TWI291940B - A method of producing glass of optical quality - Google Patents

Description

1291940 A7 B7 V. INSTRUCTION DESCRIPTION (d) The present invention relates to a method of making optical quality glass comprising melting or 'purifying a pre-sintered composition as appropriate, and applying the method to deposit a pre-sintered composition that has been purified as desired On a fiber optic prototype, a substantially cylindrical prototype extending in the direction of the major axis is set to rotate about its axis at a plasma or flame front end, and the plasma or flame is solidly parallel to the young The long axis direction of the type moves back and forth, and a first feed conduit supplies the pre-sintered composition particles. The preform is chemically vapor deposited in a known manner via a tube inside a tube mounted on a glass manufacturing lathe. And it is obtained by performing a collapsing operation to form a solid prototype. For multimode fibers, this method of making prototypes is sufficient. However, for single-mode fibers, it is advantageous to be in the chicks. The substance is added to the type to increase its diameter and, thus, in the fiber extraction, continuous fibers having a length of several tens of kilometers are obtained. a torch) is added to the prototype. The shape of the prototype is cylindrical and its rotation is set around its axis in front of the torch, and the plasma of the torch is fed with material particles, such as pre-sintered composition. The particles are melted, deposited, and vitrified on the prototype. A number of passes are required to accumulate to the desired diameter. Deposited materials, such as pre-sintered compositions, have a significant defect. Neglecting amounts of alkali elements such as sodium or lithium, and they may be present in the deposited particles, which contribute to the formation of bonds between the ruthenium group and the doping element 'such as 锗 (G e ). Absorption at these wavelengths increases the attenuation loss of the fiber at these wavelengths. This paper scale applies to the Chinese National Standard (CNS) A4 specification (210X 297 mm) (please read the notes on the back and fill out this page) ) F Department of Economics Intellectual Property Bureau Staff Consumer Cooperatives Printing -4- 1291940 A7 B7 V. INSTRUCTIONS (2) The object of the present invention is to provide a method for purifying a pre-sintered composition. (Please read the notes on the back first) Fill in this The subject matter of the present invention is a method of making optical quality glass comprising melting, or optionally purifying a pre-sintered composition, wherein a plasma or flame from a thermal energy supply tool is fed in a first feed conduit Sintering the composition particles, wherein a second feed conduit is optionally supplied to the plasma or flame to a fluorine or chlorine compound (preferably a fluorine compound) mixed with a carrier gas, and the feed conditions of the two conduits are adjusted or The metal or alkaline earth metal halogen contained in the pre-sintered composition particles is reacted with _ or chlorine (preferably fluorine/) or with chlorine or a chlorine compound (preferably a fluorine compound). The object of the present invention is also to apply the purification. The method of pre-sintering the composition deposits a pre-sintered composition on the fiber prototype which contains only a small amount of alkali or alkaline earth elements. The purpose of the present invention is also to provide a method for depositing a pre-sintered composition on an optical device, wherein the prototype extending in the long axis direction is set to be electrically generated from the thermal energy supply tool. Moving forward of the slurry or flame, preferably about its axis, wherein the plasma or flame is substantially reciprocating parallel to the longitudinal direction of the prototype, and wherein a first conduit imparts a pre-sintered composition particle Into the plasma or flame, wherein a second feed conduit is required to feed the plasma or flame with a fluorine or chlorine compound (preferably a compound) of the mixed carrier gas, the feed conditions of the two conduits being Adjusted to cause the alkali metal or alkaline earth metal element contained in the particles in the pre-sintered composition to react with fluorine or chlorine (relative to or wearing a gas compound (better compound compound). The optical device may be in the form of fiber, bismuth, auxiliary Instruments, rods, high temperature resistant materials, glass prototypes and/or optical lenses. This paper scale applies to Chinese National Standard (CNS) Α4 specifications (210X297 public meals) -5-1291940 A7 B7 V. INSTRUCTIONS (3) The plasma or flame is the seat where the molten pre-sintered composition chemically reacts with the fluorine or chlorine compound in the carrier gas. Advantageously, the plasma temperature can be adjusted to be supplied to the carrier. The gas and the feed rate of the conduit fed to the pre-sintered composition are highly efficient in the reaction. Higher temperatures maintain good reaction efficiency while increasing the feed rate of the feed conduit. The average particle size in the pre-sintered composition adjusts the amount of fluorine or chlorine compounds (preferably fluorine compounds) in the carrier gas. The smaller particles may be less fluorinated or chlorine-rich (preferably fluorine compounds) The carrier gas maintains good reaction efficiency. By eliminating the basic elements in the deposited layer of the pre-sintered composition, optical devices can be formed using far less expensive starting materials. Other features and advantages of the present invention can be read only by reading BRIEF DESCRIPTION OF THE DRAWINGS The illustrations illustrate the use of the present invention to melt or purify a pre-sintered composition for deposition on an optical fiber. The method of melting or purifying the pre-sintered composition can be used to deposit one or more layers of the pre-sintered composition on the optical device and contain only negligible amounts of alkali metal elements such as sodium. Or lithium, or alkaline earth metal elements. The deposition operation, also known as the accumulation operation, is used to increase the diameter of the prototype to facilitate the extraction of tens of kilometers of continuous fibers from the prototype. In the drawings, the method includes a The plasma torch 3, which includes the electric sensor assembly 5, and the prototype 1 of the drawing cylinder, extends along the long axis and rotates around its axis, as indicated by arrow 7. The paper size is applicable to the Chinese country. Standard (CNS) A4 size (2) 〇χ 297 mm) (Please read the notes on the back and fill out this page)

