US3565346A - Method and apparatus for forming an article of high purity metal oxide - Google Patents
Method and apparatus for forming an article of high purity metal oxide Download PDFInfo
- Publication number
- US3565346A US3565346A US744188A US3565346DA US3565346A US 3565346 A US3565346 A US 3565346A US 744188 A US744188 A US 744188A US 3565346D A US3565346D A US 3565346DA US 3565346 A US3565346 A US 3565346A
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- United States
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- torch
- nozzle
- sheath
- silicon tetrachloride
- gas
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- Expired - Lifetime
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- 238000000034 method Methods 0.000 title description 8
- 229910044991 metal oxide Inorganic materials 0.000 title description 5
- 150000004706 metal oxides Chemical class 0.000 title description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000007789 gas Substances 0.000 claims abstract description 55
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 42
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000001301 oxygen Substances 0.000 claims abstract description 41
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 41
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 29
- 239000012159 carrier gas Substances 0.000 claims abstract description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 230000007062 hydrolysis Effects 0.000 claims abstract description 11
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims description 13
- 239000011261 inert gas Substances 0.000 claims description 11
- 229910001510 metal chloride Inorganic materials 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000012809 cooling fluid Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 239000012808 vapor phase Substances 0.000 abstract description 5
- 238000002485 combustion reaction Methods 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 description 16
- 235000012239 silicon dioxide Nutrition 0.000 description 10
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 239000000155 melt Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 229910021386 carbon form Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 235000015250 liver sausages Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- XYSQXZCMOLNHOI-UHFFFAOYSA-N s-[2-[[4-(acetylsulfamoyl)phenyl]carbamoyl]phenyl] 5-pyridin-1-ium-1-ylpentanethioate;bromide Chemical compound [Br-].C1=CC(S(=O)(=O)NC(=O)C)=CC=C1NC(=O)C1=CC=CC=C1SC(=O)CCCC[N+]1=CC=CC=C1 XYSQXZCMOLNHOI-UHFFFAOYSA-N 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/28—Slip casting
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
- C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1415—Reactant delivery systems
- C03B19/1423—Reactant deposition burners
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/30—Drying methods
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/04—Multi-nested ports
- C03B2207/06—Concentric circular ports
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/04—Multi-nested ports
- C03B2207/12—Nozzle or orifice plates
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/20—Specific substances in specified ports, e.g. all gas flows specified
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/42—Assembly details; Material or dimensions of burner; Manifolds or supports
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/80—Feeding the burner or the burner-heated deposition site
- C03B2207/85—Feeding the burner or the burner-heated deposition site with vapour generated from liquid glass precursors, e.g. directly by heating the liquid
- C03B2207/86—Feeding the burner or the burner-heated deposition site with vapour generated from liquid glass precursors, e.g. directly by heating the liquid by bubbling a gas through the liquid
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/80—Feeding the burner or the burner-heated deposition site
- C03B2207/85—Feeding the burner or the burner-heated deposition site with vapour generated from liquid glass precursors, e.g. directly by heating the liquid
- C03B2207/87—Controlling the temperature
Definitions
- a sheath of oxygen containing gases is 56] Ref Cit d streamed about the jet stream of silicon tetrachloride in order erences e to prevent reaction immediately adjacent the face of the torch UNITED STATES PATENTS nozzle with a stream of combustible gas provided about the 2,719,581 10/1955 Greathead 239/132.3 sheath of gas.
- the resulting flame is 2,827,112 3/1958 lnskeep 239/ 132.3 directly applied to the mandrel wherein a layer of high purity 3,224,679 9 K 6! 23 132-3 silica is deposited thereon due to the vapor phase hydrolysis of 3,339,616 9/1967 Ward, 11'. et al. 239/1 32.3 the silicon tetrachloride.
- monocrystalline silicon is pulled" from a melt of silicon. Due to the extremely high temperatures required to provide a melt of silicon, it has been found that appreciable quantities of the material from which the crucible is constructed is lost within the melt. l-Ience, any impurities in the crucible enter into the pulled monocrystalline silicon. It has thus been found advantageous to construct the silicon melt crucible from very pure silica. It is also extremely important to provide a uniform pull" from the silicon melt, and it is thus necessary that the crucible have very uniform sidewalls and a symmetrical configuration in order to prevent sudden changes in the level of the melt during pulling due to irregularities in the crucible configuration.
- a volatile metallic chloride is vaporized and entrained in a carrier gas and then streamed from a jet nozzle.
