WO2013171955A1 - 単結晶シリコン引き上げ用シリカ容器及びその製造方法 - Google Patents
単結晶シリコン引き上げ用シリカ容器及びその製造方法 Download PDFInfo
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- WO2013171955A1 WO2013171955A1 PCT/JP2013/001839 JP2013001839W WO2013171955A1 WO 2013171955 A1 WO2013171955 A1 WO 2013171955A1 JP 2013001839 W JP2013001839 W JP 2013001839W WO 2013171955 A1 WO2013171955 A1 WO 2013171955A1
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- silica
- silica container
- concentration
- container
- single crystal
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
- C03B11/02—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing in machines with rotary tables
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
- C03B11/06—Construction of plunger or mould
- C03B11/10—Construction of plunger or mould for making hollow or semi-hollow articles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
- C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
Definitions
- the present invention relates to a silica container for pulling up single crystal silicon and a method for manufacturing the same.
- Silica glass is a lens, prism, photomask, TFT substrate for display, UV lamp tube, window material, reflector, and semiconductor industry cleaning container for projection exposure equipment (lithography equipment) for large-scale integrated circuit (LSI) manufacturing. It is used as a silicon melting container.
- these raw materials for silica glass must use expensive compounds such as silicon tetrachloride, and the melting temperature and processing temperature of silica glass are as high as about 2000 ° C., resulting in high energy consumption and high cost. It was a thing. Therefore, conventionally, a method for producing silica glass using a relatively inexpensive natural powder raw material has been considered.
- Patent Document 3 A method for improving the silicon melt etching resistance of a silica crucible for pulling single crystal silicon is disclosed in Patent Document 3, in which an effect of applying or solid-dissolving a crystallization accelerator on the inner surface of a silica glass crucible is disclosed. It is shown.
- the crystallization accelerator the alkaline earth metal element Mg, Sr, Ca, Ba, or Al of the 3b group element which is the group 2a element is shown.
- the silica glass crucible shown here the inner surface of the crucible is not recrystallized uniformly during pulling of the single crystal silicon, so the etching of the inner wall of the crucible by the silicon melt is not sufficiently reduced, and the durability of the silica crucible is Sex was not improved.
- Patent Document 4 discloses a technique for reducing the release of crystalline silica particles into the silicon melt from the inner surface of the silica crucible and a technique for strengthening the silica crucible from the outer surface of the silica crucible.
- a devitrification accelerator is present on the surface of the crucible, specifically, an alkaline earth metal selected from the group of Ba, Mg, Sr and Be is included.
- an alkaline earth metal selected from the group of Ba, Mg, Sr and Be is included.
- the surface of the crucible is not recrystallized promptly at the start of pulling of the single crystal silicon, or the entire surface is not recrystallized uniformly. It was not reduced and the durability of the silica crucible was not improved.
- Patent Document 5 as another method for recrystallizing the inner surface of the silica crucible, the OH group concentration near the surface is set to 115 ppm or more while giving a gradient to the OH group concentration at a surface depth of 0.3 to 3 mm. This indicates that the surface portion can be easily recrystallized without using a crystallization accelerator.
- the etching amount of the silicon melt on the surface portion becomes extremely large, so that the surface layer is dissolved when the polysilicon raw material lump is melted in the silica crucible, and at the time of subsequent single crystal silicon pulling There was a problem that the inner surface of the silica crucible was not recrystallized uniformly.
- Patent Document 6 discloses a low-cost silica container by a sol-gel method and a manufacturing method thereof. While the outer layer of the silica container is a white opaque layer, the inner layer is a transparent silica glass layer containing carbon. In the examples, a transparent silica glass layer having a thickness of 3 mm containing Ba and OH groups is shown. In these silica glass containers, a certain degree of recrystallization promotion effect is recognized when the container is used, but uniform recrystallization over the entire inner surface of the container at the start of use of the container has been further demanded.
- Patent Document 7 discloses a silica container that is prepared by preparing silica raw material powder doped with crystallization accelerators Ca, Sr, Ba and hydrogen gas in advance, and discharging and melting the raw material powder.
- crystallization accelerators Ca, Sr, Ba and hydrogen gas in advance, and discharging and melting the raw material powder.
- a certain degree of recrystallization promoting effect inside the container was observed when single crystal silicon was pulled up, but it was insufficient to uniformly recrystallize the entire inner surface of the container at an early point.
- Patent Document 9 and Patent Document 10 show that the thickness dimension is increased by devising the shape of the outer wall of the silica crucible as a countermeasure against the erosion (etching) of the silica crucible by the silicon melt.
- this method does not fundamentally reduce the erosion (etching) of the silica crucible body by the silicon melt, it causes a significant increase in the oxygen concentration of the silicon melt due to the melting of the silica glass, or the impurity metal contained in the silica crucible. The quality of single crystal silicon that caused element contamination or was pulled up was low.
- Japanese Patent Publication No.4-222861 Japanese Patent Publication No. 7-29871 Japanese Patent No. 3100836 Japanese Patent No. 3046545 International Publication No. WO2009 / 113525 Pamphlet JP 2010-189205 A JP 2011-84428 A JP 2011-121811 A JP 2011-121842 A JP 2011-121843 A
- the present invention has been made in view of the above-described problems, and when a silica container is used for pulling single crystal silicon, the inner surface of the container made of transparent silica glass within a short time after the start of use of the container. Providing a silica container that significantly improves the etching resistance (erosion resistance) against the silicon melt on the inner surface of the container by finely crystallizing the entire surface (glass ceramics); and An object of the present invention is to provide a method for producing a simple silica container.