Printed by the Ministry of Economic Affairs, Intellectual Property Office, Staff and Consumer Cooperatives -6 - 1291940 A7 B7 V. INSTRUCTIONS (4) The torch 3 is substantially reciprocally moved parallel to the longitudinal direction L of the prototype. The prototype is rotated by a glass work lathe (not shown). The buckle of the lathe drives the two glass rods welded to the ends of the prototype. The lathe is placed in a closed box that provides protection against electromagnetic radiation and gases emitted from chemical reactions. The first feed conduit delivers the pre-sintered composition particles 1 1 to the plasma. The feed is purely preformed by gravity. A valve (not shown) is placed outside the box to adjust the feed rate. The second feed conduit 13 supplies a gas 15 to the plasma, wherein a given amount of fluorine or chlorine compound, and preferably a fluorine compound, is delivered. The carrier gas is preferably air. The fluorine compound is, for example, sulfur hexafluoride S F 6, or F r e ο η approved by European regulations, such as C 2 F 6 . The chlorine compound may be, for example, chlorine C 1 2 . A valve is attached to the gas supply outside the box to adjust the carrier gas flow rate. Another valve connected to the gas supply is used to adjust the amount of fluorine or chlorine compounds in the carrier gas. The carrier gas may consist solely of a chlorine compound, preferably a pure fluorine compound. The plasma is the chemical reaction between the pre-sintered composition particles and fluorine or chlorine, preferably the fluorine compound. The temperature of the plasma is in the range of 500 ° C to 1 〇 '0 0 ° C to promote melting of the pre-sintered composition particles. Or a chlorine compound is reacted with an alkali metal halogen such as sodium or lithium contained in the pre-sintered composition to produce a fluoride N a F or L i F, or a chloride N a C 1 or L i C 1 and is arranged in a gaseous form. Drop it. Good reaction efficiency can be obtained under the following operating conditions:

Plasma power 40kW to l〇〇kW This paper scale is applicable to China National Standard (CNS) Α4 specification (210X297 mm) (please read the note on the back and fill out this page) 印 Printed by the Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative -7- 1291940 A7 B7 V. INSTRUCTION DESCRIPTION (6) In a preferred embodiment of the present invention, pyrolysis by granulation or compaction in a known manner according to U.S. Patent No. 5 '77 6 '240 may be used. The cerium oxide is produced to produce a pre-sintered composition. The thus pressed or granulated ceria can be an oxide for the pyrolysis of the following properties: BET surface area: 1 to 500 m 2 /g; compaction: 150 to 800 g / liter; and particle size : 10 to 800 microns. In the following, ''pyrolysis of yttrium oxide> pyrolysis of cerium oxide, vv pyrolysis yttrium oxide and v pyrolytic cerium oxide expressions to understand the meaning of the system is very subdivided, Nai a rice-scale powder prepared by converting a gaseous hydrazine compound such as methyltrifluorodecane or ruthenium tetrachloride in a high temperature flame, wherein the flame is fed with hydrogen and oxygen, and water vapor can be supplied thereto as needed. . In the following, the term 'particle granules' refers to cerium oxide produced by pyrolysis which is highly compacted by a compaction procedure or the like as described in U.S. Patent No. 5,7,6,200 powder. For the process according to the invention, it is possible to produce cerium oxide by pyrolysis which is compacted into granules by the downstream compacting step described in DE 196 01 415 A1 (corresponding to US Pat. No. 5,776,240) and having the following properties: pressure Tightness: 150g / liter to 800g / liter, preferably 2 0 0 to 5000g / liter; particle size: 10 to 800 microns; and BET surface area: 10 to 50,000 square meters / gram, preferably 20 to 130 square meters / gram; or use the United States Patent No. 5,7 7 6, 2 4 to pyrolyze two paper scales applicable to China National Standard (CNS) Α 4 specifications (21〇Χ 297 mm) (Please read the notes on the back and fill out this page) Λ Ordered by the Ministry of Economic Affairs, Intellectual Property Bureau, Staff and Consumer Cooperatives Printed -9-1291940 A7 B7 V. Invention Description (7) Cerium oxide as the base And particles having the following properties: an average particle size: 25 to 120 microns; - BET surface area: 40 to 400 square meters / gram; a hole volume: 0 · 5 to 2 · 5 ml / gram; - hole distribution: no holes Having a diameter of < 5 nm, containing only mesopores and macropores; - p Η 値, : 3. 6 to 8 · 5 ; A plug density: 220 to 700 g / liter. The following pre-sintered compositions can be used in accordance with the invention: a) pyrolysis to produce a ruthenium surface area of 90 square meters per gram, a bulk density of 35 grams per liter and a plug density of 59 grams per liter.压 It is compacted into granules according to U.S. Patent No. 5,7,7,2,240. The compacted cerium oxide has a Β E T surface area of 90 m 2 /g and a plug density of 365 g / liter. b) Pyrolysis of cerium oxide having a Β ET surface area of 50 m 2 /g and a plug density of 130 g / liter is pressed into granules according to U.S. Patent No. 5,776,240. The compacted ceria has a Β E T surface area of 50 m 2 /g and a plug density of 365 g / liter. c) pyrolysis of cerium oxide having a BET surface area of 300 m 2 /g, a bulk density of 30 g / liter and a plug density of 50 g / liter according to US Patent No. 5,7 7 6,2 4 0 The number is pressed. The compacted cerium oxide has a surface area of Β E T of 300 m 2 /g and a plug density of 289 g / liter. This paper scale applies to China National Standard (CNS) A4 specification (230X297 mm) ' -10- (please read the note on the back and fill out this page). Order · Ministry of Economic Affairs Intellectual Property Bureau Staff Consumer Cooperative Printed 1291940 A7 B7 Five (8) d) pyrolysis of cerium oxide having a BET surface area of 200 m 2 /g, a bulk density of 35 g / liter and a plug density of 50 g / liter according to U.S. Patent No. 5, 7 7 6, 2 4 0 will be pressed. The compacted ceria has a B ET surface area of 200 m 2 /g and a plug density of 219 g / liter. The