- a stream of combustible gas is formed symmetrically about the jet stream, with interaction between the two streams being prevented in a preselected region adjacent the jet nozzle.
- the streams are ignited at a zone of interaction to form a flame which is directed upon a mandrel to form an article of high purity oxide directly thereupon.
- a torch is provided with a central passage therethrough for receiving gaseous silicon tetrachloride entrained in carrier gas.
- a nozzle aperture is defined in one end of the passage to provide an output jet stream of gaseous silicon tetrachloride entrained in the carrier gas.
- a sheath chamber defined in the torch ineludes an inlet for receiving an oxygen-containing gas and has an annular opening concentrically disposed about the nozzle aperture to provide a circular stream of oxygen-containing gas around the jet stream.
- a mixing chamber is disposed about the sheath chamber within the torch body and includes inlets for hydrogen and oxygen-containing gases.
- a plurality of output openings are disposed symmetrically around the annular sheath opening to provide streams of gaseous combustible mixture to allow the torch to be ignited and directed upon a mandrel for the deposition of high purity silica thereon.
- FIG. 1 illustrates somewhat diagrammatically the formation of a silica crucible upon a rotating mandrel with the present torch
- FIG. 2 illustrates an embodiment of the present torch
- FIG. 3 illustrates an end view of the nozzle of the torch shown in FIG. 2;
- FIG. 4 illustrates a sectional side view of another embodiment of a torch according to the invention
- FIG. 5 is an end view illustrating the nozzles of the torch shown in FIG. 4.
- FIG. 6 is a sectional view taken generally along the section lines 6-6 in FIG. 4.
- the torch designated generally by the numeral 10 provides a flame for providing vapor phase hydrolysis of a gaseous volatile metal chloride to produce a metal oxide which is deposited upon a rotating mandrel 12.
- silicon tetrachloride is decomposed to form silicon dioxide according to the following equation:
- the flame produced from the torch 10 is shown diagrammatically as comprising a very hot central portion 14 wherein a vaporized silicon tetrachloride stream 16 reacts with a concentric stream of combustible gas 18 including a mixture of hydrogen and oxygen.
- the streams 16 and 18 interact at some distance below the nozzle of the torch 10 in a reaction zone which is spaced a short distance from the nozzle of the torch 10. This spacing of the reaction zone from the torch nozzle is due to the provision of a stream of sheath gas 20 around the stream of silicon tetrachloride 16, as will be subsequently described in greater detail.
- the mandrel 112 is preferably constructed from graphite and may include a suitable hard metal coating over the surface thereof.
- the mandrel 12 is rotated in the direction of the arrow 22 and is translated in a direction of the arrow 24 while the torch 10 remains stationary.
- a silica article is deposited upon the mandrel as it translates past the stationary torch 10.
- the rate of translation of the mandrel 12 is dependent upon the desired thickness of the silica article and upon parameters of the torch flame, such as flow rates of the various gases and the like. After the silica article has been deposited to the desired thickness upon the mandrel 12, the article is removed and treated with various desired processing steps to provide a final product.
- the articles have sufficient green strength" to allow removal from the mandrel due to a slight degree of sintering of the silicon dioxide particles during deposition.
- a separate conventional torch flame may be impinged on the article after deposition thereof to insure that sufficient green strength is provided.
- FIG. 2 illustrates in greater detail the preferred embodiment of the present torch 10.
- a stainless steel tube 30 extends through the length of the torch to provide a passage for vaporized silicon tetrachloride entrained in a carrier gas.
- a T- connection 32 is connected about the tube and is sealed to the tube 30 by member 34.
- a member 36 fits over a stainless steel tube 38 to provide a seal between the end of tube 38 and the tube 30.
- An annular sheath chamber 40 is thus defined between the tube 30 and tube 38.
- An inlet portion 42 of the T- connection 32 is connected to a source of sheath gas, in this instance oxygen-containing gas, so that the sheath gas is passed into the sheath chamber 40.
- a source of sheath gas in this instance oxygen-containing gas
- An annular spacer member 44 provides a fluid seal between the tube 38 and one end of a housing 46.
- Housing 46 receives a tube 48 which defines an annular mixing chamber 50 about tube 58.
- An inlet fitting 52 is connected to a source of hydrogen while an inlet fitting 54 is connected to a source of oxygen.
- Housing 46 includes a large diameter portion 56 which defines an annular cooling chamber about the tube 48.