- the present invention has been made to solve the above problems, and has a transparent layer made of transparent silica glass on the inside, and a silica for pulling single crystal silicon having an opaque layer made of opaque silica glass containing bubbles on the outside.
- a silica container for pulling single crystal silicon characterized in that it comprises a base layer, and Ba is applied to the inner surface of the high OH base layer at a concentration of 25 to 1000 ⁇ g / cm 2 .
- Such a silica container having a layer containing a high concentration of OH groups (high OH base layer) on the inner surface side of the transparent layer, and having Ba coated on the inner surface of the high OH base layer at a high concentration.
- high OH base layer a layer containing a high concentration of OH groups
- Ba coated on the inner surface of the high OH base layer at a high concentration when used for pulling single crystal silicon, the entire inner surface of the high OH base layer can be finely crystallized (glass ceramics) within a short time after the start of container use. Therefore, the etching resistance (erosion resistance) against the silicon melt on the inner surface of the silica container can be greatly improved.
- the thickness of the high OH base layer is preferably 0.5 mm or more and 3 mm or less.
- the etching resistance of the transparent layer can be sufficiently obtained. At the same time, deformation of the container at a high temperature when using the silica container can be prevented.
- the concentration of the OH group contained in the high OH base layer is preferably 300 to 1500 mass ppm, and the concentration of Ba applied to the inner surface of the high OH base layer is preferably 60 to 500 ⁇ g / cm 2 .
- the etching resistance when using the silica container can be more effectively imparted.
- the present invention also relates to a method for producing a silica container for pulling up single crystal silicon, the step of producing silica powder having a particle size of 10 to 1000 ⁇ m as raw material powder, the raw material powder is put into a mold, A step of forming a temporary molded body by temporarily forming the preform into a predetermined shape according to the inner wall of the mold while rotating the mold; and rotating the temporary molded body in the mold and removing the temporary molded body from the outside While degassing the gas component contained in the temporary molded body, the temporary molded body is heated and melted by a discharge heating melting method to form a transparent layer made of transparent silica glass on the inside and contain bubbles on the outside.
- a method for producing a silica container for pulling a single crystal silicon characterized in that an OH group concentration is 200 to 2000 mass ppm in a region on the surface side.
- a silica container having a layer containing a high concentration of OH groups on the inner surface side of the transparent layer and having Ba coated on the inner surface at a high concentration can be produced at low cost. If such a silica container, as described above, when used for pulling single crystal silicon, the entire surface on the inner surface side of the transparent layer can be finely crystallized within a short time after the start of container use, The etching resistance to the silicon melt can be greatly improved.
- the inside of the silica container has a water vapor-containing gas atmosphere until the temperature falls to at least 200 ° C. or less.
- the silica container for pulling up single crystal silicon according to the present invention when used for pulling up single crystal silicon, can finely crystallize the entire surface of the high OH base layer within a short time after the start of use of the container.
- the etching resistance to the silicon melt on the surface can be greatly improved.
- the manufacturing method of the silica container for single crystal silicon pulling which concerns on this invention can manufacture such a silica container at low cost.
- the problem to be solved by the present invention is that when using a silica container for pulling up single crystal silicon, the use of the inner surface of the colorless transparent silica glass of the container within a short time after the start of use of the silica container.
- the entire surface is finely crystallized with a crystal such as cristobalite (glass ceramics) to greatly improve the etching resistance (erosion resistance) against the silicon melt on the inner surface of the silica container.
- etching resistance on the inner surface of the silica container for pulling single crystal silicon brings a plurality of good results.
- microcavity defects sometimes called voids or pinholes are sometimes generated in the produced single crystal silicon.
- One of the causes is silicon monoxide that is generated by the reaction of the silica container surface by etching with silicon melt. It is presumed to be (SiO) gas, and these cavity defects can be reduced by improving the etching resistance.
- the cause of dislocation by inhibiting the growth of single crystal silicon may be due to the occurrence of foreign matter defects consisting of silica fine particles, and one of the causes is the surface roughened by etching with silicon melt on the surface of the silica container.
- the silica SiO 2 particles are detached. Further, an increase in the etching amount on the inner surface of the silica container causes an increase in the oxygen concentration in the silicon melt. Therefore, the improvement of etching resistance contributes to the improvement of the quality of single crystal silicon.
- impurities contained in the silica container such as alkali metal elements Li, Na, K, transition metal elements Ti, Cr, Mn, Fe, Ni, Cu, Zn, Zr, Mo , W and the like diffuse and elute into the silicon melt.
- the recrystallized silica container surface also has a shielding effect that reduces the diffusion of these impurity elements into the silicon melt.
- a single silica container has been used to pull up a single crystal silicon.
- it has been required to pull up a plurality of single crystal silicons with a single container (multiple pulling). Yes.
- the etching resistance of the silica container it is possible to reduce defects such as voids, pinholes, and foreign matters, suppress an increase in oxygen concentration, and prevent impurity contamination. Multiple pulling of high quality single crystal silicon is possible.
- a silica container for pulling up single crystal silicon according to the present invention will be described with reference to FIGS.
- a single crystal silicon pulling silica container 72 has a transparent layer 52 made of transparent silica glass on the inner side and an opaque layer 51 made of opaque silica glass containing bubbles on the outer side.
- the transparent layer 52 does not substantially contain bubbles.
- the opaque layer 51 is usually white and opaque, and the transparent layer 52 is usually colorless and transparent.
