IPC-TM-650 EN 2022 试验方法.pdf - 第149页

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. …

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

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1.0

Scope

This

method is designed to determine the resin

content percent of prepreg which is reinforced with inorganic

fabric, by removal of the resin from the reinforcement using a

burn-off step.

2.0

Applicable Documents

None.

3.0

Test Specimens

3.1 Size

Specimens

shall be approximately 102 mm x 102

mm [4.0 in. x 4.0 in]. If the reinforcement is a continuous fiber

woven fabric, the sides shall be cut on a bias to the orienta-

tion of the fabric.

3.2

Quantity and Sampling

Unless

otherwise specified,

three specimens shall be taken equally spaced across the

width (web) of a roll or from different locations in a predeter-

mined quantity of paneled prepreg, such as an inspection lot.

4.0

Apparatus or Material

4.1 Analytical Balance

Analytical

balance capable of

weighing to the nearest milligram [0.001 gram].

4.2 Muffle Furnace

Muffle

furnace capable of maintaining

550 ± 50°C [1022 ± 90°F].

4.3

Crucible

of sufficient size and type to hold the

specimen when placed in a muffle furnace.

4.4

Cutting Apparatus

Shears

or other equipment

capable of cutting specimens to the specified size.

4.5

Desiccator

Desiccation

chamber capable of maintain-

ing an atmosphere less than 30% R.H., at 23°C [73°F].

5.0

Procedure

5.1 Specimen Preparation

5.1.1

Cut

the specimens to the specified size.

5.1.2

Unless

the prepreg is tested within 10 minutes of its

manufacture, the specimens shall be desiccated for a mini-

mum of 4 hours. For referee testing, the specimens shall be

desiccated.

5.2

Measurement

5.2.1

Each specimen shall be weighed in a previously

weighed crucible to the nearest milligram.

5.2.2

Place

the crucible containing the specimen in the

muffle furnace maintained at 550 ± 50°C [1022 ± 90°F] for 5

minutes, minimum.

5.2.3

Remove

the crucible with contents from the furnace

and place in the desiccator until cooled to room temperature.

Note:

the contents of the crucible shows evidence of glass

fusion, discard the specimen and repeat the test with a new

specimen, except lower the temperature of the muffle furnace

by 50°C [122°F]. If the contents show evidence of incomplete

combustion of the resin, increase the temperature of the fur-

nace or extend the time of combustion. In any case, the

residual glass cloth, after combustion, must be completely

free of resin residue, and show no evidence of glass fusion.

5.2.4

Weigh

the crucible with contents to the nearest milli-

gram.

5.2

Calculation

The

resin content of the prepreg is calcu-

lated as follows:

Resin content (%) = Loss of Weight of Specimen x 100

Original

Weight of Specimen

5.3

Report

The

results shall be recorded in a report indicat-

ing resin content percent for each specimen and the average

of all specimens of the same materials.

6.0 Notes

6.1

Reinforcements

used for prepreg covered by this test

method may be woven or nonwoven, and continuous or non-

continuous fibers, any of which are referred to as fabrics.

6.2

Desiccator Conditions

The

Test Methods Task Group

determined that a great majority of test laboratories are unable

to consistently hold the Relative Humidity in a desiccator to

less than 20%. Based on data from participating company lab

management, the lowest practically feasible RH for use with

the affected IPC Test Methods is 30% maximum.

The

Institute for Interconnecting and Packaging Electronic Circuits

2215 Sanders Road • Northbrook, IL 60062-6135

IPC-TM-650

TEST

METHODS MANUAL

Number

2.3.16

Subject

Resin

Content of Prepreg, by Burn-off

Date

12/94

Revision

Originating Task Group

MIL-P-13949 Test Methods Task Group (7-11b)

Material

in this Test Methods Manual was voluntarily established by Technical Committees of the 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 the IPC.

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