- An inlet fitting 58 is connected to a source of cooling fluid, such as cool water, and an outlet fitting 60 allows exhausting of the cooling fluid.
- the smaller diameter portion of the housing 46 was constructed of stainless steel, while the larger diameter portion 56 of the housing was constructed of brass to prevent corrosion thereof by the cooling fluid.
- tube 48 was constructed from stainless steel and was provided with a diameter of 1 /8 inch. The entire length of the torch 10 in this embodiment thereof was approximately 9 inches.
- the nozzle 62 is fitted over the end of the torch 10. As shown in FIGS. 2 and 3, the nozzle 62 comprises a circular member with bent flanges 64 for fluid-tight connection to the torch.
- a central nozzle aperture 66 is provided in the end of tube 30.
- the end of tube 30 is received by an opening in nozzle 62 to define an annular sheath opening 68 which is concentrically disposed relative to the aperture 66 and has a substantially greater area than the aperture 66.
- Nozzle aperture 66 has a substantially smaller area than the interior area of the tube 30, such that a relatively high velocity jet of gas is provided from the nozzle aperture 66.
- Gas flowing from the concentric sheath opening 68 substantially envelopes the jet of gas from the nozzle aperture 66 to prevent immediate reaction thereof, thereby reducing crystalline accumulation of the face of the nozzle member 62 and preventing obstruction thereof.
- a plurality of apertures 70 are symmetrically disposed around the nozzle aperture 66 in a cylindrical configuration and communicate with the mixing chamber 50.
- a combustible gas contained in the mixing chamber 50 flows out of the apertures 70 and reacts with the gas flowing from the aperture 66.
- eight apertures 70 were provided, each having substantially the same area sa the nozzle aperture 66. In this practical embodiment of the torch, diameters of .063 inch were found advantageous for aperture 66 and apertures 70. For different operating conditions, greater or larger numbers of aperture 70 may be used.
- Oxygen is supplied via conduit 72 to the inlet of three flowmeters 74, 76 and 78.
- a suitable source supplies hydrogen through a conduit 80 to a flowmeter 82.
- the oxygen and hydrogen are dried prior to entering the flowmeters.
- Suitable valves are provided on the output of each of the flowmeters in order to allow regulation of the rate of flow of the hydrogen and oxygen to the e system.
- Oxygen is fed via a conduit 84 to a bubbler system designated generally by the numeral 86.
- Bubbler system 86 comprises a container filled with liquid silicon tetrachloride.
- a diffusing element 88 bubbles the oxygen upwardly through the silicon tetrachloride, thereby entraining vapors of the silicon tetrachloride in the oxygen and passing outwardly through the conduit 90.
- Conduit 90 is connected to the tube 30 to provide a metered stream of vaporized silicon tetrachloride entrained in the oxygen carrier gas.
- Oxygen is also supplied through the flowmeter 74 via a conduit 92 to the inlet fitting 42 of the T-connection member 32. Oxygen thus .flows into the sheath chamber 40 and out the annular aperture 68 in the manner previously described.
- Oxygen is further supplied via conduit 94 to the inlet fitting 54 for passage into the mixing chamber 50.
- Hydrogen is supplied through the flowmeter 82 via a conduit 96 into the inlet fitting 52 for mixing with the oxygen inside the mixing chamber 50. A mixture of combustible gas is then fed outwardly through the aperture 70 in the manner described. Because the hydrogen and oxygen are mixed within the small chamber 50 within the torch, flashback in the present torch is limited to the interior of the torch itself.
- FIGS. 4-6 illustrate another embodiment of the invention where a plurality of flames are provided.
- a metal block 10 has defined therein a generally rectangular chamber 102 including an inlet 104 for the admission of silicon tetrachloride vapors entrained in a suitable carrier gas.
- a chamber 122 is formed in the general central region of the block and includes an inlet 124 for a sheath gas such as oxygen.
- the chamber 122 includes four sheath passageways 126- 132 for passing the oxygen-containing gas outwardly through annular sheath gas openings 134- 140.
- a pair of chambers 142 and 143 are defined within the body 100 for respectively receiving a mixture of oxygen and hydrogen.
- the mixture of oxygen and hydrogen is then flowed outwardly through a plurality of apertures 144 and 145 for reaction with the gaseous silicon tetrachloride.
- the torch When ignited, the torch provides four flames to provide an even application of silicon dioxide upon a mandrel in the manner previously described.
- Water cooled pipes may be disposed on the sides of the body in order to provide cooling thereof.