- the transparent layer 52 further includes a low OH base layer 52a positioned on the opaque layer 51 side of the silica container 72 (that is, the outer surface 76 side of the silica container) and the inner surface 75 side of the silica container 72. And a high OH base layer 52b.
- the high OH base layer 52b contains OH groups at a concentration of 200 to 2000 mass ppm.
- the low OH base layer 52a has a lower OH group concentration than the high OH base layer 52b. Specifically, it is 60 massppm or less, preferably 30 massppm or less.
- the high OH base layer 52b has an OH group concentration that satisfies the above numerical range over the entire thickness range.
- Ba is further applied to the inner surface of the high OH base layer 52b (that is, the inner surface of the silica container 72) at a concentration of 25 to 1000 ⁇ g / cm 2 .
- FIG. 2 is a schematic cross-sectional view showing an enlarged cross section of the side wall of the silica container 72 according to the present invention.
- TO indicates the thickness of the opaque layer 51
- TI indicates the thickness of the transparent layer 52
- TI1 indicates the thickness of the low OH base layer 52a
- the OH group has an effect of enhancing the crystallization promoting effect of Ba.
- the OH group has a function of reducing the viscosity of silica glass at a high temperature and deteriorating the etching resistance to silicon melt, and therefore has a preferable concentration range.
- the inner layer in the transparent layer 52 made of transparent silica glass, the inner layer (high OH base layer 52b) has an OH group concentration of 200 to 2000 mass ppm, and the inner surface of the high OH base layer 52b (that is, the inside of the silica container 72).
- the entire surface can be formed into a uniform and dense white opaque recrystallized layer in a short time.
- the low OH base layer 52 a exists in the transparent layer 52 in order not to lower the viscosity and etching resistance of the transparent layer 52. That is, in the silica container 72 of the present invention, the range containing the OH group in the above range is limited to the region near the inner surface of the transparent layer 52.
- the concentration of the OH group contained in the high OH base layer 52b is preferably 300 to 1500 mass ppm.
- the concentration of Ba applied to the inner surface of the high OH base layer 52b is preferably 60 to 500 ⁇ g / cm 2 .
- the thickness TI2 of the high OH base layer 52b shown in FIG. 2 is preferably 0.5 mm or more and 3 mm or less.
- the etching resistance on the surface of the transparent layer 52 can be sufficiently obtained. If the high OH base layer 52b has a thickness of 3 mm or less, the viscosity and etching resistance can be sufficiently maintained.
- the thickness of the high OH base layer 52b is more preferably 1 mm or less.
- silica powder having a particle size of 10 to 1000 ⁇ m is prepared as the raw material powder 11.
- the raw material powder 11 can be produced, for example, by crushing and sizing a silica stone lump as follows, but is not limited thereto.
- a natural quartzite block (naturally produced crystal, quartz, quartzite, siliceous rock, opal stone, etc.) with a diameter of about 5 to 50 mm is heated in a temperature range of 600 to 1000 ° C. for about 1 to 10 hours in an air atmosphere. To do.
- the natural silica mass is then poured into water, taken out after rapid cooling and dried. This process facilitates the subsequent crushing and sizing process using a crusher or the like, but the process may proceed to the crushing process without performing the heating and quenching process.
- the natural silica mass is pulverized and sized by a crusher or the like, and the particle size is adjusted to 10 to 1000 ⁇ m, preferably 50 to 500 ⁇ m, to obtain natural silica powder.
- this natural silica powder is put into a rotary kiln composed of a silica glass tube having an inclination angle, and the inside of the kiln is made into an atmosphere containing hydrogen chloride (HCl) or chlorine (Cl 2 ) gas at 800 to 1100 ° C.
- High purity treatment is performed by heating for about 1 to 10 hours.
- the process may proceed to the next process without performing the purification process.
- the raw material powder 11 obtained after the above steps is crystalline silica
- amorphous silica glass powder can be used alone or in combination as the raw material powder 11 depending on the purpose of use of the silica container. .
- the particle diameter of the raw material powder 11 is 10 to 1000 ⁇ m, and preferably 50 to 500 ⁇ m.
- the silica purity (SiO 2 ) of the raw material powder 11 is 99.99 wt. % Or more, preferably 99.999 wt. % Or more is more preferable.
- the purity of the raw material powder 11 is 99.999 wt. % Or more is preferable.
- Al and OH groups are added to the raw material powder 11 in order to prevent the migration and diffusion of impurity metal elements from the manufactured silica container to the inner surface and further into the silicon contained. It is preferable to include a predetermined amount.
- Al can be contained by, for example, adding nitrate, acetate, carbonate, chloride or the like as a water or alcohol solution, putting silica powder into these solutions, immersing them, and then drying them.
- the OH group can be adjusted depending on the gas atmosphere, treatment temperature, and time in the subsequent drying step, which is included in the natural silica from the beginning, or moisture mixed in the intermediate step.
- the raw material powder 11 is put into a mold having rotational symmetry, and according to the inner wall of the mold while rotating the form Temporarily molding into a predetermined shape is performed to produce a temporary molded body 41.
- FIG. 4 sectional drawing showing the outline of the mold which temporarily molds the raw material powder 11 was shown.
- the mold 101 used in the present invention is made of, for example, a heat-resistant ceramic member such as graphite, alumina, silicon carbide, or silicon nitride, has rotational symmetry, and is rotated by a mold rotation motor (not shown). Can be made.
- decompression holes 103 are distributed and formed in the inner wall 102 of the mold 101.
