IPC-TM-650 EN 2022 试验方法.pdf - 第148页

1 Scope This is an electrogravimetric method for determin- ing the purity of copper foil or plating. 2 Applicable Documents None 3 Test Specimens Each copper specimen must weigh approximately five grams and be raw copper…

5.2.1.3

Immerse

the specimens in a 10% solution of oxalic

acid in water at 16°C to 32°C for 15 to 20 minutes. Provide

gentle circulation of the oxalic acid solution during this period.

Flush the specimens with running tap water at 16°C to 32°C.

Caution: Oxalic acid is toxic.

5.2.1.4

Scrub

the specimens with Grade FFF pumice to

remove resist, or wipe off the resist with a lint-free cloth moist-

ened with a suitable solvent (i.e., methylethyl ketone, trichlor-

ethylene, or toluol). In cleaning the specimens, care must be

exercised to avoid abrading the adhesive layer with the pum-

ice or attacking the adhesive or laminate with the solvent.

Specimens not involving the use of resist need not be

scrubbed.

5.2.1.5

Scrub

the specimens with a plastic-bristled brush

under running tap water at 16°C to 32°C and rinse for 30

minutes.

5.2.1.6

Rinse

the specimen in distilled water.

5.2.1.7

Dry

the specimens for one hour in an oven at 80°C

± 3°C. If specimens are for electrical tests, handle only with

rubber or polyethylene gloves.

5.2.2

Method B

5.2.2.1

Remove

foil from the specimen using a solution

containing 298g±10perliter of ammonium persulfate and

15.5 mL ± 1.0 per liter of sulfuric acid, specific gravity 1.836

(66°Be). The temperature shall be 43°C ± 3°C.

5.2.2.2

Rinse

the specimens thoroughly in running water

and dry with a clean air blast.

5.2.2.3

Dry

the specimens in an oven at 80°C ± 3°C for one

hour and allow the specimens to cool.

5.3

Petrolatum Evaluation

5.3.1

Drill

1.5 mm holes in the pads of the 3 mm lines with

good fabricating practice.

5.3.2

Remove

the developed KPR by rubbing the pattern

lightly with cold trichlorethylene liquid. Rinse in water. Scrub

the specimens with FFF pumice and water with a strong

bristle brush.

5.3.3

Plate

per MIL-P-13949. Deoxidize by dipping in 10%

hydrochloric acid for two minutes and wash in running water

for five minutes. Dry 30 minutes, minimum, at 105°C to

110°C.

5.3.4 Coat

the etched copper surface with white petrola-

tum. Specimens shall be immersed horizontally in solder

6.5mm below the surface for 20 ± 1 seconds at 260°C +5°C/-

0°C) measured 25 mm below the surface.

5.3.5

Remove

the petrolatum from the surface of the speci-

men with a two minute scrub in cold trichlorethylene, followed

by a one minute rinse in hot trichlorethylene.

5.3.6

Inspect

the surface for weave exposure, measling,

crazing, resin loss, delamination and blistering.

5.3.7

Test

four 0.8 mm lines on the specimen for peel

strength and report the average value for the four lines. This

test shall be performed in accordance with Method 2.4.8.

5.4

Report

5.4.1

The

results of the testing by this test method shall be

reported in a written report, which contains the following as a

minimum:

1. Certification that the test was performed in accordance

with this test method

2. Identification of specimens tested

3. Test results for each of the specimens tested, including the

results of the visual inspections and peel tests

IPC-TM-650

Number

2.3.14

Subject

Print,

Etch, and Plate Test

Date

4/73

Revision

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Scope

This

is an electrogravimetric method for determin-

ing the purity of copper foil or plating.

Applicable Documents

None

Test Specimens

Each

copper specimen must weigh

approximately five grams and be raw copper foil or plating

without treatment.

Apparatus or Material

4.1 Electrodes for Electrogravimetric Analysis

plati-

num gauze cathode. A platinum gauze rotating anode or a

spiral platinum wire anode.

4.2

Reagents

4.2.1

Acid

mixture for dissolving sample: Add 300 ml of

concentrated H

slowly

with stirring to 750 ml of water.

Cool and add 210 ml of HNO

4.2.2

For

cleaning the sample use 5% H

For cleaning

of the interior of the glassware use diluted HNO

(one

part

acid plus three parts distilled or deionized water by volume).

4.2.3

For

final rinsing use absolute methanol or equivalent.

