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SEMI C36-0705 © SEMI 1981, 2005 8 Previous SEMI Reference # C1.13-96, C1.27-96 C7.24-0697 Grade 1 Grade 2 Grade 3 (Specification) (Specificat ion) (Specificat ion) Arsenic (As) 0.05 ppm max 50 ppb max 50 ppb max Barium (…

SEMI C36-0705 © SEMI 1981, 2005 7

10.5.1.1 Special Reagents

10.5.1.1.1 Phosphoric Acid, Ultra Pure — Use phosphoric acid specified for ultra low metal ion content for

preparation of matrix matched calibration standards.

10.5.1.1.2 Water — The water used for all dilution, calibration, and standards should meet, at a minimum, the

criteria for Type E1.1 in ASTM D5127.

10.5.1.1.3 Internal Standard Stock Solution — An internal standard stock solution containing beryllium (Be),

germanium (Ge), indium (In), and lutetium (Lu) is utilized such that final measured solutions will have

concentrations of Be - 10 ppb, Ge - 20 ppb, In - 5 ppb, and Lu - 5 ppb as internal standard elements.

10.5.1.1.4 External Standard Stock Solution — An external standard stock solution containing the elements in

¶10.5.1 is utilized such that final diluted external calibration standards will have appropriate concentrations for the

measurement of the sample elements.

10.5.2 Sample Preparation — In a clean environment, weigh 5.00 g of sample into a 10 mL polypropylene sample

tube. Add an aliquot of the internal standard stock solution such that the final diluted sample will have the

concentration of internal standard elements in ¶10.5.1.1.3. Dilute contents to 10 mL with Type E1.1 water.

10.5.2.1 Analysis — Analyze elements using inductively coupled plasma mass spectrometry (ICP - MS). Calibrate

the sample elements with matrix matched blank and external standards.

10.6 Trace Anion Analysis – see ¶8.6, which contains procedures for trace anions.

11 Grade 4 Procedures

11.1 This section does not apply to this chemical.

12 Grade 5 Procedures

12.1 This section does not apply to this chemical.

13 Tier A Procedures

13.1 This section does not apply to this chemical.

14 Tier B Procedures

14.1 This section does not apply to this chemical.

15 Tier C Procedures

15.1 This section does not apply to this chemical.

16 Tier D Procedures

16.1 This section does not apply to this chemical.

Table 1 Impurity Limits and Other Requirements for Phosphoric Acid

Previous SEMI Reference # C1.13-96, C1.27-96 C7.24-0697

Grade 1 Grade 2 Grade 3

(Specification) (Specification) (Specification)

Assay (H

) (80%)

79.081.0% 79.081.0% 79.081.0%

Assay (H

) (86%)

85.087.0% 85.087.0% 85.087.0%

Nitrate (NO

) 5 ppm max 5 ppm max 5 ppm max

Sulfate (SO

) -- 12 ppm max 12 ppm max

Total Sulfur (as SO

) 12 ppm max -- --

Chloride (Cl) 1 ppm max 1 ppm max 1 ppm max

Aluminum (Al) 0.5 ppm max 300 ppb max 50 ppb max

Antimony (Sb) 10 ppm max 3500 ppb max 1,000 ppb max

SEMI C36-0705 © SEMI 1981, 2005 8

Previous SEMI Reference # C1.13-96, C1.27-96 C7.24-0697

Grade 1 Grade 2 Grade 3

(Specification) (Specification) (Specification)

Arsenic (As) 0.05 ppm max 50 ppb max 50 ppb max

Barium (Ba) -- -- 50 ppb max

Boron (B) -- -- 50 ppb max

Cadmium (Cd) -- 450 ppb max 50 ppb max

Calcium (Ca) 1.5 ppm max 1100 ppb max 150 ppb max

Chromium (Cr) 0.2 ppm max 200 ppb max 50 ppb max

Cobalt (Co) 0.05 ppm max 50 ppb max 50 ppb max

Copper (Cu) 0.05 ppm max 50 ppb max 50 ppb max

Gold (Au) 0.3 ppm max 150 ppb max 50 ppb max

Iron (Fe) 2.0 ppm max 700 ppb max 100 ppb max

Lead (Pb) 0.3 ppm max 300 ppb max 50 ppb max

Lithium (Li) 0.1 ppm max 100 ppb max 10 ppb max

Magnesium (Mg) 0.2 ppm max 200 ppb max 50 ppb max

Manganese (Mn) 0.1 ppm max 100 ppb max 50 ppb max

Nickel (Ni) 0.2 ppm max 200 ppb max 50 ppb max

Potassium (K) 1.5 ppm max 450 ppb max 150 ppb max

Silicon (Si) -- -- 50 ppb max

Sodium (Na) 2.5 ppm max 500 ppb max 250 ppb max

Strontium (Sr) 0.1 ppm max 100 ppb max 10 ppb max

Titanium (Ti) 0.3 ppm max 300 ppb max 50 ppb max

Zinc (Zn) 2.0 ppm max 400 ppb max 50 ppb max

Particles in bottles:

size, #/mL

(See

) (See

)

Due to the limitations of current particle counters, particle size and number areto be agreed upon between supplier and user.