- the decompression hole 103 is continuous with the decompression passage 104.
- a pressure reducing passage 105 is also passed through a rotating shaft 106 for rotating the mold 101, and vacuuming can be performed from here.
- the raw material powder 11 is introduced into the inner wall 102 of the mold 101 shown in FIG. 4, and the raw material powder 11 is temporarily formed into a predetermined shape corresponding to the inner wall 102 of the mold 101.
- the raw material powder 11 is formed into a temporary molded body 41 (see FIG. 5). Specifically, while rotating the mold 101, the raw material powder 11 is gradually put into the inner wall 102 of the mold 101, and is formed into a container shape using centrifugal force. Alternatively, the thickness of the temporary molded body 41 may be adjusted to a predetermined amount by bringing a plate-shaped inner mold (not shown) from the inside into contact with the rotating powder.
- the supply method of this raw material powder 11 to the mold 101 is not particularly limited.
- a hopper provided with a stirring screw and a measuring feeder can be used. In this case, the raw material powder 11 filled in the hopper is stirred with a stirring screw and supplied while adjusting the supply amount with a measuring feeder.
- a silica container 71 is produced in which the inner side is a transparent layer made of transparent silica glass and the outer side is an opaque layer made of opaque silica glass containing bubbles.
- the apparatus for producing the silica container 71 includes a vacuum pump for degassing, a rotary motor (not shown) for rotating the mold 101, and discharge heating and melting. It consists of a carbon electrode (carbon electrode) 212, an electric wire 212a, a high-voltage power supply unit 211, a lid 213, and the like that are heat sources for arc melting and arc discharge melting. Note that the number of carbon electrodes 212 can be two or three, and either a DC voltage or an AC voltage can be used.
- the voltage can be adjusted in the range of 100 to 1000 V, and the electric energy can be adjusted in the range of 1000 to 3000 kWh.
- the apparatus further includes components for adjusting the atmospheric gas supplied from the inside of the temporary molded body 41, such as a hydrogen gas supply cylinder 411, an inert gas supply cylinder 412, a gas supply pipe 420, and the like. May be.
- a hydrogen-containing gas As a procedure for melting and sintering the temporary molded body 41, it is preferable to start supplying a hydrogen-containing gas from the inside of the temporary molded body 41 before starting the charging between the carbon electrodes 212.
- hydrogen gas is supplied from the hydrogen gas supply cylinder 411, and inert gas (for example, nitrogen (N 2 ), argon (Ar), helium is supplied from the inert gas supply cylinder 412. (He)) is supplied and mixed, and supplied from the inside of the temporary molded body 41 through the gas supply pipe 420.
- symbol 430 shows the flow of gas. However, such atmospheric gas adjustment may not be performed.
- the degree of vacuum reduction by the vacuum pump for degassing increases (the pressure suddenly decreases), and the raw material constituting the temporary molded body 41
- the molten silica glass layer proceeds from the inside to the outside while degassing the dissolved gas such as water, oxygen, and nitrogen contained in the powder 11.
- the timing of adjusting the strength of vacuuming is important, and it is not preferable to perform strong vacuuming before the inner surface layer of the temporary molded body 41 is vitrified. This is because if fine evacuation is performed from the beginning, impurity fine particles contained in the atmospheric gas adhere to and concentrate on the inner surface portion of the temporary molded body 41 due to the filter effect. Therefore, it is preferable that the initial degree of decompression is not so high, and the vacuuming is gradually strengthened as the inner surface of the temporary molded body 41 is melted into glass.
- the atmosphere gas in the temporary molded body 41 at the time of the electric discharge heating and melting step may be air or an inert gas depending on the use of the silica container to be produced.
- the OH group concentration of 51 can be adjusted. It is preferable to keep the water vapor content of the feed gas in this step at a low value. A value in the range of 15 ° C. to ⁇ 15 ° C. as the dew point temperature of the supplied gas for the purpose of adjusting the OH group content and moisture (H 2 O) content of the opaque layer 51 in the fused and sintered silica container. May be controlled within ⁇ 2 ° C of the set value.
- gas may be supplied after passing through an appropriate dehumidifier.
- the concentration of OH groups in the transparent layer 52 is controlled in the following steps.
- the transparent layer 52 is introduced by introducing a water vapor-containing gas into the produced silica container 71 and continuing heating in the water vapor-containing gas atmosphere. Among them, the OH group concentration on the inner surface side is increased. Thereby, the high OH base layer 52 b and the low OH base layer 52 a are formed in the transparent layer 52.
- the process of continuing heating in this steam-containing gas atmosphere is performed continuously with the previous process ((3) in FIG. 3), and the same apparatus is used.
- water vapor is further supplied to the molten atmosphere by the water vapor supply device 511 and the water vapor supply pipe 520 shown in FIG.
- a hydrogen gas supply cylinder 411, an inert gas supply cylinder 412, a gas supply pipe 420, and the like may be further provided as in the previous step.
- the inside of the silica container 71 may be a water vapor-containing gas atmosphere, and the water vapor supply system may exist alone as shown in FIG. It may be connected to the tube 420.
- the arrow 530 in FIG. 8 indicates the flow of water vapor.
- air can be used, or an inert gas such as nitrogen gas, argon gas, helium gas or the like can be used.
- the water vapor concentration can be controlled, for example, by introducing a saturated water vapor amount at a temperature of 80 ° C. to 120 ° C.
- the silica container 71 heated in the steam-containing gas atmosphere is cooled to room temperature.