- the sheath of oxygen flowing from the annular apertures 134-140 prevent accumulation of crystals on the face of the nozzles and therefore prevent obstruction of the torch during usage thereof.
- EXAMPLE 1 A torch constructed in accordance with FIGS. 2 and 3 was connected to a gas supply system similar to that shown in FIG. 2 and ignited. The diameter of the center nozzle aperture of the torch was .049 inch. A nonrotating mandrel constructed of graphite was disposed 4 inches from the nozzle of the torch and the flame issuing from the torch was impinged upon the graphite mandrel for 20 minutes. The temperature of the flame approximately one-fourth inch from the mandrel was in the range of 1,500 C. One liter per minute of oxygen and l .56 liters per minute of silicon tetrachloride entrained in the oxygen was provided to the torch. To provide this flow of gas, the bubbler shown in FIG.
- Optimum efficiency was usually obtained at percentages of silicon tetrachloride below 60 percent of silicon tetrachloride in the carrier gas stream. For instance, a 20 minute deposition was provided in the manner described in example 1, with the exception that only .75 liters per minute of silicon tetrachloride was entrained in 1 liter per minute of oxygen.
- EXAMPLE 3 It was found that for a particular construction of the torch and with a particular combination of gas flow rates, an optimum distance between the torch nozzle and the mandrel existed which provided increased deposition rates. For instance, an experiment was run utilizing essentially the same flow rates and other parameters of example 2, but with the distance between the torch nozzle and the mandrel being 5 inches. In this example, only 15.9 actual grams of silicon dioxide were deposited to provide a deposition efficiency of 43 percent. For the particular torch used, it was found that a mandrel distance in the range of 4 inches was desirable.
- EXAMPLE 4 Good results were also obtained with use of the present torch by the utilization of a larger bubbler gas noule aperture at higher flow rates. For instance, a minute run was conducted utilizing a nozzle having a nozzle aperture of a diameter of .063 inches and spaced 4 inches from a mandrel. A supply of oxygen at a rate of 2 liters per minute was provided to the bubbler which was maintained at 49 C. at a pressure of 5 pounds per inch. Vaporized silicon tetrachloride was entrained in the carrier gas at a rate of 2.88 liters per minute to provide a percentage of silicontetrachloride in the entrained gas of 59 percent.
- a supply of oxygen at a rate of 1 liter per minute was supplied to the sheath chamber of the torch.
- a supply of oxygen at a rate of 5 .2 liters per minute was supplied to the mixing chamber of the torch along with a supply of hydrogen at a rate of 30 liters per minute to provide the mixture of combustible gases.
- An output velocity at the nozzle aperture of 8 X 10 feet per minute was provided.
- a deposition of 68 grams of silicon dioxide was provided by the 20 minute run to provide a deposition efficiency of 48 percent.
- the present invention thus provides a unique technique for forming high purity articles on mandrels by the direct application of oxides due to vapor phase hydrolysis by flame.
- oxygen-containing gases as used in the specification is meant to include pure oxygen. While the specification has been disclosed specifically with respect to the deposition of silicon dioxide by the decomposition of silicon tetrachloride, it will be understood that other volatile anhydrous chlorides of metallic elements from groups Ill and IV of the periodic system, such as for example, titanium tetrachloride, aluminum tetrachloride and the like could additionally be advantageously decomposed with the present technique.
- a torch for decomposing a volatile metallic element by hydrolysis to directly form an oxide article on a surface comprising;
- a torch housing including a passage terminating in a nozzle aperture for providing an output jet stream of said volatile metallic element entrained in a carrier gas;
- b. means defining a first chamber disposed adjacent said passage within said torch housing for receiving a supply of a combustible gas and including nozzle openings symmetrically disposed to said nozzle aperture for providing a stream of combustible gas about said jet stream;
- c. means defining a second chamber disposed between said passage and said first chamber for receiving a supply of gas relatively inert to said volatile metallic element and includinga sheath opening for providing a sheath stream of said inert gas between said jet stream and said stream of combustible gas sufficient when the torch is ignited to prevent residue from being formed on said nozzle aperture during operation.
