CN112341006A - Method and device for high-purity quartz tube/rod, quartz tube/rod and application - Google Patents

Method and device for high-purity quartz tube/rod, quartz tube/rod and application Download PDF

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Publication number
CN112341006A
CN112341006A CN202011091901.8A CN202011091901A CN112341006A CN 112341006 A CN112341006 A CN 112341006A CN 202011091901 A CN202011091901 A CN 202011091901A CN 112341006 A CN112341006 A CN 112341006A
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glass tube
rod
quartz glass
heating
tube
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CN202011091901.8A
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CN112341006B (en
Inventor
陈士斌
厉广强
王东超
刘守科
徐新奎
钱卫刚
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JIANGSU PACIFIC QUARTZ CO Ltd
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JIANGSU PACIFIC QUARTZ CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/007Other surface treatment of glass not in the form of fibres or filaments by thermal treatment
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B23/00Re-forming shaped glass
    • C03B23/04Re-forming tubes or rods
    • C03B23/043Heating devices specially adapted for re-forming tubes or rods in general, e.g. burners
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B23/00Re-forming shaped glass
    • C03B23/04Re-forming tubes or rods
    • C03B23/045Tools or apparatus specially adapted for re-forming tubes or rods in general, e.g. glass lathes, chucks
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B23/00Re-forming shaped glass
    • C03B23/04Re-forming tubes or rods
    • C03B23/053Re-forming tubes or rods by centrifuging
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00Type of glass produced
    • C03B2201/02Pure silica glass, e.g. pure fused quartz
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00Type of glass produced
    • C03B2201/02Pure silica glass, e.g. pure fused quartz
    • C03B2201/03Impurity concentration specified

Abstract

The invention provides a method and a device for high-purity quartz tube/rod, a quartz tube/rod and application thereof, which are characterized by comprising the following steps: a high-purification step of heating the quartz glass tube/rod while generating a continuous stable arc outside the quartz glass tube/rod to move alkali metal ions contained in the quartz glass tube/rod toward an outer wall of the quartz glass tube/rod. The technical scheme disclosed by the invention not only improves the purity of the quartz glass tube/rod, but also improves the generation efficiency, and simultaneously has simple requirements on equipment, thereby greatly saving the engineering cost.

