To manufacture a low-carbon concentration GaAs wafer required for devices such as hall sensors, FETs, HEMTs etc. at a high production yield without deteriorating the semi-insulation characteristics thereof, a method of manufacturing a semi-insulation GaAs monocrystal by controlling carbon concentration during crystal growth by a simple method is disclosed. The method of manufacturing a semi-insulation GaAs monocrystal in accordance with liquid encapsulated Czochralski method, comprises the steps of: preparing a crucible (5) formed with a crucible body (6) and a small chamber (8) communicating with a lower part of the crucible body and a carbon heater (4) processed to reduce surface blow holes thereof; putting a melted GaAs liquid and a sealing compound B.sub.2 O.sub.3 in the crucible housed in an airtight vessel in such a way that the sealing compound B.sub.2 O.sub.3 is on the melted GaAs liquid and further the melted GaAs liquid put in the small chamber contains carbon to be supplied to the melted GaAs liquid in the crucible body; heating the crucible by the heater housed in the airtight vessel; and pulling up the melted GaAs liquid from the crucible body by keeping the airtight vessel at a high pressure.