- a torch for forming a silica article directly upon a mandrel by hydrolysis of silicon tetrachloride entrained in a carrier gas comprising:
- a torch housing having a central passage therethrough with an inlet at one end for receiving gaseous silicon tetrachloride entrained in a carrier gas and having a nozzle aperture at the other end to provide an output jet stream of gaseous silicon tetrachloride entrained in a carrier gas;
- a sheath chamber defined in said torch housing about said central passage including an inlet for receiving a relatively inert gas with respect to silicon tetrachloride and having an annular opening concentrically disposed about said nozzle aperture to provide a circular stream of said inert gas around said jet stream;
- a mixing chamber disposed about said sheath chamber including inlets for hydrogen and oxygen containing gases and a plurality of outlet openings disposed symmetrically adjacent said annular opening to provide streams of gaseous combustible mixture around said circular stream of said inert gas, whereby the flame resulting from ignition of said torch may be kept away from said nozzle.
- a torch for direct formation of an oxide article on a mandrel by they hydrolysis of a volatile metal chloride comprising:
- a torch housing including inlet means for receiving a supply of the vapor of said volatile metal chloride
- each said stream of combustible gas is supplied from an aperture spaced radially outwardly from said annular opening.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Silicon Compounds (AREA)
- Chemical Vapour Deposition (AREA)
- Glass Melting And Manufacturing (AREA)
- Carbon And Carbon Compounds (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US74418868A | 1968-07-11 | 1968-07-11 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3565346A true US3565346A (en) | 1971-02-23 |
Family
ID=24991797
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US744188A Expired - Lifetime US3565346A (en) | 1968-07-11 | 1968-07-11 | Method and apparatus for forming an article of high purity metal oxide |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US3565346A (enExample) |
| JP (1) | JPS4925416B1 (enExample) |
| DE (1) | DE1934931A1 (enExample) |
| FR (1) | FR2012729A1 (enExample) |
| GB (1) | GB1272143A (enExample) |
| NL (1) | NL6910692A (enExample) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3814327A (en) * | 1971-04-06 | 1974-06-04 | Gen Electric | Nozzle for chemical reaction processes |
| US3825400A (en) * | 1973-04-17 | 1974-07-23 | V Popov | Gas fuel blowpipe for burning reaction gas mixtures |
| US3837825A (en) * | 1971-04-19 | 1974-09-24 | Sherwood Refractories | Process for making transparent silica glass |
| US3856457A (en) * | 1972-12-29 | 1974-12-24 | Air Prod & Chem | Burner of the oxy-fuel type |
| US4136828A (en) * | 1977-06-27 | 1979-01-30 | Corning Glass Works | Oxide depositing ribbon burner |
| DE2849111A1 (de) * | 1977-11-15 | 1979-05-17 | Nippon Steel Corp | Flammenspritzvorrichtung fuer feuerfestpulver |
| US4203553A (en) * | 1977-06-27 | 1980-05-20 | Corning Glass Works | Ribbon burner |
| US4717075A (en) * | 1986-07-18 | 1988-01-05 | Northern Research & Engineering Corp. | Particulate dispersion apparatus |
| US5735928A (en) * | 1993-06-18 | 1998-04-07 | Tsl Group Plc | Apparatus for manufacturing a vitreous silica article |
| US20030133850A1 (en) * | 1999-12-23 | 2003-07-17 | Watson Richard William | Partial oxidation of hydrogen sulphide containing gas |
| US6763663B2 (en) | 2001-07-11 | 2004-07-20 | Parker-Hannifin Corporation | Injector with active cooling |
| US20060162389A1 (en) * | 2002-12-20 | 2006-07-27 | Carlo Cognolato | Burner for chemical vapour deposition of glass |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5521679U (enExample) * | 1978-07-28 | 1980-02-12 | ||
| DE3403894C1 (de) * | 1984-02-04 | 1985-07-25 | Kulzer & Co GmbH, 6393 Wehrheim | Vorrichtung zum Beschichten eines metallischen Dentalprothesenteils und Verfahren zum Betrieb einer solchen Vorrichtung |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2719581A (en) * | 1952-02-13 | 1955-10-04 | Selas Corp Of America | Welding torch |
