Abstract: A clean and high-purity polycrystalline silicon mass having a small content of chromium, iron, nickel, copper, and cobalt in total, which are heavy metal impurities that reduce the quality of single-crystal silicon, can be obtained from a silicon rod by before crushing a polycrystalline silicon rod, removing at least 70 mm of a polycrystalline silicon portion from the electrode side end of the polycrystalline silicon rod extracted to the outside of a reactor is provided. Thereby, the polycrystalline silicon portion in which the total of the chromium, iron, nickel, copper, and cobalt concentrations in a bulk is not less than 150 ppta can be removed.

Abstract: To provide polycrystalline silicon suitable as a raw material for production of single-crystalline silicon. A D/L value is set within the range of less than 0.40 when multiple pairs of silicon cores are placed in a reaction furnace in production of a polycrystalline silicon rod having a diameter of 150 mm or more by deposition according to a chemical vapor deposition process and it is assumed that the average value of the final diameter of the polycrystalline silicon rod is defined as D (mm) and the mutual interval between the multiple pairs of silicon cores is defined as L (mm).

Abstract: Provided is a polycrystalline silicon rod suitable as a raw material for production of single-crystalline silicon. A crystal piece (evaluation sample) is collected from a polycrystalline silicon rod grown by a Siemens method, and a polycrystalline silicon rod in which an area ratio of a crystal grain having a particle size of 100 nm or less is 3% or more is sorted out as the raw material for production of single-crystalline silicon. When single-crystalline silicon is grown by an FZ method using the polycrystalline silicon rod as a raw material, the occurrence of dislocation is remarkably suppressed.

Abstract: According to the present invention, a resin material that has the following surface concentration of impurities is consistently used in production of polycrystalline silicon. Values obtained from quantitative analysis by ICP-mass spectrometry using a 1 wt % nitric acid aqueous solution as an extraction liquid are: a phosphorous (P) concentration of 50 pptw or less; an arsenic (As) concentration of 2 pptw or less; a boron (B) concentration of 20 pptw or less; an aluminum (Al) concentration of 10 pptw or less; a total concentration of 6 elements of iron (Fe), chromium (Cr), nickel (Ni), copper (Cu), sodium (Na), and zinc (Zn) of 80 pptw or less; a total concentration of 10 elements of lithium (Li), potassium (K), calcium (Ca), titanium (Ti), manganese (Mn), cobalt (Co), molybdenum (Mo), tin (Sn), tungsten (W), and lead (Pb) of 100 pptw or less.

Abstract: For evaluating a polycrystalline silicon rod to be used as a raw material for production of FZ Si single crystals, novel evaluation values (values of characteristics×amount of crystals) including the amount of crystals grown in the growth direction (radial direction) are defined and the homogeneity in crystal characteristics in the growth direction (radial direction) is evaluated. Specifically, the homogeneity of the polycrystalline rod is evaluated by sampling a plurality of specimen plates each having, as a principal plane thereof, a cross-section perpendicular to a radial direction of the polycrystalline rod grown by a Siemens method at equal intervals in the radial direction, determining values of characteristics of the crystals of the specimen plates by measurements, and by using evaluation values obtained by multiplying amounts of the crystals (relative amounts of the crystals) at sites where the specimen plates have been sampled by the values of the crystal characteristics.

Abstract: The present invention provides polycrystalline silicon suitably used as a raw material for producing single crystal silicon. The polycrystalline silicon rod of the present invention is a polycrystalline silicon rod grown by chemical vapor deposition performed under a pressure of 0.3 MPaG or more, wherein when a plate-shaped sample piece collected from an arbitrary portion of the polycrystalline silicon rod is observed with a microscope with a temperature increased from a temperature lower than a melting point of silicon up to a temperature exceeding the melting point of silicon, a heterogeneous crystal region, which is a crystal region including a plurality of crystal grains heterogeneously assembled and including no needle-like crystal, having a diameter exceeding 10 ?m is not observed.

Abstract: For evaluating a polycrystalline silicon rod to be used as a raw material for production of FZ Si single crystals, novel evaluation values (values of characteristics×amount of crystals) including the amount of crystals grown in the growth direction (radial direction) are defined and the homogeneity in crystal characteristics in the growth direction (radial direction) is evaluated. Specifically, the homogeneity of the polycrystalline rod is evaluated by sampling a plurality of specimen plates each having, as a principal plane thereof, a cross-section perpendicular to a radial direction of the polycrystalline rod grown by a Siemens method at equal intervals in the radial direction, determining values of characteristics of the crystals of the specimen plates by measurements, and by using evaluation values obtained by multiplying amounts of the crystals (relative amounts of the crystals) at sites where the specimen plates have been sampled by the values of the crystal characteristics.

