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SEMI C56-0305 © SEMI 2005 3 9 Analytical Procedures for Purity of 97% of Dichlorosilane NOTE 1: The sample is extremely flammable and corrosive. Test for leaks before sampli ng. Ensure good electrical ground ing. 9.1 Oth…

SEMI C56-0305 © SEMI 2005 2

Table 1 Impurity and Other Requirements for Various Grades of Dichlorosilane

Previous SEMI Reference #

C3.18-1102

(Specification)

C3.31-1102

(Specification)

Purity 97% 99%

Impurities Maximum Acceptable Level

All Other Chlorosilanes

(Monochlorosilane, Silicon

Tetrachloride, Trichlorosilane)

3% (liquid phase) 1% (liquid phase)

Aluminum 1.0 ppbw (vapor phase derived) 1.0 ppbw (vapor phase derived)

Arsenic 0.5 ppbw (vapor phase derived) 0.2 ppbw (vapor phase derived)

Boron 0.3 ppbw (vapor phase derived) 0.1 ppbw (vapor phase derived)

Carbon 10 ppmw (vapor phase derived) 1 ppmw (vapor phase derived)

Iron 50 ppbw (liquid phase) 50 ppbw (liquid phase)

Phosphorus 0.3 ppbw (vapor phase derived) 0.3 ppbw (vapor phase derived)

An analysis of significant figures has not been considered. The number of significant figures will be based on analytical accuracy and the

precision of the provided procedure.

Monochlorosilane not to exceed 0.5%

This specification applies to the appropriate phase of the cylinder as delivered.

The liquid phase purity is to be based on the chlorosilane determination. In addition, argon + helium are to be controlled in the vapor phase to

less than 0.5%. This argon + helium determination will not affect the percent purity determination.

Initial purging of the vapor phase is recommended to reduce inert gas content used in the cylinder fill procedure.

Analytical procedures for the doping elements, metals and selected impurities are to be determined between the user and supplier at the present

time.

7 Electrical Requirements

7.1 Electrical requirements for the various grades of dichlorosilane are given in Table 2

Table 2 Electrical Requirements for Various Grades of Dichlorosilane

Previous SEMI Reference #

C3.18-1102

(Specification)

C3.31-1102

(Specification)

Resistivity

Greater than 50 ohm-cm (n-type)

Greater than 150 ohm-cm (n-type)

The resistivity measurement technique is to be determined between supplier and user.

Monocrystalline silicon formed from this material, not the material itself.

8 Physical Constants

8.1 The physical constants of dichlorosilane are given in Table 3 (for information only).

Table 3 Physical Constants of Dichlorosilane (for information only)

Metric Units US Units

Molecular weight 100.99 100.99

Boiling point at 1 atm 8.2°C 46.8°F

Density of gas at 25°C (77°F) and 1 atm 4.168 kg/m

0.260 lb/ft

Specific gravity of gas at 21.1°C (70°F) and 1 atm

(air = 1)

3.48 3.48

Density of liquid at 25°C (77°F) 122 kg/m

7.62 lb/ft

SEMI C56-0305 © SEMI 2005 3

9 Analytical Procedures for Purity of 97% of Dichlorosilane

NOTE 1: The sample is extremely flammable and corrosive. Test for leaks before sampling. Ensure good electrical grounding.

9.1 Other Chlorosilanes — This procedure is for the determination of other chlorosilanes (monochlorosilane,

trichlorosilane and silicon tetrachloride) in dichlorosilane using a gas chromatograph with a thermal conductivity

detector.

9.1.1 Detection Limit — 10 ppm.

9.1.2 Instrument Parameters

9.1.2.1 Column: 3.05 m (10 ft) by 3.2 mm (1/8 in) stainless steel tubing packed with 20% OV-101 on 80/100

Chromosorb W-HP or equivalent.

9.1.2.2 Carrier Flow: 20 mL/min helium.

9.1.2.3 Sample Volume: 0.5 to 1.0 mL.

9.1.2.4 Temperatures:

Detector 350°C

Column 60°C ramped to 325°C at 10°C/min

Inlet 300°C

9.1.3 Operating Procedure

9.1.3.1 Inject a known sample of monochlorosilane, trichlorosilane and silicon tetrachloride in dichorosilane into

the column using a gas sampling valve. Record the retention times and peak areas. The order of elution is

monochlorosilane, dichlorosilane, trichlorosilane, silicon tetrachloride.

9.1.3.2 Inject the sample to be tested in the same manner as in ¶9.1.3.1. Record the areas of the peaks which have

the same retention times as those in ¶9.1.3.1.

9.1.3.3 Repeat ¶9.1.3.1.

9.1.3.4 Calculate the purity of dichlorosilane in the sample, using the equations stated below. The result may not

exceed the specification in Table 1 of this standard.

9.1.4 Calculations

9.1.4.1 Determine the total area of the chlorosilane peaks (A

) by adding the areas of the four peaks.

9.1.4.2 Divide the area of the dichlorosilane peak by A

. Multiply the result by 100% to obtain the purity of the

dichlorosilane.

10 Analytical Procedures for Purity of 99% of Dichlorosilane (see Note 1 in §9)

10.1.1 Other Chlorosilanes — Follow the procedure in §9 except add the following calculation for

monochlorosilane.

10.1.2 Calculations for monochlorosilane

10.1.2.1 Calculate the percentage the monochlorosilane in the sample using the equation stated below. The result

may not exceed the specification in table 1 of this standard.

10.1.2.2 Divide the area of the monochlorosilane peak by A

. Multiply the result by 100% to obtain the percentage

of monochlorosilane.

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