- This cooling step may be performed in an air atmosphere, but it is preferable that the inside of the silica container 71 be a water vapor-containing gas atmosphere until the temperature is lowered to at least 200 ° C. or less.
- the adjustment of the water vapor amount can be performed by the water vapor supply device 511, the water vapor supply pipe 520, etc. shown in FIG.
- the OH group concentration is set to 200 to 2000 mass ppm by heating (FIG. 3 (4)) and cooling (FIG. 3 (5)) in the steam-containing gas atmosphere.
- a Ba compound is applied to the inner surface of the transparent layer 52 of the cooled silica container 71 and dried, so that 25 to 25% of Ba is applied to the inner surface of the transparent layer 52. Apply at a concentration of 1000 ⁇ g / cm 2 .
- this step can be performed as follows.
- the Ba compound include chlorides, acetates, nitrates, carbonates and the like.
- This Ba compound is used as an aqueous solution or alcohol solution having a predetermined concentration.
- this Ba solution is applied (coated) onto the inner surface of the silica container.
- a coating method a general method such as brush coating or spray coating can be used. After applying the Ba solution, it is dried for several hours at about 25 ° C. to 200 ° C. in a clean air atmosphere.
- group 2 calcium (Ca) and strontium (Sr) are also effective for recrystallization of silica glass, but the segregation coefficient between single crystal silicon and silicon melt (Ba is silicon melt) In the present invention, Ba that is preferable in terms of the tendency to remain inside is used in the present invention.
- the silica container 72 shown in FIG. 1 can be manufactured at low cost.
- Synthetic silica glasses containing OH groups of 0, 60, 100, 300, 1000, 1500 massppm were prepared by oxyhydrogen flame hydrolysis using silicon tetrachloride (SiCl 4 ) as a raw material.
- SiCl 4 silicon tetrachloride
- a plate-like double-sided mirror-polished sample having dimensions of 50 ⁇ 50 ⁇ 3 mm in thickness was produced from these synthetic silica glasses.
- barium nitrate alcohol solutions having various concentrations were prepared, applied to the surface of each silica glass sample, and dried.
- each silica glass sample was placed in a clean air atmosphere electric furnace, heated from room temperature to 1500 ° C. in 2 hours, held at 1500 ° C. for 1 hour, and then cooled by turning off the power. Thereafter, the state of white recrystallization on the surface of each sample was visually observed. The results are shown in Table 1.
- the concentration of OH groups is about 200 to 2000 massppm for recrystallization of the surface of the transparent silica glass body at a high temperature (1500 ° C. in the preliminary experiment). It can be seen that it is necessary to apply Ba to the silica glass surface at a concentration of about 25 to 1000 ⁇ g / cm 2 .
- Example 1 According to the steps (1) to (6) shown in FIG. 3, a single crystal silicon pulling silica container was manufactured.
- the raw material powder 11 has a particle size of 50 to 500 ⁇ m and a purity of 99.999 wt. % Natural quartz powder.
- the raw material powder 11 was charged while rotating the graphite mold 101 shown in FIG. 4 and FIG.
- the internal atmosphere of the temporary molded body 41 is a mixed gas of dried H 2 4 vol% and N 2 96 vol%, and the temporary molding is performed while reducing the intake air pressure from the outer periphery. Discharge heating melting was performed inside the body 41.
- the silica container 71 which made the outer side the white opaque silica sintered compact (opaque layer 51) and made the inner side a colorless and transparent silica glass body (transparent layer 52) was produced.
- the atmosphere was changed to water vapor-containing nitrogen gas, and heating was continued to produce a silica container 71 in which the OH group concentration inside the transparent layer 52 was increased.
- the silica container 71 is cooled to room temperature while maintaining the steam-containing gas atmosphere at 200 ° C. or lower, and Ba is applied to the entire inner surface of the cooled silica container 71 at 80 ⁇ g / cm 2 to thereby apply the present invention.
- the silica container 72 (refer FIG. 1) which concerns is manufactured.
- Example 2 A silica container was produced in the same manner as in Example 1 except that the Ba concentration applied to the entire inner surface of the cooled silica container 71 was changed to 480 ⁇ g / cm 2 .
- Example 3 The OH group concentration when increasing the OH group concentration inside the transparent layer 52 was set to 220 massppm, and the Ba concentration applied to the entire inner surface of the cooled silica container 71 was changed to 40 ⁇ g / cm 2.
- a silica container was produced in the same manner as in Example 1.
- Example 4 The OH group concentration when increasing the OH group concentration inside the transparent layer 52 was set to 220 massppm, and the Ba concentration applied to the entire inner surface of the cooled silica container 71 was changed to 800 ⁇ g / cm 2. A silica container was produced in the same manner as in Example 1.
- Example 5 The OH group concentration when increasing the OH group concentration inside the transparent layer 52 was set to 800 massppm, and the Ba concentration applied to the entire inner surface of the cooled silica container 71 was changed to 60 ⁇ g / cm 2.
- a silica container was produced in the same manner as in Example 1.
- Example 6 The OH group concentration when increasing the OH group concentration inside the transparent layer 52 was set to 1200 massppm, and the Ba concentration applied to the entire inner surface of the cooled silica container 71 was changed to 100 ⁇ g / cm 2. A silica container was produced in the same manner as in Example 1.
- Example 7 The OH group concentration when increasing the OH group concentration inside the transparent layer 52 was set to 800 massppm, and the Ba concentration applied to the entire inner surface of the cooled silica container 71 was changed to 30 ⁇ g / cm 2.
- a silica container was produced in the same manner as in Example 1.