pre-sintered composition to be used in accordance with the present invention may be particles based on pyrogenically produced cerium oxide doped with an aerosol, the particles having the following physicochemical property data: Diameter: 10 to 150 μm BET surface area: 25 to 100 m 2 /g p Η値: 3 to 6 塡 plug density: 400 to 1200 g / liter In a preferred embodiment of the invention, the granule may have The following physicochemical properties: Average particle size: 1 5 to 30 μm BET surface area: 60 to 70 m 2 /g P Η値: 4 to 6 塡 plug density: 400 to 650 g / liter of these particles can be used The pyrogenically produced cerium oxide doped with sol is dispersed in water, the dispersion is spray dried and, as the case may be, the granules are tempered at a temperature of 150 to 1 10,000 for a period of 1 to 8 hours. The pyrogenically produced type of cerium oxide using aerosol-doped alumina may be a method in which the base component is flame-oxidized or, preferably, flame-hydrolyzed. The paper is applicable to the Chinese National Standard (CNS) A4 specification (210X297). PCT) (Please read the note on the back and fill out this page) Printed by the Ministry of Economic Affairs, Intellectual Property Bureau, Staff and Consumer Cooperatives -11 - 1291940 A7 B7 Ministry of Economic Affairs, Intellectual Property Bureau, Staff and Consumers Cooperatives Printed 5, Inventions (9) Manufacturing a type of cerium oxide and using a pyrolysis-doped alumina to produce a type of cerium oxide and wherein the doping amount of the doping component is 1 · 10 4 and up to 20% by weight, preferably the amount is a BET surface area of 1 to 10, 〇〇〇p pm and a doping component of aluminum or a mixture of aluminum compounds or metal aluminum suspensions or mixtures thereof, the BET surface area of the doped oxides is 5 Up to 600 square meters / gram, preferably 40 to 100 square meters / gram. The alumina doped ceria may have a D B P値 of less than 1 〇 gram / 1 〇 gram. The pyrogenically produced cerium oxide using aerosol-doped alumina can be pyrolyzed by a flame to be oxidized by flame oxidation or, preferably, by flame, by feeding an aerosol to a flame prior to the reaction. The aerosol is uniformly mixed with a gas mixture of flame oxidation or flame hydrolysis, and then the aerosol/gas mixture is reacted in a flame to be completely pyrolyzed from the gas stream in a known manner to separate the resulting doped alumina. a type of cerium oxide produced by using an aqueous solution containing a salt or a mixture of salts of aluminum or a metal in a dissolved or suspended form itself or a mixture thereof to produce an aerosol which is fogged by using a two-component nozzle Different aerosol manufacturing methods are utilized, preferably by aerosol generator or ultrasonic atomization. Useful salts are: A 1 C 1 3, A 1 2 (S〇4) 3, A1 (1^〇3)3. This is contained in £ 0 9 9 5 7 1 8 A 1 . For the preparation of pyrogenic cerium oxide and the preparation of cerium oxide (aluminum) (please read the back of the note and fill out this page). The paper size is applicable to the Chinese National Standard (CMS) Α 4 specifications (2) 〇Χ 29*7 )) -12- 1291940 A7 B7 V. Description of invention (j Table 1 Data related to the alumina-doped cerium oxide dispersion. Ministry of Finance, Intellectual Property Bureau, Staff Consumer Cooperative, Printed Test No. Solid Content Oxide _ [g/ l] atomizer disk speed [_ operating temperature [°C] waste air temperature [°C] spray dryer 1 150 disk 20,000 380 105 Niro SD12.5 2 150 disk 10,000 380 105 Niro SD12.5 3 150 Two-component nozzle 260 105 Anhydro Compakt 4 200 Two-component nozzle 260 105 Anhydro Compakt 5 250 Two-component nozzle 260 105 Anhydro Compakt 6 300 Two-component nozzle 260 105 Anhydro Compakt 7 350 Two-component nozzle 260 105 Anhydro Compakt 8 450 Two-component nozzle 260 105 Anhydro Compakt 9 600 Two-component nozzle 260 105 Anhydro Compakt 10 600 Two-component nozzle 380 110 Niro SD12.5 11 600 Two-component nozzle 420 106 Niro SD12. 5 12 600 Disc 20,000 380 107 Niro SD12.5 (Please read the note on the back and fill out this page) This paper size applies to the Chinese National Standard (CNS) A4 specification (210X297 mm) -14- 1291940