Description

Method and device for high-purity quartz tube/rod, quartz tube/rod and application
Technical Field
Embodiments of the present disclosure relate generally to the field of quartz glass production, and more particularly, to methods, apparatus, quartz tubes/rods and uses for high purity quartz tubes/rods.
Background
The high-purity quartz material is an indispensable carrier material in the field due to special physical properties such as temperature resistance, acid resistance, low expansion, light permeability and the like. The fused silica tube can be widely applied to batch-type firing furnaces as a high-purity reaction chamber, a gas/liquid inlet or a conveying pipeline. Diffusion tubes, bell jars, etc. made of quartz materials are used throughout critical processes of semiconductor processing such as diffusion, oxidation, deposition, etching, etc. The semiconductor industry has stringent requirements for the alkali metal content of the carrier material.
In the semiconductor industry, there is a need to produce large quartz tubes by a tube expansion process, which at present is generally to first take an intermediate quartz tube having an intermediate tube thickness and an intermediate outer diameter and subsequently cool it, and wherein in a second shaping step at least one length of the cooled intermediate quartz tube is supplied to a heating zone, heated zone by zone to a softening temperature and shaped while rotating around its longitudinal axis into a large quartz tube having a final tube thickness and a final outer diameter.
Because alkali metal ions can move from a high-temperature area to a low-temperature area, the content of the alkali metal ions on the inner wall of the large quartz tube can be increased by the conventional tube expanding process, and the requirement of the conductor industry on the content of the alkali metal in a carrier material cannot be met.
In the prior art, the inner wall and the outer wall of a quartz glass tube are respectively provided with a direct current electrode for high purity, but the method has the defects of complex structure, low efficiency, high energy consumption, direct contact between the electrodes and the glass tube, generation of the electrodes in the purification process of the glass tube and easy generation of defects on the surface of the glass tube.
Disclosure of Invention
According to an embodiment of the present disclosure, there is provided a method of high-purifyingquartz glass tube/rod, including: a high-purification step of heating the quartz glass tube/rod while generating a continuous stable arc outside the quartz glass tube/rod to move alkali metal ions contained in the quartz glass tube/rod toward an outer wall of the quartz glass tube/rod.
Further, the heating of the quartz glass tube/rod is a uniform distribution of one or more heating sources around the circumference of the quartz glass tube/rod, the heating sources being plasma torches, oxyhydrogen flame torches, or lasers; the quartz glass tube/rod is heated at a temperature of 1700 ℃ to 1900 ℃.
In the above aspect and any possible implementation, the continuous stable arc is an alternating arc generated by providing a pair of electrodes on the outside of the quartz glass tube/rod, and applying an alternating voltage of 50-200kv and a current of 80-200mA to the electrodes.
As in the above-described aspects and any possible implementation, the pair of electrodes are arranged on the same cross section or on different cross sections of the quartz glass tube/rod.
As with the above-described aspects and any possible implementation, the arc is not in contact with the outer surface of the quartz glass tube/rod, as are the electrodes.
The aspect and any possible implementation described above, wherein the quartz glass tube/rod is rotated with its mandrel as a rotation axis at a rotation speed of 30-70 r/min; the electrode and the torch are horizontally moved outside the quartz glass tube/rod in a direction parallel to the axial direction of the quartz glass tube/rod at a horizontal moving speed of 40 to 100 mm/min.
As for the aspect described above and any possible implementation manner, the method for high-purifying a quartz glass tube further includes, after the high-purifying step: expanding the tube at 1700-1900 deg.c and at 80-200r/min and the horizontal moving speed of the blast burner 40-100 mm/min.
As for the above-described aspect and any possible implementation manner, the method for purifying a quartz glass tube further includes, before the step of purifying, the steps of: expanding the tube at 1700-1900 deg.c and at 80-200r/min and the horizontal moving speed of the blast burner 40-100 mm/min.
In a second aspect of the present disclosure, there is provided a high-purity silica glass tube/rod produced by the above method, characterized in that the content of lithium ions in the inner wall surface layer is 0.5ppm or less; the lithium ion content of the bulk impurity is 0.1ppm or less.
In a third aspect of the present disclosure, there is provided an application of the above quartz glass tube/rod in the fields of optical fiber, semiconductor and photovoltaic.
In a fourth aspect of the present disclosure, there is provided a high-purity processing apparatus for a quartz glass tube/rod, comprising a base station, a fixing mechanism, a heating mechanism, a shaping mechanism, an ionizing mechanism and a controller; wherein the content of the first and second substances,
the two groups of fixing mechanisms are arranged on the top surface of the base station and are used for installing and fixing the quartz glass tubes/rods and driving the quartz glass tubes/rods to rotate by taking the axis of the quartz glass tubes/rods as a shaft;
the heating mechanism is arranged on the top surface of the base station, is positioned between the two groups of fixing mechanisms and is used for heating the quartz glass tube/rod, and the heating mechanism can move along the axial direction of the quartz glass tube/rod;
the shaping mechanism is fixedly arranged on the heating mechanism and is used for shaping the part of the quartz glass tube/rod which expands outwards under the action of centrifugal force after being heated;
the ionization mechanism is fixedly arranged on the heating mechanism and generates an alternating current arc in the radial direction of the quartz glass tube/rod;
