en) * 2011-07-07 2014-05-22 Tata Steel Nederland Technology B.V. Coated steel substrate and method for making the same

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9404187B2 (en) 2011-07-07 2016-08-02 Tata Steel Nederland Technology B.V. Coated steel substrate and method for making the same
US20150072091A1 (en) * 2012-04-11 2015-03-12 Seb S.A. Primer Compositions for Non-Stick Coatings and Method for Manufacturing Same
US10030151B2 (en) * 2012-04-11 2018-07-24 Seb S.A. Primer compositions for non-stick coatings and method for manufacturing same
US20190277439A1 (en) * 2014-11-10 2019-09-12 Sanoh Industrial Co., Ltd. Coated metal pipe for vehicle piping
US11574764B2 (en) * 2015-01-22 2023-02-07 Alps Electric Co., Ltd. Dust core, method for manufacturing dust core, electric/electronic component including dust core, and electric/electronic device equipped with electric/electronic component
CN108699685A (zh) * 2016-03-07 2018-10-23 塔塔钢铁英国有限公司 用于电池壳的钢片的制造方法和根据所述方法制作的电池壳
US10920314B2 (en) * 2016-03-07 2021-02-16 Tata Steel Uk Limited Method for manufacturing a steel sheet for a battery case and battery case made according the method
WO2021094404A1 (en) * 2019-11-13 2021-05-20 Tata Steel Ijmuiden B.V. Method for producing a part of steel or aluminium
US20220357650A1 (en) * 2021-05-07 2022-11-10 Entegris, Inc. Metal plating with lubricant
WO2023144709A1 (en) 2022-01-25 2023-08-03 Tata Steel Limited Preparation and application of polyimide intermediates for anti-corrosion coating on metal surfaces

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Publication number Publication date
AU2012280627A1 (en) 2014-01-16
IN2014CN00762A (enrdf_load_stackoverflow) 2015-04-03
WO2013004394A1 (en) 2013-01-10
EP2729540B1 (en) 2015-06-17
EP2729540A1 (en) 2014-05-14
AU2012280627B2 (en) 2016-01-21

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