FORD WSS-M33J7-B1-2002 ENAMEL COMPLIANCE VOC HIGH SOLIDS THERMOSET BASECOAT BASECOAT CLEARCOAT WET-ON-WET PROCESS WITH WSS-M33J7-B2 ETCH & SCRATCH RESISTANT EXTERIOR TO BE USED WI.pdf

1、 ENGINEERING MATERIAL SPECIFICATION Material Name Specification Number Date Action Revisions 2002 11 14 Activated T. Dusbiber Printed copies are uncontrolled Page 1 of 21 Copyright 2002, Ford Global Technologies, Inc. ENAMEL, COMPLIANCE VOC, HIGH SOLIDS, THERMOSET WSS-M33J7-A1 BASECOAT, BASECOAT/CLE

2、ARCOAT WET-ON-WET PROCESS WITH WSS-M33J7-A2, ETCH RESISTANT, EXTERIOR ENAMEL, COMPLIANCE VOC, HIGH SOLIDS, THERMOSET WSS-M33J7-A2 CLEARCOAT, BASECOAT/CLEARCOAT WET-ON-WET PROCESS WITH WSS-M33J7-A1, ETCH RESISTANT, EXTERIOR ENAMEL, COMPLIANCE VOC, HIGH SOLIDS, THERMOSET WSS-M33J7-A3 TINTED CLEARCOAT,

3、 BASECOAT/CLEARCOAT WET-ON-WET PROCESS, ETCH RESISTANT, EXTERIOR ENAMEL, COMPLIANCE VOC, HIGH SOLIDS, THERMOSET WSS-M33J7-B1 BASECOAT, BASECOAT/CLEARCOAT WET-ON-WET PROCESS WITH WSS-M33J7-B2, ETCH a solution in water of 0.75 % by weight CaSO4 adjusted to a pH of 4; deionized water (DI) and tap water

4、, Bee Dropping (Ford Method 24) available from Global Paint Engineering (North America Paint Engineering). Apply 0.05 ml of specified solutions along entire length of 2 test panels. Place on gradient bar (38 - 82 C, calibrated for heat-up rate of 2 minutes or less for 0.9 mm steel substrate). Remove

5、 1 panel after 15 minutes at temperature, other after 30 minutes. Rinse any remaining solution with water. Examine panels for etching, discoloration, pitting, etc. Report etch-free temperature for test material and control. NOTE: Process window evaluation will be done using 2 solutions: (1) Sulfuric

6、 Acid pH3, 15 minute exposure; and (2) CaSO4 pH4, 30 minute exposure. 3.8.3 Xylene Resistance No softening, or dulling permitted Using a circular motion, rub surface of enamel 10 times with wetted cheesecloth. ENGINEERING MATERIAL SPECIFICATION WSS-M33J7-A1/A2/A3/B1/B2/B3 Page 8 of 21 Copyright 2002

7、, Ford Global Technologies, Inc. 3.8.4 Fluid Spotting Resistance (FLTM BI 113-01) No color change, dulling, surface distortion, spotting or permanent softening permitted. Test 2 sets of panels: (1) Aged per test method (2) Unaged and conditioned less than 8 h The following fluids will be tested: . D

8、eionized Water . Liquid Soap . Windshield Washer Fluid (Current Production Fill), Concentrated (100 %) . Coolant Solution (Current Production Fill), Concentrated (100 %) . Motor Oils (Current Production Fill) . Bug and Tar Remover* (Ford Part No. B7A-19520-AA) . Rust Preventative Coatings (including

9、 cavity waxes) *Aged panels only, apply Remover as directed on package, leave on for 5 minutes. Clean and rinse panels. 3.8.5 Cold Checking Resistance 15 cycles (FLTM BI 107-02) 3.8.6 Fuel Resistance No color change, dulling, surface distortion or permanent softening permitted. 3.8.6.1 Plastic Subst

10、rates (FLTM BO 101-05) 3.8.6.2 Metal Substrates Procedure for Drip Test: Run tests using Blends “A“ and “B“ separately The size of the test panels shall be 100 x 150 mm. A burette must be used to allow the Gasohol to drip at a rate which requires approximately 1 h for the 50 mL to be evacuated (equi

11、valent to approximately 1 drop every 3 s). Note: The panel shall be placed paint side up at an angle of 60 deg from the horizontal. The distance from the tip of the burette to the spot where the drop impinges on the panel is 300 mm. (The spot is centered 100 mm above the lower edge of the test panel

