MIL- STD-883F 2004 TEST METHOD STANDARD MICROCIRCUITS.pdf - 第177页

MIL-STD-883F METHOD 1034.1 18 June 2004 3 c. Tak e one of the 1000 ml beakers of premi x and pour about 200 ml of t he premix into t he funnel. W hen the s oluti on has drai ned through t he funnel, t urn off the vacuum …

MIL-STD-883F

METHOD 1034.1

18 June 2004

3.1 Dye penetration procedure outline

a. Mix dye solution.

Loctite Resinol RTC 18018

Loctite Accelerator for PMS 17724

Morton Fluorescent Yellow G

Note: Solutions with an established or verifiable equivalent makeup and performance may be used.

b. Place the parts in a beaker of the dye solution.

c. Place the beaker in the vacuum oven.

d. Leave the beaker for 15 minutes at a vacuum of 1 to 0.3 torr.

e. Bring the vacuum oven back to atmospheric pressure, then wait 15 minutes.

f. Remove the parts from the dye solution.

g. Wipe off the parts to remove the excess dye.

h. Heat the parts in the oven at 100°C for 1 hour to harden the polymer mixture.

i. Mount the parts for crosssectioning.

j. Crosssection the parts.

k. View the parts under magnification.

l. Take an optical photo of the crosssection.

m. Take a photo of the crosssection under UV to document the depth of penetration.

NOTE: Lay down a double layer of protective mats before starting this procedure. The dye spreads and stains quite

easily. Be sure to wear the appropriate protective apparel, which includes chemical gloves, goggles, and a lab

coat.

3.1.1 PREMIX solution preparation

. Prepare a stock solution (PREMIX solution) of the resinol and yellow dye.

3.1.1.1 Mixing the solution

. A mixture of 100 parts resinol to 1 part yellow dye powder is required to make the PREMIX

solution.

a. Measure and pour 2000 ml of resinol into a beaker.

b. Measure 20 g of yellow dye and pour it into the 2000 ml of resinol. Stir this mixture for 5 minutes, then separate

the mixture into two 1000 ml beakers to make it easier to work with. Place a mixing magnet in each of the

beakers, then place the beakers on mixing plates. Stir the mixtures for two to three hours.

3.1.1.2 Filtering the PREMIX

. The PREMIX must be filtered to ensure that any undesolved particles are removed from

the solution.

a. Take a WHATMAN 42 filter and place it in the 11 cm Buckner funnel. Place the funnel adapter on the stem of the

funnel. Then place the funnel into the top of the bell jar. Place a 250 ml beaker on the bell jar base. Place the

bell jar and funnel over the beaker on the bell jar base.

b. Turn on the vacuum pump.

MIL-STD-883F

METHOD 1034.1

18 June 2004

c. Take one of the 1000 ml beakers of premix and pour about 200 ml of the premix into the funnel. When the solution

has drained through the funnel, turn off the vacuum pump, and pour the filtered solution into an empty container

marked "RESINOL AND YELLOW DYE G MIXTURE". Repeat this process until all of the solution is filtered.

d. Remove the filter and replace it with a new one.

e. Repeat step 3 with the second 1000 ml beaker of solution.

f. Wash the beakers in a soap and water solution.

3.1.2 Setup of PREMIX and accelerator

. A mixture of 200,000 parts PREMIX to 1 part accelerator is required. Due to

the small amount of accelerator required, the mixture of premix and accelerator is performed in two steps. First a 200:1

mixture is prepared, then a 1000:1 mixture is made utilizing the 200:1 solution in order to achieve a 200,000:1 mixture.

a. Measure out 10 ml of premix (resinol/yellow dye stock solution) with a graduated cylinder. Pour the 10 ml into a

small beaker.

b. Insert the Drummond pipette and plunger into the accelerator solution. The glass pipette has two green markings.

The first marking is 0.05 ml, and the second marking is 0.1 ml.

c. Draw up 0.05 ml (1st green mark) of accelerator, and mix it into the 10 ml of premix.

d. Place a mixing magnet into the solution, and place the beaker on the mixing plate. Stir the solution for 5 minutes.

