1、 ENGINEERING MATERIAL SPECIFICATIONDate Action Revisions 2009 06 10 Activated N. B. Chamberlain, T. Honey, J. Richardson, J. Tardiff, NA Printed copies are uncontrolled Copyright 2009, Ford Global Technologies, LLC Page 1 of 5 PRETREATMENT SOLUTION, ZIRCONIUM OXIDE, INITIAL FILL WSS-M3B82-A1 PRETREA
2、TMENT SOLUTION, ZIRCONIUM OXIDE, FEED MATERIAL WSS-M3B82-A2 PRETREATMENT SOLUTION, ZIRCONIUM OXIDE, ADJUSTMENT MATERIAL WSS-M3B82-A3 1. SCOPE The materials defined within these specifications are the basic components for the automotive pretreatment system using zirconium oxide. These materials shall
3、 provide good paint adhesion to the metal surface with adequate durability and corrosion resistance. 2. APPLICATION These specifications were originally released for zirconium oxide pretreatment bath materials used in automotive assembly plants. It is intended for use over such substrates as cold ro
4、lled steel, galvanized, galvannealed and aluminum parts. WSS-M3B82-A1 Zirconium Oxide Pretreatment Solution, Initial Fill is the bath at the point of initial make-up prior to production vehicles being processed. WSS-M3B82-A2 Zirconium Oxide Pretreatment Solution, Feed Material are the individual rep
5、lenisher packages to maintain the pretreatment bath during production. WSS-M3B82-A3 Zirconium Oxide Pretreatment Solution, Adjustment Material are materials used to adjust the bath properties such as pH and cation contamination reduction. 3. REQUIREMENTS 3.1 STANDARD REQUIREMENTS FOR PRODUCTION MATE
6、RIALS Material Suppliers and part producers must conform to the Companys Standard For Production Materials (WSS-M99P1111-A). 3.2 COMPOSITION Supplier must maintain the following characteristics to a maximum tolerance of plus or minus 5% of the initial sample or as reported with the initial sample. A
7、ll other essential components must be reported with the initial sample and maintained as part of the Control Plan as required in 3.1. ENGINEERING MATERIAL SPECIFICATIONWSS-M3B82-A1/A2/A3 Printed copies are uncontrolled Copyright 2009, Ford Global Technologies, LLC Page 2 of 5 3.2.1 Initial Fill and
8、Feed Materials with Zirconium Oxide: (WSS-M3B82-A1 and A2) 3.2.1.1 Zirconium Initial Sample+- 5% (Atomic absorption or Inductively coupled plasma emission spectrometry) 3.2.1.2 Density, kg/l at 25 C Initial Sample +- 0.03 kg/l (ASTM 1475) 3.2.2 Feed Materials and Adjustment Materials: (WSS-M3B82-A2
9、and A3) 3.2.2.1 Critical constituents Initial Sample +- 5% (atomic absorption or Inductively coupled plasma emission spectrometry) 3.2.2.2 Density, kg/l at 25 C Initial Sample +- 0.03 kg/l (ASTM 1475) 3.3 COMPOSITIONAL ANALYSIS Ford Motor Company, at its option, may conduct mass spectroscopy and/or
10、other analysis of material/parts supplied to this specification. The analyses established for initial approval shall constitute the reference standard and shall be kept on file at the designated material laboratory. All samples shall produce the same analyses that correspond to the reference standar
11、d when tested under the same conditions. 3.4 PHYSICAL PROPERTIES The coating where applied will be continuous and meet the requirement of either the coating weight as described below or coating thickness. The technique employed to initially define the coating (Auger/XRF or ICP) as part of the submis
12、sion for material approval will be required to redefine the coating for all future comparative work. 3.4.1 Coating Weight Cold-Rolled Steel 20 - 200 mg/m2Electrogalvanized Steel 40 - 300 mg/m2Hot-dipped Galvanized Steel 40 - 300 mg/m2 Galvannealed Steel 40 - 300 mg/m2 Aluminum 10 - 50 mg/m23.4.2 Coa
13、ting Thickness (See paragraph 4.3) Cold-Rolled Steel 15 85 nm Electrogalvanized Steel 60 200 nm Hot-dipped Galvanized Steel 40 180 nmGalvannealed Steel 40 210 nmAluminum 10 120 nm Minimum and maximum coating weight and coating thickness levels are not be to be violated. Coating weight and coating th
14、ickness are dependent on dwell time in the bath. Tighter ranges for coating weight and coating thickness will be determined at the plant level in the control plan. ENGINEERING MATERIAL SPECIFICATIONWSS-M3B82-A1/A2/A3 Printed copies are uncontrolled Copyright 2009, Ford Global Technologies, LLC Page
15、3 of 5 3.5 PREPARATION OF TEST PANELS Test panels shall be prepared according to the exterior performance specification WSS-M2P180. 3.6 PROCESS WINDOW DEFINITION The supplier shall perform a Design of Experiments (DOE) utilizing response surface analysis to determine the Process Window for the syste
16、m. Four variables are recommended-% zirconium components concentration, pH, process time and process temperature. These variables should be run with good cleaning and suspect cleaning as outside array elements to the variables previously defined. An initial screening experiment should be run to dete
17、rmine what level will generate a window which includes testing to failure. This screening experiment should be reviewed with the Materials Engineer to set up the final DOE. Response attributes to the DOE should be based on the materials tested. Minimal critical testing required: Adhesion (FLTM BI 10
18、6-01), Water Resistance (FLTM BI 104-01), Chip Resistance (SAE J400 and FLTM BI 157-06), Corrosion Resistance (FLTM BI 123-01 and CETP L467 this should be defined by the approving Ford materials engineer) . Process Window characteristics must be submitted and archived with the initial approval packa