| US2827112A (en) * | 1953-08-28 | 1958-03-18 | Union Carbide Corp | Flame blasting and apparatus therefor |
| FR1249283A (fr) * | 1959-11-07 | 1960-12-30 | Tech D Expl De Chauffage Soc | Procédé de brassage d'un mélange combustible et brûleur pour la mise en oeuvre de ce procédé |
| US3224679A (en) * | 1962-06-26 | 1965-12-21 | Shell Oil Co | Combustion device for hydrocarbon fuel |
| US3339616A (en) * | 1965-06-03 | 1967-09-05 | Chemetron Corp | Apparatus for combustion of fuels and burner therefor |
| US3364970A (en) * | 1967-04-03 | 1968-01-23 | Messer Griesheim Gmbh | Cutting torch nozzle and method |
| US3387784A (en) * | 1966-10-27 | 1968-06-11 | Chemetron Corp | Burner for fluid fuels |
| US3411717A (en) * | 1966-07-01 | 1968-11-19 | John H. Flynn | Liquid-cooled gas burner |
-
1968
- 1968-07-11 US US744188A patent/US3565346A/en not_active Expired - Lifetime
-
1969
- 1969-06-17 GB GB30591/69A patent/GB1272143A/en not_active Expired
- 1969-07-08 FR FR6923149A patent/FR2012729A1/fr not_active Withdrawn
- 1969-07-10 DE DE19691934931 patent/DE1934931A1/de active Pending
- 1969-07-10 JP JP44054797A patent/JPS4925416B1/ja active Pending
- 1969-07-11 NL NL6910692A patent/NL6910692A/xx unknown
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2719581A (en) * | 1952-02-13 | 1955-10-04 | Selas Corp Of America | Welding torch |
| US2827112A (en) * | 1953-08-28 | 1958-03-18 | Union Carbide Corp | Flame blasting and apparatus therefor |
| FR1249283A (fr) * | 1959-11-07 | 1960-12-30 | Tech D Expl De Chauffage Soc | Procédé de brassage d'un mélange combustible et brûleur pour la mise en oeuvre de ce procédé |
| US3224679A (en) * | 1962-06-26 | 1965-12-21 | Shell Oil Co | Combustion device for hydrocarbon fuel |
| US3339616A (en) * | 1965-06-03 | 1967-09-05 | Chemetron Corp | Apparatus for combustion of fuels and burner therefor |
| US3411717A (en) * | 1966-07-01 | 1968-11-19 | John H. Flynn | Liquid-cooled gas burner |
| US3387784A (en) * | 1966-10-27 | 1968-06-11 | Chemetron Corp | Burner for fluid fuels |
| US3364970A (en) * | 1967-04-03 | 1968-01-23 | Messer Griesheim Gmbh | Cutting torch nozzle and method |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3814327A (en) * | 1971-04-06 | 1974-06-04 | Gen Electric | Nozzle for chemical reaction processes |
| US3837825A (en) * | 1971-04-19 | 1974-09-24 | Sherwood Refractories | Process for making transparent silica glass |
| US3856457A (en) * | 1972-12-29 | 1974-12-24 | Air Prod & Chem | Burner of the oxy-fuel type |
| US3825400A (en) * | 1973-04-17 | 1974-07-23 | V Popov | Gas fuel blowpipe for burning reaction gas mixtures |
| US4203553A (en) * | 1977-06-27 | 1980-05-20 | Corning Glass Works | Ribbon burner |
| US4136828A (en) * | 1977-06-27 | 1979-01-30 | Corning Glass Works | Oxide depositing ribbon burner |
| DE2849111A1 (de) * | 1977-11-15 | 1979-05-17 | Nippon Steel Corp | Flammenspritzvorrichtung fuer feuerfestpulver |
| US4717075A (en) * | 1986-07-18 | 1988-01-05 | Northern Research & Engineering Corp. | Particulate dispersion apparatus |
| US5735928A (en) * | 1993-06-18 | 1998-04-07 | Tsl Group Plc | Apparatus for manufacturing a vitreous silica article |
| US20030133850A1 (en) * | 1999-12-23 | 2003-07-17 | Watson Richard William | Partial oxidation of hydrogen sulphide containing gas |
| US6763663B2 (en) | 2001-07-11 | 2004-07-20 | Parker-Hannifin Corporation | Injector with active cooling |
| US20060162389A1 (en) * | 2002-12-20 | 2006-07-27 | Carlo Cognolato | Burner for chemical vapour deposition of glass |
| US8567218B2 (en) | 2002-12-20 | 2013-10-29 | Prysmian Cavi E Sistemi Energia S.R.L. | Burner for chemical vapour deposition of glass |
Also Published As
| Publication number | Publication date |
|---|---|
| GB1272143A (en) | 1972-04-26 |
| NL6910692A (enExample) | 1970-01-13 |
| JPS4925416B1 (enExample) | 1974-06-29 |
| DE1934931A1 (de) | 1970-01-15 |
| FR2012729A1 (enExample) | 1970-03-20 |
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