7 B Ministry of Economic Affairs Intellectual Property Bureau Employees Consumption Cooperative Printed 5, invention description (j Table 2 Physicochemical data of spray-dried cerium oxide of the first alumina. Test No. 塡 Plug Density Dry Reduction Combustion Reduction pH 値 Specific Surface Area d50 Ila(Cilas) [克/升] 『%1 ί%1 (BET) 〖m2/gl mm 1 527 0.3 0.2 4.7 63 18 2 536 0.6 0.3 5.7 63 24 3 455 0.8 0.3 4.8 63 19 4 504 0.5 0.5 5.5 63 21 5 532 0.5 0.5 4.5 62 26 6 536 0.3 0.5 4.8 63 22 7 559 0.4 0.6 5.1 62 25 8 550 0.9 0.2 5.0 62 23 9 601 0.3 0.5 5.1 62 21 10 603 0.4 0.5 5.7 63 18 11 618 0.3 0.6 5.1 63 24 12 578 0.2 0.5 5.9 65 23 (Please read the notes on the back and fill out this page), τ Γ

This paper scale applies to China National Standard (CNS) A4 specification (210X297 mm) -15- 1291940 7 Β Table 3 Physicochemical data of titanium dioxide P 2 5 Titanium dioxide P25 CAS no. 13463-67-7 Water behavior hydrophilic appearance loose white Powder BET surface area "mVg 50± 15 Average size of the original particles Nano 21 Pressure tightness 2) Gram / liter of about 100 Swollen 10) Gram / liter of about 3.7 Dry reduction 3) Departure from the supplier (l〇5°C2 Hour) <1.5 Combustion loss 4) (l〇〇〇 °C2 hours) <2 pH5) in 4% aqueous dispersion) 3-4 Si〇28) <0.2 Al2〇38) <0.3 Fe2038) <0.01 Ti028) >99.5 Ζγ〇28) HfD28) • HC19) <0.3 sieve residue 6) (Mockei*5s method, 45 μm) <0.05 (Please read the back note and fill out this page) • —I. Γ Printed by the Intellectual Property Office of the Intellectual Property Office of the Ministry of Economic Affairs " according to DIN 6613 1 2) according to DIN ISO 787/XI, JISK 5101/18 (unscreened) 3) according to DIN ISO 787/11, ASTM D 280 , JIS K 5101/21 4) according to DIN 5592 1, ASTM D 1208, JIS K 5101/23 5) according to DIN ISO 787/ΙΧ, ASTM D 1 208, JIS Κ 5 101/24 6) According to DIN ISO 787/XVIII; JIS K 5101/20 7) Relative to the material dried at 105 °C for 2 hours 8) Relative to the material burning at 1000 t for 2 hours 9) HC1 content is the component of combustion reduction 1()) Determination of λ using air comparison density bottle This paper scale applies to China National Standard (CNS) A4 specification (210X297 mm) -17- Ministry of Economic Affairs Intellectual Property Office Staff Consumer Cooperative Printed 1291940 A7 __B7__ V. Invention Description (β The titanium dioxide is prepared by spraying a volatile titanium compound into an oxyhydrogen flame formed by hydrogen gas and air. In most cases, titanium tetrachloride is used. This material is produced in a hydrogen-oxygen gas reaction. Hydrolyzed by water to obtain titanium dioxide and hydrochloric acid. After leaving the flame, the titanium dioxide enters a so-called condensation zone where the titanium dioxide primary particles and the original aggregates are cohesive. This stage is presented as an aerosol type product in the cyclone. It is separated from the gaseous accompanying material and post-treated with moist hot air. The particle size of titanium dioxide can be varied by changing the reaction conditions, for example, flame temperature, hydrogen to oxygen ratio, titanium tetrachloride usage, residence time in the flame, and length of the condensation zone. The pyrogenic titanium dioxide was dispersed in fully deionized water according to ΕΡ 1 078 883 Α1. Use a dispersing device that operates on the rotor/stator principle. The resulting dispersion was spray dried. The final product is deposited using a filter or cyclone. This paper scale applies to the Chinese National Standard (CNS) Α4 specification (210Χ297 mm) (please read the notes on the back and fill out this page)