See SEMI C1, ‘Calibration and Measurement Method for Particles in Liquids’.

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 or equipment mentioned herein. These standards are subject to change without

notice.

By publication of this standard, Semiconductor Equipment and Materials International (SEMI) takes no position

respecting the validity of any patent rights or copyrights asserted in connection with any items 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 of

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

consent of SEMI.

PHOSPHORIC ETCHANTS SEMI C37-0699 © SEMI 1981, 19991

SEMI C37-0699

SPECIFICATION FOR PHOSPHORIC ETCHANTS

This specification was technically approved by the Global Process Chemicals Committee and is the direct

responsibility of the North American Process Chemicals Committee. Current edition approved by the North

American Regional Standards Committee on April 23, 1999. Initially available on SEMI OnLine May 1999;

to be published June 1999. This document replaces SEMI C2.3 in its entirety. Originally published in 1981.

1 Purpose

1.1 The purpose of this document is to standardize

requirements for phosphoric etchants used in the

semiconductor industry and testing procedures to

support those standards. Test methods have been shown

to give statistically valid results. This document also

provides guidelines for grades of phosphoric etchants

for which a need has been identified. In the case of the

guidelines, the test methods may not have been

statistically validated yet.

2 Scope

2.1 The scope of this document is all grades of

phosphoric etchants used in the semiconductor industry.

3 Limitations

3.1 None.

4 Referenced Documents

SEMI C1 — Specifications for Reagents

SEMI C2 — Specifications for Etchants

5 Terminology

5.1 phosphoric etchant — any combination of phos-

phoric, nitric, and acetic acids with the relative compo-

sition expressed in terms of 85% phosphoric acid, 70%

nitric acid, and glacial acetic acid, respectively. In the

expression, all the relative volumes shall be reduced to

a ratio of the smallest whole numbers. For example, a

16:1:2 phosphoric etchant would imply a mixture of 16

volumes of 85% phosphoric acid, 1 volume of 70%

nitric acid, and 2 volumes of glacial acetic acid. If a

component is absent, its relative volume shall be taken

as zero. For example, a 16:1:0 phosphoric etchant

implies that no acetic acid is present.

6 Composition

6.1 The content of each of the components of a

phosphoric etchant shall be expressed on a weight/

weight basis of the 100 percent acid in the total mix-

ture. For the volume-to-weight conversion, the densities

shall be taken as 1.695, 1.415, and 1.050 g/mL for 85%

phosphoric acid, 70% nitric acid, and glacial acetic

acid, respectively.

7 Tolerances

7.1 The tolerances allowed for the absolute percentage

of each of the components of a phosphoric etchant shall

be:

Phosphoric Acid: ± 1.0% (± 0.20 meq/g)

Nitric Acid: ± 0.5% (± 0.08 meq/g)

Acetic Acid: ± 0.5% (± 0.08 meq/g)

8 Requirements

8.1 The requirements for phosphoric etchants for

Grade 1 are listed in Table 1.

9 Grade 1 Procedures

9.1 Total Acidity — Weigh accurately 2.5 to 3.0 g of

sample in a tared weighing bottle. Transfer with water

to a 25 mL beaker and dilute to approximately 100 mL.

Add 10 drops of thymolphthalein indicator solution and

titrate with standardized 1 N sodium hydroxide solution

to the blue endpoint. Calculate the total acidity (A):

Total Acidit

meq

()=

of NaOH

Weight of sample g

()

9.2 Phosphoric Acid — Weigh accurately 2.5 to 3.0 g

of sample in a tared weighing bottle. Quantitatively

transfer the sample with 40 to 60 mL of water into a

platinum or polyfluorocarbon dish. Evaporate the

solution on a steam bath in a hood (1 to 2 hours). Rinse

down the inner sides of the dish with 10 to 15 mL of

water and re-evaporate for 1 hour. Cool and dilute with

50 mL of water. Add 10 drops of thymolphthalein

indicator solution and titrate with standardized 1 N

sodium hydroxide solution to the blue endpoint.

% Phosphoric Acid

of NaOH

4.900

Weight of sample g

()

9.3 Nitric Acid — Weigh accurately a sample

containing 0.9 to 1.1 g of nitric acid in a tared 100 mL

volumetric flask. Dilute to volume with water and mix

thoroughly. Following the manufacturer's directions,

ready a spectrophotometer and set the wavelengh to 302

nm. Transfer the sample solution to a 1 cm fused silica

cell and measure the absorbance versus water. Read

from a previously established calibration curve the

grams of nitric acid present in the sample solulion (see