semi合集-English.pdf - 第6688页

SEMI C34-0699 © SEMI 1981, 1999 3 Previous SEMI Refe rence # C2.1-95 C7.19-9 5 Grade 1 Tier A (Specif ication) (G uideline) Cadm iu m ( Cd) 0.3 ppm m ax 10 ppb m ax Calcium (Ca) -- 10 ppb m ax Chrom ium (Cr) 0.2 ppm m ax…

SEMI C34-0699 © SEMI 1981, 1999 MIXED ACID ETCHANTS2

ready a spectrophotometer and set the wavelength to

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

silica cell and measure the absorbance of the sample

solution versus water. Read from a previously

established calibration curve the grams of nitric acid

present in the sample solution (see SEMI C2, Section

3.2, Determination of Nitric Acid by Ultraviolet

Absorption Spectrophotometry).

% Nitric Acid

grams of HNO

calibration curve

100

Weight of sample g

()

9.4 Acetic Acid — The acetic acid content is

calculated by deducting the acidity found for each of

the other components from the value for the total

acidity.

% Acetic Acid

A-

%HF

2.001

−

%HNO

6.302













6.005

9.5 Arsenic and Antimony (as As) — To 50 g of

sample in a polyfluorocarbon dish, add 5 mL of

hydrochloric acid and 5 mL of sulfuric acid. Mix gently

and evaporate in a sandbath in a hood to dense fumes of

sulfur trioxide. Cool, cautiously add 10 mL of water,

and re-evaporate to dense fumes of sulfur trioxide.

Cool, and cautiously wash into a generator flask with

water to make a volume of 35 mL. Proceed as described

in the General Method for Arsenic (and Antimony)

under SEMI C1, Section 3.4.5, starting with the

sentence which begins, "Swirl the flask…" Any red

color in the silver diethyldithiocarbamate solution of

the sample should not exceed that in the standard

containing 0.0015 mg of arsenic (As).

9.6 Trace Element Contents — Determine the levels

of specified trace elements and establish that they do

not exceed the specification limits using a suitable

emission spectrographic procedure (see SEMI C1,

Section 3.5, for Guidelines for Determination of Trace

Elements by Emission Spectrography).

10 Grade 2 Procedures

10.1 This section does not apply to this chemical.

11 Grade 3 Procedures

11.1 This section does not apply to this chemical.

12 Grade 4 Procedures

12.1 This section does not apply to this chemical.

13 Grade 5 Procedures

13.1 This section does not apply to this chemical.

14 VLSI Grade Procedures

14.1 This section does not apply to this chemical.

15 Tier A Procedures

15.1 Standardized test methods are being developed

for all parameters at the purity levels indicated. Until

standardized test methods are published, test

methodology shall be determined by user and producer.

The Process Chemicals Committee considers a test

method to be valid only if there is a documented

recovery study showing a recovery of 75 - 125%.

Recovery is for a known sample spike at 50% of the

specified level.

16 Tier B Procedures

16.1 This section does not apply to this chemical.

17 Tier C Procedures

17.1 This section does not apply to this chemical.

18 Tier D Procedures

18.1 This section does not apply to this chemical.

Table 1 Impurity Limits and Other Requirements for Mixed Acid Etchants

Previous SEMI Reference # C2.1-95 C7.19-95

Grade 1 Tier A

(Specification) (Guideline)

Aluminum (Al) 0.3 ppm max 10 ppb max

Antimony (Sb) -- 10 ppb max

Arsenic (As) -- 10 ppb max

Arsenic and Antimony (as As) 0.03 ppm max --

Barium (Ba) -- 10 ppb max

Boron (B) 0.2 ppm max 10 ppb max

SEMI C34-0699 © SEMI 1981, 19993

Previous SEMI Reference # C2.1-95 C7.19-95

Grade 1 Tier A

(Specification) (Guideline)