12、.) The test panel shall be placed in a flat open dish to contain accumulated Gasohol. ENGINEERING MATERIAL SPECIFICATION WSS-M33J7-A1/A2/A3/B1/B2/B3 Page 9 of 21 Copyright 2002, Ford Global Technologies, Inc. Conduct testing in a well ventilated hood at ambient room temperature of 24 +/- 2 C, away f

13、rom all sources of ignition. Gasohol Composition by Volume Blend A: ASTM Reference Fuel C 85 % Methanol 15 % Blend B: ASTM Reference Fuel C 15 % Methanol 85 % Remove panels from test and allow them to recover for 1 h at ambient room conditions. Examine panels for color change, dulling, and surface d

14、istortion or permanent softening. 3.8.7 Scratch and Mar Resistance Nano Scratch Test Requirement: Average of the weathered and un-weathered Fracture Load must be greater than: (mN) WSS-M33J7-A2, A3 8.0 WSS-M33J7-B2, B3 13.0 Average of the weathered and un-weathered Plastic deformation must not be gr

15、eater than: (micrometers) WSS-M33J7-A2, A3 0.40 WSS-M33J7-B2, B3 0.35 3.8.7 Scratch and Mar Resistance (Cont.) Nano Scratch Test Test Method: Expose paint systems to 3 months natural Florida weathering (SAE J1976) or 400h accelerated weathering (SAE J1960, modified with type “S“ borosilicate inner a

16、nd outer filters, 0.55 W/m2 radiant exposure). The normal force at fracture and the permanent deformation at 5mN are to be determined on full paint systems both before and after weathering. Evaluate samples using a CSM Instruments Nano Scratch Tester or equivalent with the following instrument condi

17、tions: ENGINEERING MATERIAL SPECIFICATION WSS-M33J7-A1/A2/A3/B1/B2/B3 Page 10 of 21 Copyright 2002, Ford Global Technologies, Inc. Load Type: Progressive Initial Load: 0.1 mN Final Load: Sample Dependant (60 mN max) Scanning Load: 0.1 mN Scratching Speed: 3.0 mm/min Loading Rate: 40.0 mN/min Rockwel

18、l Diamond Tip: R=2m; a=90 Record individual un-weathered and weathered values for normal force at fracture and permanent deformation at 5mN, for each of 3 runs. The normal force at fracture is determined by taking the average of the first 3 incidents of fracture that are greater than 1/3 the distanc

19、e of the scratch width. Report the average combined un-weathered and weathered results for normal force at fracture and permanent deformation at 5mN. 3.8.8 Intercoat Adhesion, max Grade 2 (FLTM BI 106-01, Part B) 3.8.9 Chipping Resistance No chip greater (SAE J400, as indicated) than 3 mm dia. in al

20、l 1.41 liter (-18 C and 25 C) conditions below 3.8.9.1 First Run Condition (No Repair) No more than 3 % area removed 3.8.9.2 High Bake Repair Condition No more than 7 % area removed 3.8.10 High Performance Stone Chip 4 Resistance, min (FLTM BI 157-06) 3.8.11 Sag Resistance Equal to or (FLTM BI 122-0

21、2) better than control enamel 3.8.12 Water Immersion 240 h (FLTM BI 104-01, B) No blistering, dulling, wrinkling, softening and/or loss of adhesion permitted. ENGINEERING MATERIAL SPECIFICATION WSS-M33J7-A1/A2/A3/B1/B2/B3 Page 11 of 21 Copyright 2002, Ford Global Technologies, Inc. 3.9 WEATHERING Af

22、ter exposure (para 3.9.1 and 3.9.2), panels must meet the requirements of para 3.9.3. 3.9.1 Natural Weathering Florida Exposure (SAE J1976, Procedure A) New Pigment 2 years required, 3 - 5 years and 10 year submission New Color, Known 1 year required, 2 - 5 years and 10 year Pigments and Resins subm

23、ission New Resin Technology 5 years required, 10 year submission (one panel for every year of testing as specified in para 5.2, Table 3) 3.9.2 Accelerated Weathering (SAE J1960, 0.55 W/m2Irradiance) New Pigment 4000 h in applicable resin system New Color, Known 3000 h required Pigment and Resins New

24、 Resin Technology 6000 h required, Borosilicate Inner and Outer Filters (para 4.2, Table 3) 3.9.3 Testing After Exposure (FLTM BI 160-01, B) 3.9.3.1 Appearance After 1 year exposure, there shall be no visual color change, minimal gloss and DOI loss not to exceed 2 year requirement. There shall be no