Abstract: A reaction furnace for producing a polycrystalline silicon according to the present invention is designed so as to have an in-furnace reaction space in which a reaction space cross-sectional area ratio (S=[S0?SR]/SR) satisfies 2.5 or more, which is defined by an inner cross-sectional area (So) of a reaction furnace, which is perpendicular to a straight body portion of the reaction furnace, and a total sum (SR) of cross-sectional areas of polycrystalline silicon rods that are grown by precipitation of polycrystalline silicon, in a case where a diameter of the polycrystalline silicon rod is 140 mm or more. Such a reaction furnace has a sufficient in-furnace reaction space even when the diameter of the polycrystalline silicon rod has been expanded, and accordingly an appropriate circulation of a gas in the reaction furnace is kept.

Abstract: In the present invention, once a polycrystalline silicon rod is grown by the Siemens process, the polycrystalline silicon rod is heat-treated within a temperature range from 750° C. to 900° C. to relieve residual stress in the crystal. According to the experiment of the present inventors, residual stress can be relieved satisfactorily by heat treatment at the above-described low temperature, and in addition, metal contamination cannot be induced and the physical properties of the polycrystalline silicon rod cannot be changed. The above heat treatment can be conducted inside a furnace used to grow the polycrystalline silicon rod, and can also be conducted outside a furnace used to grow the polycrystalline silicon rod. According to the present invention, a polycrystalline silicon rod with residual stress (?) of not more than +20 MPa evaluated by a 2?-sin2? diagram can be obtained.

Abstract: A reactor 200 according to the present invention includes a heater storage section serving as a space section capable of accommodating a carbon heater to initial heating of silicon core wires. A carbon heater 13 is loaded in a deposition reaction space 20 in the reactor 200 only when necessary for initial heating of silicon core wires 12. After initial heating of the silicon core wires 12 is finished, the carbon heater 13 is unloaded from the deposition reaction space to the heater storage section 30. As a result, the carbon heater 13 is not unduly damaged in the reactor any longer and its deterioration is reduced. In addition, because of reduction in reaction with hydrogen gas in the reactor, the generation of methane is reduced, and thus carbon contamination of polycrystalline silicon is reduced.

Abstract: A reaction furnace for producing a polycrystalline silicon according to the present invention is designed so as to have an in-furnace reaction space in which a reaction space cross-sectional area ratio (S=[S0?SR]/SR) satisfies 2.5 or more, which is defined by an inner cross-sectional area (So) of a reaction furnace, which is perpendicular to a straight body portion of the reaction furnace, and a total sum (SR) of cross-sectional areas of polycrystalline silicon rods that are grown by precipitation of polycrystalline silicon, in a case where a diameter of the polycrystalline silicon rod is 140 mm or more. Such a reaction furnace has a sufficient in-furnace reaction space even when the diameter of the polycrystalline silicon rod has been expanded, and accordingly an appropriate circulation of a gas in the reaction furnace is kept.

Abstract: For evaluating a polycrystalline silicon rod to be used as a raw material for production of FZ Si single crystals, novel evaluation values (values of characteristics×amount of crystals) including the amount of crystals grown in the growth direction (radial direction) are defined and the homogeneity in crystal characteristics in the growth direction (radial direction) is evaluated. Specifically, the homogeneity of the polycrystalline rod is evaluated by sampling a plurality of specimen plates each having, as a principal plane thereof, a cross-section perpendicular to a radial direction of the polycrystalline rod grown by a Siemens method at equal intervals in the radial direction, determining values of characteristics of the crystals of the specimen plates by measurements, and by using evaluation values obtained by multiplying amounts of the crystals (relative amounts of the crystals) at sites where the specimen plates have been sampled by the values of the crystal characteristics.

Abstract: A polycrystalline silicon ingot having a value of Te?Ts, ?T, of 50° C. or less, wherein Ts and Te are the onset temperature and the completion temperature of melting, respectively, when the temperature is increased at a rate of 60° C./minute or less in the temperature range of 1400° C. or more is used as the production raw material for single crystal silicon. The present invention provides a polycrystalline silicon ingot or polycrystalline silicon rod suitable for stably producing single crystal silicon.

Abstract: A reactor 200 according to the present invention includes a heater storage section serving as a space section capable of accommodating a carbon heater for initial heating of silicon core wires. A carbon heater 13 is loaded in a deposition reaction space 20 in the reactor 200 only when necessary for initial heating of silicon core wires 12. After initial heating of the silicon core wires 12 is finished, the carbon heater 13 is unloaded from the deposition reaction space to the heater storage section 30. As a result, the carbon heater 13 is not unduly damaged in the reactor any longer and its deterioration is reduced. In addition, because of reduction in reaction with hydrogen gas in the reactor, the generation of methane is reduced, and thus carbon contamination of polycrystalline silicon is reduced.

