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SEMI C3.55-02 00 © SEMI 2000 4 5.5.2.5 Cali bration St andards — 1–5 p p m ( mole/ mo l e) 5.5.3 Operating Procedure — (see S E M I C3, Section 6, Gas Ch ro m atography for standard proce dures). 5.5.3.1 Inject the calib…

SEMI C3.55-0200 © SEMI 20003

5.2.4 Calibration

5.2.4.1 Run titration blank consisting of 150 mL

deionized water.

5.2.4.2 Calculate the concentration of chloride, using

the formula below. The result may not exceed the

specification in Section 2 of this standard.

mL mL

wt.NaCl(g)

100.0mL

60.66%Cl

100%NaCl

100mL

0.005l

35.453g / mole

0.082atmL/ moleK

28.316L

sample blank

standard

blank

−

××

−

××

mL mL

wt.NaCl(g)

100.0mL

60.66%Cl

100%NaCl

100mL

0.005l

35.453g / mole

0.082atmL/ moleK

28.316L

sample blank

standard

blank

−

××

−

××

1 × 10

ppm = ppm Cl-

5.3 Hydrocarbons C

– C

— This procedure is for the

determination of hydrocarbons (methane, ethane, and

propane) in silane using a gas chromatograph with a

flame ionization detector.

5.3.1 Detection Limit — 50 ppb (mole/mole)

5.3.2 Instrument Parameters

5.3.2.1 Columns:

Column 1: VZ-10, 60/80, 2 m (6.6 ft) by 3.2 mm (1/8

in) OD by 2.2 mm (0.085 in) ID stainless

steel;

Column 2: VZ-10, 60/80, 1 m (3.3 ft) by 3.2 mm (1/8

in) OD by 2.2 mm (0.085 in) ID stainless

steel;

or equivalent.

5.3.2.2 Carrier Flow — 30 mL/min nitrogen

5.3.2.3 Sample Volume — 10 mL

5.3.2.4 Temperatures:

Detector 150°C

Column Oven 45°C

5.3.3 Calibration Standards — 1 ppm (mole/mole) for

all components to be tested, balance helium.

5.3.4 Operating Procedures — (see SEMI C3, Section

6, Gas Chromatography for standard procedures).

5.3.4.1 Inject the calibration standard and sample as

described in Section 6.6 of SEMI C3. The order of

elution is methane, ethane, propane and butane (see

NOTE 2).

5.3.4.2 Compare the average peak area of the methane

peak in the calibration standard to that of the

hydrocarbons found in the silane sample being tested.

Calculate the concentrations of the analytes as

described in Section 6.8 of SEMI C3 based on the

methane response. The result shall be reported in the

unit of concentration needed and to the number of

significant digits of the variable with the least number

of significant digits. This value may not exceed that

specified in Section 2.

5.4

Hydrogen — This procedure is for the

determination of hydrogen in silane using a gas

chromatograph with a thermal conductivity detector.

5.4.1 Detection Limit — 15 ppm (mole/mole)

5.4.2 Instrument Parameters

5.4.2.1 Columns:

Molecular sieve 5A, 2.4 m (8 ft) by 6.4 mm (1/4 in) OD

by 4.7 mm (0.185 in) ID, or equivalent.

5.4.2.2

Carrier Flow — 30 mL/min argon

5.4.2.3 Sample Volume — 1.0 mL

5.4.2.4 Temperatures:

Detector 40°C

Column Oven 40°C

5.4.3 Calibration Standards — 20–100 ppm

(mole/mole), balance argon.

5.4.4 Operating Procedures — (see SEMI C3, Section

6, Gas Chromatography for standard procedures)

5.4.4.1 Inject the calibration standard and sample as

described in Section 6.6 of SEMI C3. (See NOTE 2.)

5.4.4.2 Compare the average peak area of the

hydrogen peak in the calibration standard to that of the

hydrogen found in the silane sample being tested.

Calculate the concentrations of the analytes as

described in Section 6.8 of SEMI C3 based on the

methane response. The result shall be reported in the

unit of concentration needed and to the number of

significant digits of the variable with the least number

of significant digits. This value may not exceed that

specified in Section 2.

5.5

Disiloxane, Disilane and Methyl Silane — This

procedure is for the determination of disiloxane,

disilane and methyl silane in silane using a gas

chromatograph with flame ionization detector.

5.5.1 Detection Limit — 0.1 ppm (mole/mole)

5.5.2 Instrument Parameters

5.5.2.1 Column:

28% DC-200 on Chromosorb PAW, 45/60 mesh, 14 m

(46 ft) SS, or equivalent.