19、ge and agreed upon by the approving materials engineer. 3.7 RESISTANCE PROPERTIES Resistance properties panels shall be prepared using standard paint processing parameters as defined in 3.5 3.7.1 Paint Adhesion, max Grade 1 (FLTM BI 106-01, Method B) 3.7.2 Water Resistance 240 h (FLTM BI 104-01) No
20、blistering, dulling, softening, loss of adhesion, and or any other film failure. Adhesion shall be tested according to para 3.7.1 within 20 minutes after removal from water. 3.7.3 Humidity Resistance 240 h (FLTM BI 104-02, Method A) No blistering, dulling, softening, and/or loss of adhesion. Adhesio
21、n shall meet the requirements of para 3.7.1. ENGINEERING MATERIAL SPECIFICATIONWSS-M3B82-A1/A2/A3 Printed copies are uncontrolled Copyright 2009, Ford Global Technologies, LLC Page 4 of 5 3.7.4 Corrosion Resistance 3.7.4.1 FLTM BI 123-01, max 3 mm creep from the Scribe Cold Rolled Steel 15 Cycles Zi
22、nc/Zinc alloy coatings & Al 60 Cycles 3.7.4.2 CETP L467, max 6 weeks (CETP:00.00-L-467, Laboratory Accelerated Corrosion Test) (VCS 1021.29, Scribing of Coated Test Object and Evaluation of Propagation of Corrosion from Scribed Line) Cold rolled steel 10 mm maximum scribe creepage Zinc coated steel
23、6 mm maximum scribe creepage Aluminum 4 mm maximum scribe creepage 3.7.5 Chip Resistance, max 3.7.5.1 Grit Blast, Split Shot Rating 4 (FLTM BI 157-06) 3.7.5.2 Stone Chip, 1.4 L Rating 5B or 97% (SAE J400, -20 +/- 2 C & 23 +/- 2 C) paint retention, no Chips 3mm Dia 3.7.6 Glass Bonding / Paint System
24、Compatibility Shall meet all requirements of Ford Automotive Operations Procedure No. AVP-T118-001, latest revision. 4. GENERAL INFORMATION The material data included herein is for information only and not a requirement for the supplier. Contact The Design Responsible Materials Engineering Activity
25、for the substances currently used in production. 4.1 SUBSTRATES CRS Electrogalvanized Steel Hot Dipped Galvanized Steel Galvannealed Steel Aluminum (AA6111) 4.2 PAINT SYSTEMS (potential paint systems usage for production) E-coat primer + Primer surfacer + Topcoat (basecoat/clearcoat) ENGINEERING MAT
26、ERIAL SPECIFICATIONWSS-M3B82-A1/A2/A3 Printed copies are uncontrolled Copyright 2009, Ford Global Technologies, LLC Page 5 of 5 4.3 Zirconium Oxide Thickness (3.4.2) Coating thickness of zirconium oxide coatings can be determined using one of the substrate appropriate methods below. Coating Thicknes
27、s Method for all Substrates Auger and XRF The XRF instrument generates a XRF spectrum with counts for zirconium within the coating. Calibration is required to convert the counts of zirconium found in the coating to coating thickness. To calibrate the instrument, Auger spectroscopy is used to determi
28、ne the thickness of the coating in nanometers. The zirconium counts can then be correlated to the thickness of the coating found using Auger. At least four different thicknesses over the range of the expected coating thickness must be used to calibrate the portable XRF. Each substrate must have its
29、own calibration curve. The Auger sputter rate calibration should be completed using silicon dioxide. The conversion factor for zirconium oxide coatings is 0.425. On aluminum only the Auger measurements must be done in regions between copper nodules. Coating Thickness Method for Cold-Rolled and Zinc
30、Galvanized Steel only XPS and XRF The XRF instrument generates a XRF spectrum with counts for zirconium within the coating. Calibration is required to convert the counts of zirconium found in the coating to coating thickness. To calibrate the instrument, XPS is used to determine the thickness of the
31、 coating in nanometers. The coating thickness is determined by sputtering the coating off at a rate of 1 A/sec. The zirconium depth profile of a typical zirconium oxide coating will show a plateau or hump, after which the Zr will drop and “tail off“. The thickness has been defined as the point at wh
32、ich the Zr profile drops below ten atomic percent. Each substrate has its own calibration curve and at least four different thicknesses over the range of the expected coating thickness must be used to calibrate the portable XRF. The area of analysis using the XPS prevents an accurate measurement of
33、the coating thickness on aluminum. The sputter rate calibration for XPS should be completed using silicon dioxide. Coating Weight Method for all Substrates ICP and XRF The XRF instrument generates a XRF spectrum with counts for zirconium within the coating. Calibration is required to convert the cou
34、nts of zirconium found in the coating to coating weight. To calibrate the instrument, ICP is used to determine the thickness of the coating in mg/m2. The standard ASTM method for ICP is ASTM E1479. The zirconium oxide coating is stripped off the metal panel using a known volume of 10% HNO3 and 2% HF
35、 in deionized water. A known sample size of the fluid is run through ICP to generate a spectra. The zirconium levels in the spectra provide the concentration of zirconium in the fluid, from which a coating weight can be calculated. Each substrate must be analyzed separately and at least four samples that are representative of the expected range of coating thicknesses must be analyzed.