25、 blistering, cracking, peeling or microchecking. After 2 years Florida exposure or 3000 h accelerated weathering, no less than AATCC color rating 4. There shall be no blistering, cracking, peeling or microchecking. After 5 Florida years exposure or 6000 h accelerated weathering, there shall be no ex

26、cessive color change, blistering, cracking, peeling or microchecking. ENGINEERING MATERIAL SPECIFICATION WSS-M33J7-A1/A2/A3/B1/B2/B3 Page 12 of 21 Copyright 2002, Ford Global Technologies, Inc. 3.9.3.2 Gloss After Exposure (ASTM D 523, 20 degree Glossmeter) 2 year exposure, min 3000 h, min Non-Tinte

27、d Clearcoats, max 15 % loss (WSS-M33J7-A2, B2) Tinted Clearcoats, max 20 % loss (WSS-M33J7-A3, B3) 3.9.3.3 QMS or Wave Scan DOI (Appearance is to be measured with a reliable instrument such as Autospect Inc QMS-BP or Byk Gardner Wave Scan.) 2 year exposure, min 3000 h, min Non-Tinted Clearcoats, max

28、 20 % loss (WSS-M33J7- A2, B2) Tinted Clearcoats, max 30 % loss (WSS-M33J7- A3, B3) 3.9.3.4 Basecoat/Clearcoat Durability Index New Resin Technology Only (TBC/1250) + (X/2000) greater than or equal to 8 X = TICC if TICC is less than 1.2(TCC) otherwise X= TCC Method to Determine: TBC - Stability of U

29、VA free basecoat/clearcoat interface Report TBC (stability of UVA free basecoat/clearcoat interface) defined as the time for clearcoat delamination failure for each color. If the color has not failed by 5000 h, TBC = 5000. ENGINEERING MATERIAL SPECIFICATION WSS-M33J7-A1/A2/A3/B1/B2/B3 Page 13 of 21

30、Copyright 2002, Ford Global Technologies, Inc. TICC - Time to zero UVA absorbance using isolated clearcoat film Prepare quartz slides with clearcoat only. Adjust clearcoat thickness to obtain a starting absorbance (340 nm region) of 2 - 2.5 after clearcoat nominal bake. Measure clearcoat thickness i

31、n micrometers. Calculate absorbance per micrometer. Correct for absorbance per micrometer assuming 100% theoretical mixing of basecoat and clearcoat UVA. Evaluate clearcoat UVA absorbance using a UV-VIS spectrophotometer. Observe the UV spectrum from 450 nm to 250 nm. Determine maximum 340nm region

32、absorbance on initial (baseline) sample and after 1000, 3000 and 5000 hour exposure to Xenon Arc weatherometer (SAE J1960, modified with type “S“ borosilicate inner and outer filters, 0.55 W/m2 radiant exposure). Plot absorbance as a function of exposure time to determine absorbance loss rate (absor

33、bance loss per hour). Calculate TICC (time to zero UVA absorbance using isolated clearcoat film) by the following equation: -1(absorbance/micrometer)(clearcoat film thickness) / (absorbance loss rate) = hours to clearcoat absorbance equals zero. TCC - Time to zero UVA absorbance using full paint sys

34、tem Remove clearcoat from the sample (avoid basecoat layer) with a razor or equivalent scraping device or by in-plane microtomy. Using either solvent extraction from the scraping method or direct measurement with a UV microscope and summing the layers, and evaluate clearcoat UVA absorbance using a U

35、V-VIS spectrophotometer. Observe the UV spectrum from 450 nm to 250 nm. Determine absorbance on initial (baseline) sample and after 1000, 3000 and 5000 hour exposure to Xenon Arc weatherometer (SAE J1960, modified with type “S“ borosilicate inner and outer filters, 0.55 W/m2 radiant exposure). Plot

36、absorbance loss as a function of exposure time to determine UVA loss rate (absorbance loss per hour). Extrapolate UVA loss rate plot to zero absorbance. Determine the exposure hours at zero clearcoat UVA absorbance. Report as TCC ENGINEERING MATERIAL SPECIFICATION WSS-M33J7-A1/A2/A3/B1/B2/B3 Page 14

37、 of 21 Copyright 2002, Ford Global Technologies, Inc. 3.9.3.5 Clearcoat Photooxidation 2.5 max New Technology Clearcoat photooxidation value, max 2.5change in (-OH,-NH)/-CH)ratio Method: Photochemical stability is determined by a comparison of the chemical state change of the topcoat surface before