This completes the mixing of the 200:1 premix:accelerator solution.

e. Clean the pipette and plunger in a soap and water solution. They must be clean when they are used in step h.

f. Fill a graduated cylinder with the amount of premix (resinol/yellow dye solution) that is needed to submerse the

devices requiring dye penetration. Most jobs will require 25 ml of solution. The amount will vary depending upon

the number and size of the devices in the job.

g. Pour the 25 ml of premix (or the desired amount) into a small beaker.

h. Using a clean plunger and pipette, a small amount of the 200:1 premix:accelerator solution is added to the desired

amount of premix. For 25 ml of premix, 0.025 ml of 200:1 premix/accelerator solution is used. Other typical

mixtures are listed below.

10 ml premix : 0.010 ml 200:1 premix/accelerator solution

25 ml premix : 0.025 ml 200:1 premix/accelerator solution

50 ml premix : 0.050 ml 200:1 premix/accelerator solution

75 ml premix : 0.075 ml 200:1 premix/accelerator solution

100 ml premix : 0.100 ml 200:1 premix/accelerator solution

i. Place a mixing magnet into the solution and place on a mixing plate for 5 minutes. This creates the final

200,000:1 premix:accelerator solution.

j. The 200:1 solution can now be discarded by placing it in the bottle marked "RESINOL, YELLOW DYE G, and

ACCELERATOR WASTE".

k. Clean all of the glassware and pipettes with a soap and water solution.

MIL-STD-883F

METHOD 1034.1

18 June 2004

3.1.3 Vacuum setup.

a. Place the parts in the premix/accelerator mixture.

b. Place the beaker in a petri dish to catch any spill solution that spills over during the vacuum operation.

c. Place a larger beaker over the beaker with solution in it to prevent splattering all over the vacuum oven.

3.1.3.1 Vacuum

. Many vacuum ovens can be used for this procedure as long as the oven is able to reach 1 to 0.3 torr.

The oven should have a gauge that can accurately measure the pressure at this level. One method is given below.

a. Place the door of the vacuum chamber by unscrewing the handle counter clockwise.

b. Place the beaker set-up into the vacuum chamber.

c. Close the vacuum oven door. Close the door latch and turn it clockwise until tight.

d. Close the valves on both sides of the oven. The vacuum is monitored by the gauge on the top of the oven. The

vacuum meter is connected to the outtake of the oven.

e. Turn on the vacuum pump.

f. Monitor the outgassing of the solution while its under vacuum. Violent outgassing will start at approximately 10

torr. The valves on either side of the oven (one on the left side and one on the right side of the oven) can be

cracked open to lessen the vacuum on the inside of the oven. By doing this, the outgassing can be controlled, so

that the mixture doesn't spill over.

g. Once the outgassing stops, close the valves on the vacuum oven and wait for the pressure to decrease to 1 torr.

The working vacuum for the procedure is 1 to 0.3 torr.

h. Once the Granville-Phillips vacuum gauge reaches 1 torr, wait for 15 minutes.

3.1.3.2 Post vacuum procedure

a. At the end of 15 minutes, turn off the vacuum pump.

b. Open both of the intake valves until the vacuum inside the chamber is equal to the outside pressure. Leave the

devices in this state for 15 minutes.

c. At the end of the 15 minutes, open the door and remove the beakers from the vacuum chamber.

3.1.4 Cleaning the devices

a. Remove the devices from the solution.

b. Pad off the excess solution with a paper towel and cotton swab.

c. The remaining mixture can now be discarded into the bottle marked "RESINOL, YELLOW DYE G, AND

ACCELERATOR WASTE".

d. The beakers, pipettes, and glassware can all be cleaned in soap and water.

3.1.5 Baking the devices

a. Place the devices in a petri dish, and place the dish into an oven preheated to 100 degrees C. Bake for 1 hour.

b. After the bake, the parts can be mounted for crosssectioning.