Cadmium (Cd) 0.3 ppm max 10 ppb max

Calcium (Ca) -- 10 ppb max

Chromium (Cr) 0.2 ppm max 10 ppb max

Cobalt (Co) -- 10 ppb max

Copper (Cu) 0.1 ppm max 10 ppb max

Gallium (Ga) -- 10 ppb max

Germanium (Ge) -- 10 ppb max

Gold (Au) 0.3 ppm max --

Iron (Fe) 0.3 ppm max 10 ppb max

Lead (Pb) 0.3 ppm max 10 ppb max

Magnesium (Mg) 0.3 ppm max 10 ppb max

Manganese (Mn) -- 10 ppb max

Molybdenum (Mo) -- 10 ppb max

Nickel (Ni) 0.1 ppm max 10 ppb max

Potassium (K) 0.3 ppm max 10 ppb max

Sodium (Na) 0.3 ppm max 10 ppb max

Strontium (Sr) 0.3 ppm max --

Tin (Sn) 0.3 ppm max 10 ppb max

Titanium (Ti) 0.3 ppm max 10 ppb max

Zinc (Zn) 0.3 ppm max 10 ppb max

Particles in bottles:

size, #/mL

≥1.0 µm ≥1.0 µm, 25 max

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.

NITRIC ACID SEMI C35-0301 © SEMI 1979, 20011

SEMI C35-0301

SPECIFICATIONS AND GUIDELINE FOR NITRIC ACID

These specifications and this guideline were technically approved by the Global Process Chemicals

Committee and are the direct responsibility of the North American Process Chemicals Committee. Current

edition approved by the North American Regional Standards Committee on October 17, 1999. Initially

available at www.semi.org February 2001; to be published March 2001. This document replaces SEMI

C1.12, C7.6, and C8.6 in their entirety. Originally published in 1979, 1990, and 1992 respectively;

previously published June 1999.

1 Purpose

1.1 The purpose of this document is to standardize

requirements for nitric acid 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 nitric acid 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 nitric

acid used in the semiconductor industry.

2.2 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.

3 Limitations

3.1 None.

4 Referenced Standards

4.1 SEMI Standards

SEMI C1 — Specifications for Reagents

4.2 ASTM Standards

ASTM D5127 — Standard Guide for Ultra Pure Water

Used in the Electronics and Semiconductor Industry

NOTE 1: As listed or revised, all documents cited shall be the

latest publications of adopted standards.

5 Terminology

5.1 None.

6 Physical Property (for information only)

Density at 25°C

1.42 g/mL

1 American Society for Testing and Materials, 100 Barr Harbor

Drive, West Conshohocken, Pennsylvania 19428-2959, USA.

Telephone: 610.832.9585, Fax: 610.832.9555. Website:

www.astm.org

7 Requirements

7.1 The requirements for nitric acid for Grades 1 and 2

and Tier B are listed in Table 1.

8 Grade 1 Procedures

NOTE 2: Each laboratory is responsible for verifying the

validity of the method within its own operation.

8.1 Assay — Accurately weigh a small glass-stoppered

conical flask containing about 15 mL of water. Deliver

from a pipet about 2 mL of the sample near the water

surface, stopper immediately, cool, and reweigh. Dilute

to about 50 mL with water, add 0.10 mL of methyl

orange indicator solution, and titrate with standardized

1 N sodium hydroxide to a red to yellow color change.

% Assay =

aOH

6.301

Weight of sample (g)

8.2 Color — Dilute 2.0 mL of platinum-cobalt stock

solution (APHA No. 500) to 100 mL with water.

Compare this standard (APHA No. 10) with 100 mL of

sample in Nessler tubes. View vertically over a white

background. The sample must be no darker than the

standard.

8.3 Chloride — Dilute 84 mL (120 g) of sample with

10 mL of water, add 1 mL of silver nitrate reagent

solution, and evaporate to dryness on a steam bath in a

hood. Dissolve the residue in 0.5 mL of ammonium

hydroxide, dilute with 20 mL of water, and add 1.5 mL

of nitric acid. Any turbidity produced should be no

greater than that produced when 0.01 mg of chloride

ion (Cl) is treated as the sample.

8.4 Phosphate — To 35 mL (50 g) of sample add 10

mL of sodium carbonate reagent solution and evaporate

to dryness on a steam bath in a hood. Dissolve the

residue in 25 mL of 0.5 N sulfuric acid. Add 1 mL of

ammonium molybdate reagent solution and 1 mL of p-

(methylamino)phenol sulfate reagent solution. Allow to

stand at room temperature for 2 hours. Any blue color

produced should be no greater than that produced when

0.01 mg of phosphate ion (PO

) is treated as the sample.

8.5 Sulfate — To 70 mL (100 g) of sample add 10 mL

of sodium carbonate reagent solution and evaporate to