1、 FORD LABORATORY TEST METHODBU 153-01Printed copies are uncontrolled Copyright 2005, Ford Global Technologies, LLC Page 1 of 4 RHEOLOGICAL TESTING FOR DETERMINING THE VISCOSITY OF ADHESIVES AND SEALERS Application This method is used to evaluate the viscosity of adhesives and sealers as a function o
2、f shear rate. Such properties help to optimize the processing of these materials throughout the manufacturing process, particularly in the flow of these materials through the dispensing system, from the pump to the nozzle. Apparatus Required Rheometer An extrusion rheometer, equipped with an orifice
3、 of 0.32 cm diameter and at least 3.2 cm length. The rheometer should be capable of determining the rheological properties of substances that will flow at room temperature with the application of pressure from 0 to 100 psi, in a viscosity range of 1 to 1 million centipoises. For example, Burrell Sev
4、ers Model A120 Rheometer equipped with an orifice of 0.32 cm inner diameter and 5 cm length, and a sample cylinder of 4 cm inner diameter and 29.5 cm length. (Figure 1) Temperature Control Devices (a) An oven capable of achieving a temperature range of 100 125 F +/- 2 F (b) A refrigerator or freezer
5、 capable of achieving a temperature of 54 F +/- 2 F Miscellaneous (a) Balance to make weight measurements (b) Thermocouple or similar device to make temperature measurements. For example, Omega Thermocouple Probe machined into rheometer sample cylinder, to measure material temperature (Figure 1) (c)
6、 Paper cups (d) Stopwatch Materials Required Adhesive/Sealer Adhesives and sealers (Ford specifications WSB-M4G60-B4, WSB-M4G348-A/A2, WSS-M4G348-A3/A4 and WSB-M2G388-A) will be tested according to this test method. Conditioning and Test Conditions All test values indicated herein are based on mater
7、ial conditioned in a controlled atmosphere of 23 +/- 2 C and 50 +/- 5% relative humidity for not less than 24 h prior to testing. Materials will be tested at 23 C unless otherwise stated. Date Action Revisions 2005 03 08 Activated M. Brutto FORD LABORATORY TEST METHODBU 153-01Printed copies are unco
8、ntrolled Copyright 2005, Ford Global Technologies, LLC Page 2 of 4 Procedure 1. Load material into rheometer and attach orifice of 0.32 cm diameter. Fill the orifice with material by applying a small amount of pressure. 2. Three different tests should be run under the following conditions: a. Test O
9、ne: Room Temperature Testing - 23 25 C (73 77 F) 1. Extrude material through orifice into a paper cup, for 1 minute, at the following pressures: a. 5 psi b. 10 psi c. 20 psi d. 30 psi e. 50 psi f. 70 psi g. 90 psi 2. For each pressure, record the weight of material extruded in 1 minute. 3. Run three
10、 replicates per pressure. b. Test Two: Elevated Temperature Testing - 43 46C (110 115F) 1. Condition the rheometer sample cylinder in an oven for 30 minutes at 52 C (125 F). Remove sample cylinder from oven and run test listed in Step 2 below, while maintaining a material temperature of 43 46 C (110
11、 115 F). Material temperature should be monitored throughout the experiment using a thermocouple probe or similar device. Generally, two pressures can be run at one time; then sample cylinder should be re-conditioned in an oven for an additional 30 minutes at 52 C (125 F). 2. Extrude adhesive throug
12、h orifice into a paper cup, for 30 seconds, at the following pressures: a. 5 psi b. 10 psi c. 20 psi d. 30 psi e. 50 psi f. 70 psi g. 90 psi 3. For each pressure, record the weight of material extruded in 30 seconds. 4. Run three replicates per pressure. c. Test Three: Cold Temperature Testing -12 1
13、3 C (54 56 F) 1. Condition the rheometer sample cylinder in a refrigerator or freezer until the material reaches a temperature of 12 C (54 F). Remove sample cylinder from refrigerator/freezer and run test listed in Step 2 below, while maintaining a material temperature of 12 13 C (54 56 F). Material
14、 temperature should be monitored throughout the experiment using a thermocouple probe or similar device. Generally, two pressures can be run at one time; then sample cylinder should be re-conditioned in refrigerator / freezer until material reaches a temperature of 12 C (54 F). 2. Extrude adhesive t
15、hrough orifice into a paper cup, for 1 minute, at the following pressures: a. 10 psi b. 20 psi c. 30 psi d. 50 psi e. 70 psi f. 90 psi g. 95 psi 2. For each pressure, record the weight of material extruded in 1 minute. 3. Run three replicates per pressure. FORD LABORATORY TEST METHODBU 153-01Printed
16、 copies are uncontrolled Copyright 2005, Ford Global Technologies, LLC Page 3 of 4 3. Calculate Shear Rate (1/s) and Viscosity (Poise) for each test conducted (calculate the average of three replicates). The equations for an extrusion rheometer are derived from the capillary rheometer equations and
17、are as follows: Shear Rate = 4Q / ( R3) Units of 1/sViscosity = P R4/ (8LQ) Units of Poise Where: Q = Quantity extruded in milliliters (or approximately cc) per second R = Radius of orifice in cm. L = Length of orifice in cm. P = Pressure in dynes per square centimeter (Dynes / cm2= (6.9 x 104) psi)
18、 4. Plot Viscosity (poise) versus Shear Rate (1/s) for the three tests performed in step 2. The shear rate should be plotted on a logarithmic scale. A Power Law fit of the data may be performed. Tests 1, 2 and 3 should be plotted on the same graph. An example is shown in Figure 2. The shear rate ran
19、ge should extend approximately from 0.5 or 1 to 100 1/s if possible. NOTE: It may not be possible to extrude high viscosity materials at low pressures (5, 10, and possibly 20 psi). NOTE: For low viscosity materials, it may not be possible to achieve low shear rates (0.5 1 1/s) with a 0.32 cm diamete
20、r orifice. In these cases, a smaller diameter orifice can be used to achieve these low shear rates. Alternatively, these low shear rate points can be calculated using Power Law fit equations. Report 1. Adhesive identification including: Manufacturer, code number, type, date manufactured, lot number.
21、 2. Conditioning procedure for material prior to testing. 3. Test conditions including: Orifice radius, orifice length, material temperature and pressures for each test. 4. Graph of Viscosity versus Shear Rate for each test performed and each adhesive. The shear rate should be plotted on a logarithm
22、ic scale. References 1. Macosko, C.W., Rheology: Principles, Measurements, and Applications New York: Wiley-VCH, 1994. 2. SAE J1524, Method of Viscosity Test for Automotive Type Adhesives, Sealers, and Deadeners August 1995. FORD LABORATORY TEST METHODBU 153-01Printed copies are uncontrolled Copyrig
23、ht 2005, Ford Global Technologies, LLC Page 4 of 4 Figure 1: Burrell Severs Model A120 Rheometer Burrell Severs Rheology Data60B4 Material01000020000300004000050000600000.1 1.0 10.0 100.0 1000.0 10000.0Shear Rate (1/s)Viscosity(poise)55FRoom Temperature115FFigure 2: Example Plot of Viscosity versus Shear Rate