- Example 8 The OH group concentration at the time of increasing the OH group concentration inside the transparent layer 52 was set to 1200 massppm, and the Ba concentration applied to the entire inner surface of the cooled silica container 71 was changed to 30 ⁇ g / cm 2.
- a silica container was produced in the same manner as in Example 1.
- Comparative Example 1 From a raw material powder similar to the raw material powder used in Example 1, a silica container (the outer side is a white opaque silica sintered body and the inner side is a colorless transparent silica glass) by a conventional reduced pressure arc melting method (however, in an air atmosphere). Body.). Moreover, Ba was not applied to the inner surface of the silica container.
- Silica containers were produced by the conventional atmospheric pressure melting method and powder material spraying arc melting method. That is, first, a temporary substrate is formed from the raw material powder similar to the raw material powder of Example 1, and a silica substrate comprising a white opaque silica glass layer on the outside and a white translucent silica glass layer on the inside by a normal pressure arc melting method was made. Synthetic cristobalite powder (particle size: 50 to 300 ⁇ m, purity: 99.9999 wt.%) was melted while sprayed inside the silica substrate to form a transparent silica glass layer (additional inner surface layer).
- Example 3 The silica container was manufactured by changing the following points from Example 1. That is, the heating and melting atmosphere of the temporary molded body was changed to air from which water vapor was removed from the beginning, and the cooling process was performed without introducing water vapor. Further, the Ba concentration applied to the entire inner surface of the cooled silica container was changed to 950 ⁇ g / cm 2 .
- Example 4 A silica container was produced in the same manner as in Example 2 except that Ba was not applied to the cooled silica container.
- Method for measuring particle size of raw material powder Two-dimensional shape observation and area measurement of each raw material powder were performed with an optical microscope or an electron microscope. Next, assuming that the shape of the particle is a perfect circle, the diameter was calculated from the area measurement value. This method was repeated statistically and is shown in Tables 2 to 7 as values of the particle size range (the raw material powder of 99 wt.% Or more is included in this range).
- Layer thickness measurement of silica container The thickness of each layer was calculated
- OH group concentration measurement A glass sample was cut and adjusted from the opaque layer portion and the transparent layer portion, and the OH group concentration was measured by infrared absorption spectrophotometry. However, regarding the inner surface portion of the transparent layer, two points of 0.5 mm depth and 1 mm depth from the surface were measured and indicated as arithmetic average values. Further, regarding the deep part of the transparent layer, two points of 1.5 mm depth and 2.0 mm depth were measured and indicated as arithmetic average values.
- Al concentration and Ba concentration analysis Sampling was performed from a portion from the inner surface to a depth of 1 mm and a portion from a depth of 1.5 mm to 2.5 mm, and the solution was adjusted by acid treatment to perform concentration analysis. Concentration analysis was performed by plasma emission spectrometry (ICP-AES), plasma mass spectrometry (ICP-MS), or atomic absorption spectrophotometry (AAS).
- ICP-AES plasma emission spectrometry
- ICP-MS plasma mass spectrometry
- AAS atomic absorption spectrophotometry
- Single crystal silicon continuous pulling (multi pulling) evaluation In the produced silica container, the purity was 99.9999999 wt. % Metal polysilicon was added, the temperature was raised to obtain a silicon melt, and then the single crystal silicon was pulled up three times (multiple pulling), and the success rate of single crystal silicon growth was evaluated.
- the pulling conditions are as follows: the inside of the pulling device (CZ device) is an atmosphere of 100% argon (Ar) gas, the pulling speed is 0.6 mm / min, the single crystal silicon size is 300 mm in diameter, 600 mm in length, and the operation time of one batch is about 80 hours. It was.
- the classification of the success ratio of three times of single crystal silicon growth was as follows. Successful 3 times ⁇ (Good) Successful ⁇ (Slightly bad) 1 success x (bad)
- Etched thickness is less than 1.5mm ⁇ (Good)
- Etched thickness is 1.5mm to less than 3mm ⁇ (somewhat bad)
- Etched thickness is 3mm or more x (defect)
- the etching resistance of the inner surface of the silica container can be increased, and the continuous pulling of the single crystal silicon is in a state where there are few voids, pinholes and foreign matters. I was able to do it. That is, the silica containers of Examples 1 to 8 were generally superior for pulling single crystal silicon than the silica containers of Comparative Examples 1 to 4.
- the present invention is not limited to the above embodiment.
- the above embodiment is merely an example, and the present invention has the same configuration as that of the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.