-18- 1291940 V. INSTRUCTIONS (y) Table 4 Data of the Ministry of Economic Affairs Intellectual Property Office Staff Consumer Cooperative Printed and Spray-dried T i〇2 P 2 5 Water Dispersion Example H20 Quantity [kg] Ti〇2 P25 Amount [kg] Atomizer physical disk speed [rpm] Operation? Μ [°C] Discharge air brewing [°C] Deposition 1 10 1.5 Disc 35,000 345 100 Cyclone 2 10 1.5 Disc 45,000 370 105 Cyclone 3 10 1.5 Disc 20,000 350 95 Cyclone 4 10 2.5 Disc 15,000 348 100 Cyclone 5 100 15 Two-fluid 445 130 Filter 6 100 15 Disc 10,000 450 105 Filter 7 10 2.5 Disc 20,000 348 105 Cyclone 8 10 1.5 Disc 15,000 348 105 Cyclone 9 10 2.5 Disc 35,000 300 105 Cyclone (please read the notes on the back and fill out this page) This paper size applies to the Chinese National Standard (CNS) A4 specification (210X 297 mm) -19 - 1291940

7 B Ministry of Economic Affairs Intellectual Property Bureau Staff Consumer Cooperative Printed 5, Invention Description (^ Table 5 Physicochemical data of spray-dried T i〇2 P 2 5 dispersion Example BET surface area rm2/gl Compaction [g/L] pH D50値(Cilas) Drying reduction m Combustion reduction [%1 1 51 641 3.9 14.6 0.9 0.9 2 50 412 3.7 10.6 0.8 1.0 3 52 680 3.5 25.0 0.8 1.0 4 51 710 3.7 43.6 0.8 1.2 5 52 660 4.0 17.1 0.9 0.9 6 53 702 3.9 27.5 0.9 0.9 7 50 708 3.5 26.7 1.1 0.6 8 53 696 3.9 30.1 1.0 0.9 9 49 640 3.7 16.0 0.7 0.8 (Please read the notes on the back and fill out this page) i€., τ Γ This paper size applies. China National Standard (CNS) A4 specification (21 OX 297 mm) -20- 1291940 A7 B7 V. Description of invention (Y can use a spray-type atomizer or a nozzle-type atomizer, such as a single-substance nozzle or gas Atomizing nozzles. The tempering of the granules can be carried out in a fixed bed, for example in a chamber furnace, and in a fluid bed, such as a rotary dryer. Example 1 3 0.25 kg / hr previously volatilized Aluminum chloride (A 1 C 13) and 1 〇〇Nm3/hr The hydrogen gas is combined with 45 ONm3 / hr of air in a burner of known design and construction. After the flame reaction, the fine-grained high surface area alumina is separated from the accompanying hydrochloric acid gas in the filter or in the cyclone. Then, it is treated with a humid air at a high tray to remove any trace of any self-adhesive HC 1. The resulting high surface area pyrogenic alumina has the physicochemical properties listed in Table 6. For comparison purposes, the market will also be available. The relevant data for the pyrolyzed alumina (trade name Alumina C) available from Degussa-HiilS AG/Frankfim are listed in Table 7. (Please read the notes on the back and fill out this page.) Bureau employee consumption cooperative printed on this paper scale applicable to China National Standard (CNS) Α4 specification (210X297 mm) -22- 1291940 A7 B7 V. Invention description (2 (^ Table 6 unit high surface area alumina Alu 130 alumina C BET Specific surface area, stroke meter / gram [m2 / g] 121 100 Sems 値 (pH 4 to 9) Ml / 2g 9.38 7.05 PH 4% aqueous dispersion 4.93 4.5 Dry weight loss % 3.3 3.0 Bulk density gram / liter 55 48 Compact bulk Density克/升 63 57 DBP absorption 値 % by weight Unmeasurable; no end point Can be determined 231 (Please read the note on the back and fill out this page) Printed by the Intellectual Property Intelligence Bureau Staff Consumer Cooperative DBP: Dibutyl phthalate

Sears® measurement system EP 0 717 088 〇 Example 2 Alumina having the following physicochemical properties was used as a pyrogenically produced alumina, and its system was carried on the pigment data sheet η 〇 · 5 6 ”Highly