38、and after exposure to 5000 hour Xenon Arc weatherometer (SAE J1960, modified with type “S“ borosilicate inner and outer filters, 0.55 W/m2 radiant exposure). Evaluate the topcoat photooxidation stability using Fourier Transform Infrared Photo-Acoustic Spectroscopy (FTIR-PAS). Obtain spectra of the s

39、urface layer of topcoat, approximately the top 7 micron, experimentally defined as the photo-acoustic sampling depth by modulation at 3 kHz at 3000 wavenumbers in a rapid-scan FTIR-PAS experiment or 3 kHz phase modulation in a step-scan FTIR-PAS experiment. The reference material, used to obtain the

40、 Relative PAS Intensity spectrum, should be a polymer filled with carbon black to at least 50% for a rapid-scan experiment and to at least 65% for a step-scan experiment. Compression set rubber works best. Resolution - laser sampling at every second laser crossing, 4000 data points, 8K transform, tr

41、iangle apodization, phase corrected. Noise (definition) - root mean square(rms) noise in 3600 - 2500 wavenumbers region based on two carbon black filled polymer background spectra, ratioed to obtain 100% Relative PAS Intensity line. Noise limit - 0.75% rms, Relative PAS Intensity. 100% line - flat f

42、rom 4000 - 2000 wavenumbers, +/- 10% Determine the ratio of the integrated intensity of the O-H plus N-H stretching region to that of the C-H stretching region, i.e. (-OH,-NH)/CH, on a retain and 5000 hour exposed sample. Integrate the intensity under the PAS spectrum (between the spectrum and the b

43、aseline) between 3700 and 2200 wavenumbers (the entire -OH,-NH,-CH stretch region). Integrate the intensity under the PAS spectrum between 3125 and 2750 wavenumbers (the -CH stretch region). Subtract the -CH area from the total area to obtain the (-OH,-NH) area. Divide the (-OH,-NH) area by the -CH

44、area to obtain the (-OH,-NH)/CH area. Subtract (-OH,-NH)/CH at time zero from (-OH,-NH)/CH at 5000 hour exposure to provide the change in the ratio (-OH,-NH)/CH. Report the change in ratio (-OH,-NH)/CH as the photooxidation value. Note: Absorbed water contributes strongly to the (-OH,-NH) area and r

45、esults in a false measure of polymer based OH, NH photooxidation products. Therefore, it is important to remove samples at the end of a dry, light cycle of the weatherometer before FTIR-PAS evaluation. ENGINEERING MATERIAL SPECIFICATION WSS-M33J7-A1/A2/A3/B1/B2/B3 Page 15 of 21 Copyright 2002, Ford

46、Global Technologies, Inc. 3.9.3.6 Adhesion After Water Immersion (FLTM BI 104-01) 16 h (FLTM BI 106-01, Part B) Grade 2, max There shall be no blistering or delamination between any layer of enamel system. To be evaluated on all exposure intervals. 3.10 BASECOAT WSS-M33J7-A1, B1, ONLY FOR INTERIOR A

47、PPLICATIONS (Non-visible or non-UV-exposed areas) 3.10.1 Physical Properties 3.10.1.1 The physical properties of basecoat WSS-M33J7-A1, B1 are determined by requirements of the basecoat/clearcoat enamel. Refer to para 3.3 for specific requirements. 3.10.2 Preparation of Test Panels Panels will be pr

48、epared as in para 3.4 and 4.2. 3.10.3 Appearance 3.10.3.1 Color (FLTM BI 109-01) The color of the basecoat is determined by the requirements of the basecoat/clearcoat enamel to match the Ford master panel. 3.10.3.2 Gloss, All Colors (ASTM D 523, 20 degree Glossmeter) Gloss varies with each color due

49、 to pigmentation requirements. 3.10.3.3 Gloss, After Rebake (ASTM D 523, 20 degree Glossmeter) No more than 4 units decrease in gloss is permitted when rebaked at target bake conditions. 3.10.3.4 General The basecoat shall bake out to a presentable, serviceable film showing no craters, seediness, abnormal roughness or excessive metallic mottling. It shall have reasonable tolerance for ordinary cleaning. ENGINEERING MATERIAL SPECIFICATION WSS-M33J7-A1/A2/A3/B1/B2/B3 Page 16 of 21 Copyright 2002, Ford Global Technologies, Inc. 3.10.4 Film Propertie