4.2.4

Distilled

or deionized water.

4.3

Other apparatus

4.3.1

Fume

hood for removing fumes from dissolution.

4.3.2

Hot

plate for heating the test solution to 80-90 °C

[176-194 °F].

4.3.3

Analytical

balance capable of weighing copper sample

and platinum cathode to the nearest 0.1 mg.

4.3.4

Oven

for drying the specimen and cathode at approxi-

mately 110 °C [230 °F].

4.3.5

Current

source capable of supplying a current density

based on the cathode area of at least 0.6 A/dm

ASF].

4.3.6

Tall-form

180 ml to 300 ml lipless beaker provided

with a close-fitting split cover.

Procedure

5.1 Test

5.1.1

Clean

the copper foil by dipping in 5% H

room

temperature, wash thoroughly in tap water, then distilled

water, rinse in absolute methanol or equivalent, dry for a few

minutes in hot air oven at 110 °C [230 °F] and cool in a des-

iccator. Weigh the copper test specimen to the nearest

0.1 mg and transfer to a tall-form 180 ml to 300 ml lipless

beaker provided with a close-fitting cover. Place the beaker

into a fume hood.

5.1.2

Add

45 ml of H

-HNO

mixture

and allow to stand

covered for a few minutes until reaction has nearly ceased.

5.1.3

Heat

at a temperature of 80-90 °C [176-194 °F] until

dissolution is complete and brown fumes have been expelled.

Never boil.

5.1.4

Cool

slightly and carefully wash down the cover and

insides of the beaker with distilled water and dilute the solu-

tion sufficiently to cover the cathode cylinder. The purpose of

the wash is to make sure that any of the ionized copper that

may be on the cover or inside surface of the beaker is in the

solution from which the copper is to be reduced by electro-

plating onto the platinum cathode.

5.1.5

Allow

solution to cool to ambient conditions.

5.1.6 Weigh

the cathode to the nearest 0.1 mg.

5.1.7

Insert

the electrodes in the solution, cover to prevent

splashing or evaporation, and electrolyze at a current density

of 0.6 A/dm

ASF]. (When a current density of 0.6 A/dm

used,

the electrolysis takes about 16 hours and is conve-

niently carried on overnight.)

5.1.8

When

the solution becomes colorless, reduce the cur-

rent density to about 0.3 A/dm

ASF] and wash down the

cover glasses, electrode stems and the inside of the beaker.

2215

Sanders Road

Northbrook, IL 60062-6135

IPC-TM-650

TEST

METHODS MANUAL

Number

2.3.15

Subject

Purity,

Copper Foil or Plating

Date

05/04

Revision

Originating Task Group

Rigid Printed Board Performance Task Group

(D-33a)

Material

in this Test Methods Manual was voluntarily established by Technical Committees of IPC. This material is advisory only

and its use or adaptation is entirely voluntary. IPC disclaims all liability of any kind as to the use, application, or adaptation of this

material. Users are also wholly responsible for protecting themselves against all claims or liabilities for patent infringement.

Equipment referenced is for the convenience of the user and does not imply endorsement by IPC.

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5.1.9

Continue

the electrolysis until the deposition of the

copper is complete, as indicated by failure to plate on a new

surface of the electrode stem when the level of the solution is

raised by adding distilled water. (Metal added to solution by

washing glass and cover will typically plate in approximately

one hour.)

5.1.10

Without

interrupting the current, remove the elec-

trodes from the solution.

5.1.11 Remove

the cathode. Wash with distilled water. Dip

in absolute methanol or equivalent and dry rapidly in a hot air

oven at 110 °C [230 °F] (approximately five minutes). Cool to

ambient in a desiccator and weigh to the nearest 0.1 mg.

5.1.12

Shut

off current supply to just set up.

5.2

Calculations

5.2.1

Calculate

the percentage of copper by weight by the

following method:

Weight of copper recovered C

A-B

where:

A = weight of cathode plus deposited copper in grams.

B = initial weight of the cathode in grams

Copper, by weight (%) = (C

)

X 100

where:

weight of copper recovered in grams

initial weight of copper test sample in grams

6 Notes

6.1

Interferences

this method any silver present in the

test sample is deposited with the copper, and is reported as

copper.

IPC-TM-650

Number

2.3.15

Subject

Purity,

Copper Foil or Plating

Date

05/04

Revision

age2of2

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