Dispersed Metal Oxides According to the Aerosil Process 5, 4th Edition, February 1 989, among Degussa AG (Table 7). This paper scale applies to the Chinese National Standard (CNS) A4 specification (210X 297 mm) -23- 1291940

B V. Description of invention (g Table 7 Alumina c CAS no. 1344-28-1 BET surface area 1:) m2/g 100± 15 Average size of the original particles Nano 13 Compressed bulk density 2) gram / liter of about 80 Specific gravity 1 ()) g / l about 3.2 dry reduction 3) from the supplier factory leaving (l 〇 5 ° C 2 hours) < 5 annealing reduction 4) 7) (l 〇〇〇 ° C 2 hours) <3 pH5 ) (in 4% aqueous dispersion) 45-5.5 Si028) <0.1 ai2o38) <99.6 Fe2038) <0.2 Ti028) >0.1 Zr028) Hf028) HC18)9) <0.5 sieve residue 'Mocker's method, 45 microns) <005 (Please read the note on the back and fill out this page) Printed by the Ministry of Economic Affairs, Intellectual Property Bureau, Staff Cooperatives " according to DIN 66131 2) According to DIN ISO 787/XI, JIS K 5101/18 ( Unscreened) 3) according to DIN ISO 787/11, ASTM D 280, JIS K 5101/21 4) according to DIN 5592 1, ASTM D 1208, JIS K 5101/23 5) according to DIN ISO 787/ΙΧ, ASTM D 1208, JIS Κ 5101/24 〇 according to DIN ISO 787/XVIII; JIS K 5101/20 7) Relative to the substance dried at 105 °C for 2 hours 8) Relative to the HC1 content at 1 TC (TC 2 hours of substance 9) Annealing Part of the reduction 1 ()) using the air comparison pycnometer to determine the paper size applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) -24· 1291940 A7 B7 V. Invention Description (j When manufacturing alumina, The volatile aluminum compound is injected through a nozzle into an oxyhydrogen flame composed of hydrogen and air. In most cases, aluminum trichloride is used. This substance is hydrolyzed to form an oxidation under the influence of moisture generated in the hydrogen-oxygen reaction. Aluminium and hydrochloric acid. After leaving the flame, the alumina enters a so-called condensation zone where the alumina precursor particles and the original alumina aggregates will coagulate. In this stage, the product in the form of an aerosol is in the cyclone. Internally separated from the accompanying gaseous material and then post-treated with moist heat. The alumina particle size can be varied using reaction conditions such as flame temperature, hydrogen to oxygen ratio, amount of aluminum trichloride, residence time in fire, or Length of the coagulation zone. The manufacture of the particles of the invention disperses the pyrogenically produced alumina in fully deionized water. A dispersing device operating according to the ion/stator principle is used. The resulting dispersion was spray dried. Use a filter or cyclone to separate the finished product. The tempering of the spray particles can be carried out in a scum furnace. Table 8 lists the manufacturing conditions. Table 9 lists the data related to the obtained products (please read the notes on the back and fill out this page)

Printed by the Intellectual Property Office of the Ministry of Economic Affairs, the Consumer Cooperatives. This paper scale applies to the Chinese National Standard (CNS) A4 specification (210X 297 mm) -25-1291940

