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SEMI P8-0997 © SE MI 1984, 1997 1 SEMI P8-0997 METHOD FOR THE DETERMIN A TI ON OF WATER IN PHOTORESIST 1 Scope 1.1 T his meth o d is intended for th e app lication of the Karl Fischer titration to the determination of wa…

SEMI P7-0997 © SEMI 1982, 2003 2

ethyl ketone or acetone for typical novolac positive

resists or equivalent and xylene for rubber based

negative resists or equivalent).

4.11 Dry the tube by blowing dry, filtered air through

the viscometer for a few minutes.

4.12 The viscometer should periodically be cleaned

with chromic acid to remove trace organic deposits.

5 Calculation

5.1 Average the flow measurements.

5.2 Kinematic viscosity in cTs = Viscometer constant

× efflux time in seconds.

5.3 Dynamic viscosity in cP = Photoresist density at

25.0° C in g/mL × kinematic viscosity in cSt.

NOTICE: SEMI makes no warranties or

representations as to the suitability of the standards set

forth herein for any particular application. The

determination of the suitability of the standard is solely

the responsibility of the user. Users are cautioned to

refer to manufacturer’s instructions, product labels,

product data sheets, and other relevant literature

respecting any materials mentioned herein. These

standards are subject to change without notice.

The user’s attention is called to the possibility that

compliance with this standard may require use of

copyrighted material or of an invention covered by

patent rights. By publication of this standard, SEMI

takes no position respecting the validity of any patent

rights or copyrights asserted in connection with any

item mentioned in this standard. Users of this standard

are expressly advised that determination of any such

patent rights or copyrights, and the risk of infringement

of such rights, are entirely their own responsibility.

International), 3081 Zanker Road, San Jose, CA 95134. Reproduction o

the contents in whole or in part is forbidden without express written

consent of SEMI.

SEMI P8-0997 © SEMI 1984, 19971

SEMI P8-0997

METHOD FOR THE DETERMINATION OF WATER IN PHOTORESIST

1 Scope

1.1 This method is intended for the application of the

Karl Fischer titration to the determination of water in

photoresists. An electrometric method is used for

determining the endpoint. The procedure is applicable

to most resists that have polymer and solvent systems

fully compatible with Karl Fischer reagent and diluent.

The resist manufacturer should be consulted to

determine if this procedure can be used with the resist

in question.

2 Referenced Documents

2.1 ASTM Standard

E 203 — Water by the Karl Fischer Method

2.2 Reagent Chemicals — Sixth E dition, American

Chemical Society Specifications

3 Apparatus

3.1 Automatic titrator, equipped for Karl Fischer

titrations. The titrator should be equipped with a

titration vessel with a port for sample entry, desiccated

vent tube, and a platinum versus platinum electrode.

Mechanical stirring of the titration solvent should be

provided for. The manufacturer’s suggested operating

procedure should be followed, and the endpoint timer

set for 20 seconds.

3.2 Hypodermic syringes with lock tip, 0.25 mL and

10 mL.

3.3 Syringe needles, 5 to 8 cm length, 20 and 22

gauge.

3.4 Lint-free tissue.

3.5 Analytical balance, capable of weighing to 0.1 mg.

3.6 Reagents

3.6.1 Distilled water.

3.6.2 Methanol, ACS Reagent Grade.

3.6.3 Karl Fischer reagent with a titer of 3.0 (± 5.0)

mg of water per ml of titrant. Typical preparation

involves a one-to-one dilution of stabilized Karl Fischer

reagent with Karl Fischer diluent from the same

supplier.

1 American Society for Testing and Materials, 100 Barr Harbor

Drive, West Conshohoken, PA 19428-2959

4 Procedure

4.1 Standardization of Karl Fischer Reagent — The

Karl Fischer reagent should be standardized

immediately before its use in water determinations.

4.1.1 Install Karl Fischer reagent in the titrator and

flush all lines of the titration equipment at least three

times.

4.1.2 Fill the titration vessel with enough methanol to

cover the electrodes, and seal.

4.1.3 Titrate the methanol automatically with the Karl

Fischer reagent to the endpoint (blank).

4.1.4 Draw 0.1 mL of distilled water into a 0.25 mL

syringe equipped with a 22 gauge needle. Draw the

water from the needle into the syringe by inverting the

syringe (needle up) and drawing the plunger downward

an additional 1 to 2 cm.

4.1.5 Wipe the needle with lint-free tissue.

4.1.6 Weigh the syringe assembly to the nearest 0.1

mg (W

4.1.7 Inject the water into the titration vessel.

4.1.8 Titrate to the same endpoint used for the

methanol blank.

4.1.9 Reweigh the syringe assembly to the nearest 0.1

mg (W

4.1.10 Record the number of milliliters of titrant

consumed (V

4.1.11 Calculate the Karl Fischer factor (F):

F =

mg water injecte

mL KF titrant

−

4.1.12

Repeat the standardizing titration twice and

calculate the mean value for F from the three values

(which should fall within a range of 0.02).

4.2

Determination of Water

4.2.1 Fill the titration vessel with enough methanol to

cover the electrodes, and seal.

4.2.2 Titrate the methanol automatically with the Karl

Fischer reagent to the endpoint (blank).

4.2.3 Flush a dry 10 mL syringe fitted with a 20 gauge

needle several times with the sample to be tested. Fill

the syringe with 3–5 mL of photoresist sample.

4.2.4 Wipe the needle with lint-free tissue.

4.2.5 Weigh the syringe assembly to the nearest 0.1

mg (W

4.2.6 Inject the sample into the titration vessel.

4.2.7

Titrate to the same endpoint used for the

methanol blank.

4.2.8 Reweigh the syringe assembly to the nearest 0.1

mg (W

4.2.9 Record the number of milliliters of titrant used

4.2.10

Calculate the water content of the sample.

Weight % H

mL KF titrant × F

sample weight in mg

×100

× F

− W

×100

4.3 Remarks — Photoresists which contain interfering

compounds (such as aldehydes and ketones) may

require modification of the solvent or titration

conditions. For further information, see Section 3.4 of

ASTM Standard E 203. For some negative

(polyisoprene) photoresists, solubility can be improved

by substituting ethylene glycol as the solvent for

methanol.

NOTICE: These standards do not purport to address

safety issues, if any, associated with their use. It is the

responsibility of the user of these standards to establish

appropriate safety and health practices and determine

the applicability of regulatory limitations prior to use.

SEMI makes no warranties or representations as to the

suitability of the standards set forth herein for any

particular application. The determination of the

suitability of the standard is solely the responsibility of

the user. Users are cautioned to refer to manufacturer’s

instructions, product labels, product data sheets, and

other relevant literature respecting any materials

mentioned herein. These standards are subject to

change without notice.

The user’s attention is called to the possibility that

compliance with this standard may require use of

copyrighted material or of an invention covered by

patent rights. By publication of this standard, SEMI

takes no position respecting the validity of any patent

rights or copyrights asserted in connection with any

item mentioned in this standard. Users of this standard

are expressly advised that determination of any such

patent rights or copyrights, and the risk of infringement

of such rights, are entirely their own responsibility.

International), 3081 Zanker Road, San Jose, CA 95134. Reproduction o

the contents in whole or in part is forbidden without express written

consent of SEMI.