Abstract: A reaction furnace for producing a polycrystalline silicon according to the present invention is designed so as to have an in-furnace reaction space in which a reaction space cross-sectional area ratio (S=[SO?SR]/SR) satisfies 2.5 or more, which is defined by an inner cross-sectional area (So) of a reaction furnace, which is perpendicular to a straight body portion of the reaction furnace, and a total sum (SR) of cross-sectional areas of polycrystalline silicon rods that are grown by precipitation of polycrystalline silicon, in a case where a diameter of the polycrystalline silicon rod is 140 mm or more. Such a reaction furnace has a sufficient in-furnace reaction space even when the diameter of the polycrystalline silicon rod has been expanded, and accordingly an appropriate circulation of a gas in the reaction furnace is kept.

Abstract: A hydrogen gas recovery system according to the present ingestion is configured by a condensation and separation apparatus (A) that condenses and separates chlorosilanes from a hydrogen-containing reaction exhaust gas exhausted from a polycrystalline silicon production step, a compression apparatus (B) that compresses the hydrogen-containing reaction exhaust gas, an absorption apparatus (C) that absorbs and separates hydrogen chloride by contacting the hydrogen-containing reaction exhaust gas with an absorption liquid, a first adsorption apparatus (D) comprising an adsorption column filled with activated carbon for adsorbing and removing methane, hydrogen chloride, and part of the chlorosilanes each contained in the hydrogen-containing reaction exhaust gas, a second adsorption apparatus (E) comprising an adsorption column filled with synthetic zeolite that adsorbs and removes methane contained in the hydrogen-containing reaction exhaust gas, and a gas line (F) that recovers a purified hydrogen gas having a re

Abstract: A system for purifying trichlorosilane that can prevent re-contamination by the dissociation of an adduct occurring in association with the conversion of high boiling point compounds or the remaining of impurities due to an equilibrium constraint is provided. Trichlorosilane containing impurities serving as a donor or an acceptor in silicon crystals is supplied to a multistage impurity conversion step. These impurities in the trichlorosilane are converted into high boiling point compounds in the presence of a distillation aid. A plurality of impurity conversion step sections (101 to 10n) are connected in series, and any of the impurity conversion step sections comprises a reception section a for the trichlorosilane from the preceding stage section, an introduction section b for the distillation aid, a transmission section c for the trichlorosilane to the subsequent stage section, and a drain section d that discharges a remainder out of the impurity conversion step section.

Abstract: Provided is a polycrystalline silicon rod suitable as a raw material for production of single-crystalline silicon. A crystal piece (evaluation sample) is collected from a polycrystalline silicon rod grown by a Siemens method, and a polycrystalline silicon rod in which an area ratio of a crystal grain having a particle size of 100 nm or less is 3% or more is sorted out as the raw material for production of single-crystalline silicon. When single-crystalline silicon is grown by an FZ method using the polycrystalline silicon rod as a raw material, the occurrence of dislocation is remarkably suppressed.

Abstract: A polycrystalline silicon rod is synthesized by the Siemens method (S101). After the polycrystalline silicon rod is covered from above with a plastic bag whose inner surface has been washed, and housed in the plastic bag in a reactor (S103), the polycrystalline silicon rod is removed out of the reactor (S104), and heat-sealed and stored in an enclosed state (S105). According to the present invention, steps conventionally considered as essential, such as washing, etching, and water washing, are not always necessary, and therefore the concentrations of fluorine ions, nitrate ions, and nitrogen dioxide ions remaining on the surface can each be less than 0.2 ppbw. In addition, by covering with the plastic bag, the metal contamination levels decrease significantly. Moreover, when the handling according to the present invention is performed, surface contamination hardly proceeds even if the polycrystalline silicon rod is stored for a long period.

Abstract: The present invention provides a technique by which heat can be efficiently recovered from a coolant used to cool a reactor, and contamination with dopant impurities from an inner wall of a reactor when polycrystalline silicon is deposited within the reactor can be reduced to produce high-purity polycrystalline silicon. With the use of hot water 15 having a temperature higher than a standard boiling point as a coolant fed to the reactor 10, the temperature of the reactor inner wall is kept at a temperature of not more than 370° C. Additionally, the pressure of the hot water 15 to be recovered is reduced by a pressure control section provided in a coolant tank 20 to generate steam. Thereby, a part of the hot water is taken out as steam to the outside, and reused as a heating source for another application.