5.5.2.2 Carrier Flow — 30 mL/min helium

5.5.2.3 Sample Volume — 2 mL

5.5.2.4 Temperatures — Column 60°C

SEMI C3.55-0200 © SEMI 2000 4

5.5.2.5 Calibration Standards — 1–5 ppm (mole/

mole)

5.5.3 Operating Procedure — (see SEMI C3, Section

6, Gas Chromatography for standard procedures).

5.5.3.1 Inject the calibration standard and sample as

described in Section 6.6 of SEMI C3. The order of

elution is silane matrix, methyl silane, siloxane (for

information only) and disilane. (See NOTE 2.)

5.5.3.2 Compare the average peak area of the

components being measured in the calibration standard

to that of the same analytes found in the silane sample

being tested. Calculate the concentrations of the

analytes as described in Section 6.8 of SEMI C3. The

result shall be reported in the unit of concentration

needed and to the number of significant digits of the

variable with the least number of significant digits.

This value may not exceed that specified in Section 2.

5.6

Water — This procedure is for the determination

of trace moisture (water) in silane using a vibrating

quartz hygrometer.

5.6.1 Detection Limit — 0.1 ppm (vol/vol)

5.6.2 Instrument Parameters

5.6.2.1 Flow Requirements — Set the sample pressure

and flow rate in accordance with the instrument

manufacturer’s instructions.

5.6.3 Calibration Standards — Check the hygrometer

calibration with silane using an external permeation

device. Construct a calibration curve which contains at

least three points covering the range of interest. The

standards employed will have been verified

independently on a condensation dewpoint/frostpoint

hygrometer. (See Figure 2.)

5.6.4

Operating Procedure — At the first start-up of

the hygrometer, calibrate it with moisture standards in

silane. Then check the calibration once a month and

modify the hygrometer if necessary. Direct standard to

unit with stainless lines which have been purged. Note

that silane is spontaneously flammable. Thus the

experimental set-up should be leak-free and thoroughly

purged before the introduction of silane. Obtain

representative sample of the gas to be analyzed and

direct to the unit. Wait until the equilibrium and read

the moisture content. The result may not exceed the

specification.

5.6.4.1

Construct a calibration curve with previously

verified standards. Direct standard to unit with

stainless steel lines which have been purged.

5.6.4.2 Obtain representative sample of gas to be

analyzed and direct to unit as with the standards. (See

NOTE 1.)

5.6.4.3

Construct a calibration curve and determine the

ppm moisture content in sample gas. The result may

not exceed the specification in Section 2 of this

standard.

5.7 Elemental Analysis in Deposited Layer —

Procedures for the analysis of elemental impurities in

deposited layers of polysilicon should be designated

and should be referenced from a recognized industry

standard (including but not limited to ISO, ASTM,

etc.).

5.7.1 Typical Detection Limits

Compound Detection Limit

Carbon (C) 0.2 ppma

Oxygen (O) 0.2 ppma

Boron (B) 0.02 ppba

Aluminum (Al) 0.02 ppba

Gallium (Ga) 0.02 ppba

Phosphorus (P) 0.02 ppba

Arsenic (As) 0.02 ppba

Antimony (Sb) 0.02 ppba

Iron (Fe) 0.3 ppba

Chromium (Cr) 0.01 ppba

Nickel (Ni) 0.2 ppba

Copper (Cu) 0.02 ppba

Zinc (Zn) 0.03 ppba

5.8 Resistivity — Procedures for the measurement of

resistivity in deposited layers of polysilicon should be

designated and should be referenced from a recognized

industry standard (including but not limited to ISO,

ASTM, etc.).

NOTE 1: Before performing this or any other analytical

operation it is necessary to perform the following:

• Familiarize yourself with the products involved and the

potential hazards by consulting the MSDS's for all

hazardous substances involved and by consulting the

CGA’s “Handbook of Compressed Gases” for all gases

involved.

• Know how to safely handle and store each hazardous gas

by consulting the applicable CGA pamphlets.

• Use all necessary and applicable personal protective

equipment.

• Follow all instructions relative to the safe operation of

the equipment by consulting the LAC Safety Manual and

applicable equipment manufacturers manual(s).

It must be noted that silane is a pyrophoric gas and all sample

plumbing must be purged of air completely before introducing

silane. Extra special attention must be paid to leak checking

all connections and checking the vent plumbing to be certain

that effluents are vented properly. If there are any

questionable connections or leaks, report this to the supervisor

immediately and do not proceed with the analysis.

NOTE 2: Introduce the calibration standard as many times as

necessary to achieve the desired precision. Detection limit

calculated on these calibrations should achieve at least that

listed for this procedure.

Figure 1

Chloride Scrubbing Apparatus

Figure 2

Moisture Analysis in Silane