This standard applies to silicon polycrystalline rods grown by depositing silicon polycrystalline on thin silicon cores by hydrogen reduction of trichlorosilane and silicon tetrachloride. GB/T 4059-1983 Test method for phosphorus in atmosphere zone of silicon polycrystalline GB/T4059-1983 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Polycrystalline silicon--Examination method -Zone-melting on phosphorus under controlled atmosphereUDC 669.782 :548
.2:543.06
GB 4059—83
This standard applies to silicon polycrystalline rods grown by reducing trichlorosilane and silicon tetrachloride with hydrogen to deposit silicon polycrystalline on a thin silicon core. The effective range of the detection impurity concentration is 0.02～20ppba. The N-type resistivity range is 10～2000Q·cm. 1 Principle of the method
1.1 Principle
The difference in the effective segregation coefficient of phosphorus and boron in silicon during silicon zone melting and the difference in the evaporation rate of phosphorus and boron from silicon are used. 1.2 Method
Atmosphere zone melting method.
2 Sample preparationwww.bzxz.net
2.1 Sampling location
Except for the overlap of the silicon core of the bridge-shaped silicon polycrystalline rod or the 10mm-section of the straight silicon polycrystalline rod away from the graphite chuck, the sample can be taken (as shown in Figure 1). 2.2 Sample size
Diameter 10~40mm.
Length 70~200mm.
2.3 Sample treatment
2.3.1 Wash the sample in chemically pure acetone to remove oil. 2.3.2
Wash with chemically pure ethanol for 20~30s and then rinse with deionized water with a resistivity greater than 10M. Etch in a mixed acid solution of super pure HF:HNO:=1 (3~5) volume for 2min. 2.3.32
Etch in the second portion of the mixed acid solution of high-grade pure HF:HNO3=1:(3～5) for 2 minutes, and rinse the sample with deionized water with a resistivity greater than 10MS until it is neutral. 2.3.5
Boil the sample with ultrasonic or deionized water for multiple times, wash, dry, and package for use. Instruments and equipment
Internal heating zone furnace.
4 Seed crystal preparation
4.1 Seed crystal specifications
N-type <111 silicon single crystal with a resistivity greater than 300s2.cm. Cut into 5m×5m×50mm. 4.2 Seed crystal treatment
Same as 2.3 sample treatment.
5 Inspection conditions
Atmosphere requirements
National Bureau of Standards 1983-1220 Issued
1984~12-01 Implementation
5.1.1 Atmosphere type
Hydrogen, argon or hydrogen-fluorine mixed gas.
5.1.2 Atmosphere specifications
GB 405983
Dew point is lower than -45℃. Oxygen content is less than 5ppm5.2 Zone melting times
1~2 times to form a single crystal.
5.3 Zone melting speed
Purification speed 6~8mm/min.
Crystallization speed 3~5mm/min.
5.4 Melting zone height
Equal to the diameter of the test rod.
5.5 Melting zone travel
More than 10 melting zones.
5.6 Test result size
Diameter 12±2mm.
Length greater than 10 melting zones.
Test method
6.1 Test of conductive type
Thin silicon core
No sampling allowed
GB4059—83
Tested by GB1550-—79 "Determination of conductivity type of silicon single crystal". 6.2 Test of longitudinal resistivity
Tested by GB1551—79 "DC two-probe measurement method for resistivity of silicon single crystal". Value of phosphorus detection resistivity
All silicon polycrystalline samples are required to be N-type single crystals after zone melting test. The distribution of longitudinal resistivity curve of test results is close to the theoretical curve (as shown in Figure 2). The resistivity value from the first melting zone to 80% of the length of the test rod is taken as the phosphorus detection resistivity value without deducting the base boron compensation. h(s2.cm)
8 Re-inspection
If the test result of the bar material is P type, mixed type, the resistivity distribution is very abnormal, or there are sparks and sparks during the zone melting test process1, a re-inspection should be carried out.
GB4059-83
Appendix A
(Supplement)
A.1Since the silicon polycrystalline product standard has life parameter requirements for silicon polycrystalline in atmosphere zone melting test, this standard adopts GB1553-79 "Measurement Method for DC Photoconductivity Decay of Silicon Single Crystal Life" test. Additional Notes:
This standard was proposed by the Ministry of Metallurgical Industry of the People's Republic of China. This standard was drafted by Emei Semiconductor Materials Factory. The main drafter of this standard was Zhao Zupei.
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