AB V. Description of invention (g Table 8 Data relating to spray drying of A 1 2 0 3 water dispersion sprayed by the Ministry of Economy, Intellectual Property Bureau, employee consumption cooperatives, printing example H20 quantity [kg] ai2o3 quantity [kg] atomizer materialization tray Rotation speed [rpm] Operating temperature [°C] Waste air temperature [°C] Spray dryer 1 100 15 Single substance nozzle 420 105 Niro SD 12.5 2 100 10 Single substance nozzle 412 102 Niro SD 12.5 3 5 0.75 Disc type 15000 298 1058 Niro Minor 4 16.5 2.50 Disc 25000 300 107 Niro Minor 5 20 3.0 Disc 35000 300 105 Niro Minor 6 8 1.2 Disc 20000 298 106 Niro Minor 7 600 90 Disc 10000 437 100 Niro SD 12.5 8 300 45 Disc 20000 458 100 Niro SD 12.5 9 50 7.5 Gas atomizing nozzle 260 105 Anhydro Compakt 10 300 45 Gas atomizing nozzle 458 108 Niro SD 12.5 11 200 30 Gas atomizing nozzle 457 100 Niro SD 12.5 12 4.25 0.75 Gas atomizing nozzle 380 105 Niro Minor (please read the notes on the back and fill out this page) This paper size applies to the Chinese National Standard (CNS) A4 specification (210X297 mm) -26- 1291940 Ministry of Economics Production Bureau Staff Consumer Cooperatives Printed A7 B7 V. Invention Description (d Table 9 Physical and Chemical Data of Spray-Dry Alumina Test No. Plug Density Dry Reduced Combustion Reduction pH値d50 値(Cilas) [g/L] 『%1 F %1 [μm] 1 505 2.3 2.3 5.0 39.4 2 502 1.8 2.0 4.9 40.9 3 473 1.4 2.7 4.9 31.1 4 471 1.5 2.4 5.1 20.5 5 466 1.5 2.6 5.0 14.5 6 477 1.5 1.5 5.4 27.7 7 525 1.6 1.9 5.0 39.3 8 474 1.5 2.8 4.8 27.6 9 506 3.4 2,1 5.0 28.0 10 533 1.9 2.5 5.0 30.6 11 516 1.8 2.5 4.7 25.8 12 483 1.7 2.6 4.9 8.8 (Please read the notes on the back and fill out this page) This paper scale applies to Chinese national standards ( CNS ) A4 size (210X297 mm) -27-

Claims (1)

I29T940 j♦ this A8 B8 C8 D8 VI. Application for Patent Scope Annex 4A: Patent Application No. 91 i 1 7046 Replacement of Chinese Patent Application (Please read the first note on the back of the page) 1 · A method of manufacturing optical quality glass, including Melting or optionally purifying a pre-sintered composition, wherein the pre-sintered composition is a metal oxide or metalloid oxide particle which is spray dried by dispersing a metal oxide or metalloid oxide in water and yielding The granules are prepared at a temperature of from 150 to 1 '10 ° C for a period of from 1 to 8 hours, wherein the first feed conduit is used to feed the pre-sintered composition into the plasma or flame from the thermal energy supply means. a granule, and wherein a fluorine or chlorine compound mixed with a carrier gas is optionally fed to the plasma or flame by a second feed conduit, the feed conditions of the two conduits being adjusted to enable the pre-sintered composition The alkali metal or alkaline earth metal element contained is reacted with fluorine or chlorine of the fluorine or chlorine compound. Ministry of Economic Affairs, Intellectual Property Office, Staff Consumer Cooperative, Printed 2 - A method of depositing a pre-sintered composition on an optical device, wherein a prototype extending along the long axis direction is set to be a plasma from a thermal energy supply tool or The flame is actuated about its axis and the plasma or flame is substantially reciprocating parallel to the long axis of the prototype, wherein the pre-sinter composition is a metal oxide or metalloid oxide particle that oxidizes the metal The metal or metalloid oxide is dispersed in water, spray dried, and the resulting particles are prepared at a temperature of 150 to 1,100 ° C for 1 to 8 hours, and the first feed is used therein. The conduit feeds the plasma or flame into the pre-sintered composition particles, and wherein the plasma or flame is fed with a fluorine or chlorine compound mixed with the carrier gas, as needed, using the second feed conduit, the paper dimensions of the two conduits Applicable to China National Standard (CNS) A4 Specification (210X297 mm) 8 888 ABCD Ministry of Economic Affairs Intellectual Property Bureau Staff Consumer Cooperative Printed 1291940 VI. Patent Application Scope 2 Feeding conditions are adjusted Such that the particulate composition is pre-sintered as alkali metal or alkaline earth metal element to react with the fluorine or chlorine of the fluorine or chlorine compound. This paper scale applies to China National Standard (CNS) A4 specification (210X297 mm) -2-