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Abstract
Description
シリカガラス表面の再結晶化に関するOH基濃度とBa濃度の影響を予備的に検討するため、以下のような実験を行った。
× 再結晶化せず、無色透明のまま
△ 若干再結晶化した、白色半透明化
○ 少しムラが存在するが全面再結晶化した、白色不透明化
◎ 全面均一に再結晶化した、完全な白色不透明化
*1 表面の結晶質シリカ粒が剥がれやすい状態
図3に示した工程(1)~(6)に従い、単結晶シリコン引き上げ用シリカ容器を製造した。まず、原料粉11として、粒径50~500μm、純度99.999wt.%の天然石英粉を作製した。
冷却したシリカ容器71の内側表面全面に塗布するBa濃度を480μg/cm2に変更した他は、実施例1と同様にシリカ容器を製造した。
透明層52の内側のOH基濃度を高める際のOH基濃度を220massppmに設定し、かつ、冷却したシリカ容器71の内側表面全面に塗布するBa濃度を40μg/cm2に変更した他は、実施例1と同様にシリカ容器を製造した。
透明層52の内側のOH基濃度を高める際のOH基濃度を220massppmに設定し、かつ、冷却したシリカ容器71の内側表面全面に塗布するBa濃度を800μg/cm2に変更した他は、実施例1と同様にシリカ容器を製造した。
透明層52の内側のOH基濃度を高める際のOH基濃度を800massppmに設定し、かつ、冷却したシリカ容器71の内側表面全面に塗布するBa濃度を60μg/cm2に変更した他は、実施例1と同様にシリカ容器を製造した。
透明層52の内側のOH基濃度を高める際のOH基濃度を1200massppmに設定し、かつ、冷却したシリカ容器71の内側表面全面に塗布するBa濃度を100μg/cm2に変更した他は、実施例1と同様にシリカ容器を製造した。
透明層52の内側のOH基濃度を高める際のOH基濃度を800massppmに設定し、かつ、冷却したシリカ容器71の内側表面全面に塗布するBa濃度を30μg/cm2に変更した他は、実施例1と同様にシリカ容器を製造した。
透明層52の内側のOH基濃度を高める際のOH基濃度を1200massppmに設定し、かつ、冷却したシリカ容器71の内側表面全面に塗布するBa濃度を30μg/cm2に変更した他は、実施例1と同様にシリカ容器を製造した。
実施例1で用いた原料粉と同様の原料粉から、従来法の減圧アーク溶融法(ただし、空気雰囲気)により、シリカ容器(外側は白色不透明シリカ焼結体であり、内側は無色透明シリカガラス体である。)を作製した。また、シリカ容器内表面にBaを塗布することはしなかった。
従来法の常圧アーク溶融法及び粉体原料散布アーク溶融法でシリカ容器を製造した。すなわち、まず、実施例1の原料粉と同様の原料粉から仮成形体を形成し、常圧アーク溶融法により、外側が白色不透明シリカガラス層、内側が白色半透明シリカガラス層からなるシリカ基体を作製した。このシリカ基体の内側に合成クリストバライト粉(粒径50~300μm、純度99.9999wt.%)を散布しつつ溶融させて、透明シリカガラス層(追加内表層)を形成した。
実施例1から以下の点を変更してシリカ容器を製造した。すなわち、仮成形体の加熱溶融雰囲気を終始水蒸気を除去した空気とし、水蒸気を導入しないまま冷却工程に移行した。また、冷却したシリカ容器の内側表面全面に塗布するBa濃度を950μg/cm2に変更した。
冷却後のシリカ容器にBaを塗布しないこと以外は、実施例2と同様にしてシリカ容器を製造した。
各実施例及び比較例において用いた原料粉及び製造したシリカ容器の物性、特性評価を以下のようにして行った。
光学顕微鏡又は電子顕微鏡で各原料粉の二次元的形状観察及び面積測定を行った。次いで、粒子の形状を真円と仮定し、面積測定値から直径を計算して求めた。この手法を統計的に繰り返し行い、粒径の範囲(この範囲の中に99wt.%以上の原料粉が含まれる)の値として、表2~7に示した。
シリカ容器をカッターで切断し、シリカ容器の側壁全高さの中央部分における断面をスケールで測定することにより、各層の厚さを求めた。
不透明層部分、透明層部分からガラスサンプルを切断、調整し、赤外線吸収分光光度法でOH基濃度測定を行った。ただし、透明層内表面部に関しては、表面から0.5mm深さ及び1mm深さの2点を測定し、算術平均値として示した。また、透明層深部に関しては1.5mm深さ及び2.0mm深さの2点を測定し、算術平均値として示した。
Dodd,D.M. and Fraser,D.B.(1966) Optical determination of OH in fused silica. Journal of Applied Physics, vol.37, P.3911.
内表面から深さ1mmまでの部分及び深さ1.5mmから2.5mmまでの部分から各々薄片状にサンプリングし、酸処理により溶液調整を行い、濃度分析を行った。濃度分析は、プラズマ発光分析法(ICP-AES)又はプラズマ質量分析法(ICP-MS)又は原子吸光光度法(AAS)で行った。
製造したシリカ容器の中に純度99.9999999wt.%の金属ポリシリコンを投入し、昇温を行いシリコン融液とし、次いで単結晶シリコンの引き上げを3回繰り返して行い(マルチ引き上げ)、単結晶シリコン育成の成功率として評価した。引き上げ条件は、引き上げ装置(CZ装置)内をアルゴン(Ar)ガス100%雰囲気、引き上げ速度0.6mm/分、単結晶シリコン寸法は直径300mm、長さ600mm、1バッチの操業時間は約80時間とした。単結晶シリコン育成3回繰り返しの成功比率の分類は以下の通りとした。
3回成功 ○(良好)
2回成功 △(やや不良)
1回成功 ×(不良)
前記の単結晶シリコン連続引き上げにおいて、各単結晶シリコンマルチ引き上げ後の1本目の単結晶シリコンの任意の部位から、直径300mm、厚さ200μmの両面研磨仕上げのシリコンウェーハ各200枚を作製した。次いで各々のシリコンウェーハの両面に存在するボイドとピンホールと異物の個数をパーティクル検出器により測定し、統計的に数値処理を行いシリコンウェーハ200枚あたりの欠陥の無い枚数を求めた。ボイド、ピンホール、異物のいずれも検出されないシリコンウェーハ枚数に応じて以下のような評価とした。
無欠陥シリコンウェーハ枚数 200枚~199枚 ○
無欠陥シリコンウェーハ枚数 198枚~197枚 △
無欠陥シリコンウェーハ枚数 196枚以下 ×
前記の単結晶シリコン連続引き上げの評価終了後、各シリカ容器の当初のシリコン融液面上部近くの部分(シリコン融液と接触していない部分)から、シリカ容器側壁の全厚さにわたって、寸法が200mm×50mm×側壁全厚さであるサンプルを切り出した。次いで、ルツボ形状の評価試験用シリカガラス製容器を別途用意し、用意した評価試験用シリカガラス製容器内に多結晶シリコンを充填し電気炉で溶融し、シリコン融液とした。該シリコン融液中に各サンプルの下部半分を沈めた。この状態で電気炉内で1500℃で80時間保持した後、各サンプルを引き上げた。次いで、各サンプルのうち、切り出す前にシリカ容器内表面側であった側の表面のエッチング量を、断面厚さをスケールで測定することにより求めた。
エッチングされた厚さが1.5mm未満 ○(良好)
エッチングされた厚さが1.5mm~3mm未満 △(やや不良)
エッチングされた厚さが3mm以上 ×(不良)
Claims (5)
- 内側に透明シリカガラスから成る透明層を有し、外側に気泡を含有する不透明シリカガラスから成る不透明層を有する単結晶シリコン引き上げ用シリカ容器であって、
前記透明層が、前記シリカ容器の内表面側に位置し、OH基を200~2000massppmの濃度で含有する高OH基層と、該高OH基層よりもOH基濃度が低い低OH基層とから成り、
前記高OH基層の内表面にBaが25~1000μg/cm2の濃度で塗布されているものである
ことを特徴とする単結晶シリコン引き上げ用シリカ容器。 - 前記高OH基層の厚さが0.5mm以上3mm以下であることを特徴とする請求項1に記載の単結晶シリコン引き上げ用シリカ容器。
- 前記高OH基層が含有するOH基の濃度が300~1500massppmの濃度であり、
前記高OH基層の内表面に塗布されたBaの濃度が60~500μg/cm2である
ことを特徴とする請求項1又は請求項2に記載の単結晶シリコン引き上げ用シリカ容器。 - 単結晶シリコン引き上げ用シリカ容器の製造方法であって、
原料粉として、粒径10~1000μmのシリカ粉を作製する工程と、
前記原料粉を型枠内に投入し、該型枠を回転させつつ該型枠の内壁に応じた所定の形状に仮成形して仮成形体を作製する工程と、
前記型枠内の仮成形体を回転させるとともに該仮成形体を外側から減圧することにより該仮成形体に含まれるガス成分を脱ガスさせつつ、放電加熱溶融法により前記仮成形体を加熱溶融させ、内側を透明シリカガラスから成る透明層とし、外側を気泡を含有する不透明シリカガラスから成る不透明層としたシリカ容器を作製する工程と、
前記作製したシリカ容器の内側に水蒸気含有ガスを導入し、該水蒸気含有ガス雰囲気にて加熱を継続することにより、前記透明層のうち、内表面側のOH基濃度を高める工程と、
前記水蒸気含有ガス雰囲気による加熱を行ったシリカ容器を室温まで冷却する工程と、
前記冷却したシリカ容器の透明層の内表面にBa化合物を塗布し、乾燥させることにより、前記透明層の内表面にBaを25~1000μg/cm2の濃度で塗布する工程と
を含み、
前記水蒸気含有ガス雰囲気による加熱及び前記冷却により、前記透明層の内表面側の領域において、OH基濃度を200~2000massppmとすること
を特徴とする単結晶シリコン引き上げ用シリカ容器の製造方法。 - 前記冷却工程において、少なくとも200℃以下の温度に低下するまで前記シリカ容器の内側を水蒸気含有ガス雰囲気とすることを特徴とする請求項4に記載の単結晶シリコン引き上げ用シリカ容器の製造方法。
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-
2013
- 2013-03-18 WO PCT/JP2013/001839 patent/WO2013171955A1/ja active Application Filing
- 2013-03-18 CN CN201380002396.7A patent/CN103703171A/zh active Pending
- 2013-03-18 KR KR1020147009050A patent/KR20140058678A/ko active Search and Examination
- 2013-03-18 JP JP2014502284A patent/JP5595615B2/ja active Active
- 2013-03-18 US US14/234,588 patent/US20140150715A1/en not_active Abandoned
- 2013-03-18 EP EP13791405.7A patent/EP2725122A4/en not_active Withdrawn
- 2013-04-22 TW TW102114214A patent/TWI486314B/zh not_active IP Right Cessation
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016047693A1 (ja) * | 2014-09-24 | 2016-03-31 | 株式会社Sumco | シリコン単結晶の製造方法及び製造システム |
WO2022249570A1 (ja) * | 2021-05-25 | 2022-12-01 | 株式会社Sumco | 石英ガラスルツボ及びその製造方法並びにシリコン単結晶の製造方法 |
Also Published As
Publication number | Publication date |
---|---|
TW201348157A (zh) | 2013-12-01 |
CN103703171A (zh) | 2014-04-02 |
TWI486314B (zh) | 2015-06-01 |
JPWO2013171955A1 (ja) | 2016-01-12 |
KR20140058678A (ko) | 2014-05-14 |
US20140150715A1 (en) | 2014-06-05 |
EP2725122A4 (en) | 2015-04-08 |
JP5595615B2 (ja) | 2014-09-24 |
EP2725122A1 (en) | 2014-04-30 |
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