the controller is arranged on the side face of the base station, and the fixing mechanism, the heating mechanism, the molding mechanism and the ionization mechanism are all electrically connected with the controller.
Further, fixed establishment including fixed set up in the brace table of base station top surface, the fixed electric bearing that is provided with of top surface of brace table, the fixed solid fixed ring that is provided with on electric bearing's the interior anchor ring, evenly imbed along the hoop in the solid fixed ring and be provided with the flexible driver part of being no less than 2, flexible driver part's flexible end stretch to gu fixed ring's center sets up, the curved fixed plate of tip fixedly connected with of flexible end, the fixed plate is kept away from be provided with the skid resistant course on the face of flexible end.
Further, the heating mechanism comprises a track groove arranged on the top surface of the base station and located between the two sets of fixing mechanisms, the track groove is arranged along the axial direction of the quartz glass tube/rod, a moving block is arranged above the track groove, a driving part embedded into the track groove is arranged on the bottom surface of the moving block, mounting plates are symmetrically arranged on the two sides of the moving plate, the mounting plates are close to the quartz glass tube/rod, heating sources are arranged on the plate surfaces of the mounting plates, and the heating sources are arranged at the same height as the quartz glass tube/rod.
Further, the heating source is a plasma torch, a oxyhydrogen flame torch, or a laser.
Further, the shaping mechanism comprises a pipe expanding supporting wheel which can move along the direction close to or far away from the quartz glass tube, and the pipe expanding supporting wheel is coaxially and axially arranged below the quartz glass tube.
Further, the pipe expanding riding wheel is a graphite wheel.
Furthermore, the ionization mechanism comprises an alternating current power supply, and a first electrode and a second electrode which are electrically connected with the alternating current power supply, wherein the first electrode and the second electrode are respectively and fixedly arranged on the heating mechanism and symmetrically distributed on two sides of the quartz glass tube/rod and are arranged close to the quartz glass tube/rod.
It should be understood that the statements herein reciting aspects are not intended to limit the critical or essential features of the embodiments of the present disclosure, nor are they intended to limit the scope of the present disclosure. Other features of the present disclosure will become apparent from the following description.
Drawings
The above and other features, advantages and aspects of various embodiments of the present disclosure will become more apparent by referring to the following detailed description when taken in conjunction with the accompanying drawings. In the drawings, like or similar reference characters designate like or similar elements, and wherein:
FIG. 1 is a schematic view showing the construction of a high-purity processing apparatus for a silica glass tube/rod;
FIG. 2 shows a schematic side view of the securing mechanism;
FIG. 3 is a schematic sectional view of the heating mechanism;
FIG. 4 is a schematic side view of the heating mechanism;
fig. 5 shows a schematic structural view of the molding mechanism.
Reference numbers in the figures: 11. quartz glass tubes/rods; 12. a base station; 13. a fixing mechanism; 14. a heating mechanism; 15. a molding mechanism; 16. an ionization mechanism; 17. a controller; wherein the content of the first and second substances,
31. a support table; 32. an electric bearing; 33. a fixing ring; 34. a telescopic driving member; 35. a telescopic end; 36. a fixing plate;
41. a track groove; 42. a moving block; 43. a drive member; 44. mounting a plate; 45. a heating source;
51. molding a cylinder; 52. molding a piston rod; 53. a mounting frame; 54. a pipe expanding riding wheel.
61. A first electrode; 62. a second electrode.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present disclosure more clear, the technical solutions of the embodiments of the present disclosure will be described clearly and completely with reference to the drawings in the embodiments of the present disclosure, and it is obvious that the described embodiments are some, but not all embodiments of the present disclosure. All other embodiments, which can be derived by a person skilled in the art from the embodiments disclosed herein without making any creative effort, shall fall within the protection scope of the present disclosure.
In addition, the term "and/or" herein is only one kind of association relationship describing an associated object, and means that there may be three kinds of relationships, for example, a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
In the present disclosure, a quartz glass tube/rod is heated while a continuous stable arc is generated outside the quartz glass tube/rod, so that alkali metal ions contained in the quartz glass tube/rod move to the outer wall of the quartz glass tube/rod. Thereby reducing the alkali metal ions on the inner wall of the quartz tube, and having higher efficiency and better effect compared with direct current.
In an embodiment of the method for increasing the purity of a silica glass tube/rod of the present disclosure, an alternating voltage is applied to the silica glass tube/rod in a radial direction from a pair of electrodes on the outer side of the silica glass tube/rod to generate an alternating current arc, and alkali metal ions in the silica glass tube/rod are moved to the outer wall of the silica glass tube/rod.
In some embodiments, the quartz glass tube/rod is heated by uniformly distributing one or more heating sources around the circumference of the quartz glass tube/rod, the heating sources being plasma torches, oxyhydrogen flame torches, or lasers; the quartz glass tube/rod is heated at a temperature of 1700 ℃ to 1900 ℃.
In some embodiments, the two heating sources are horizontally and symmetrically arranged on two sides of the quartz glass tube/rod, and the heating sources are arranged on an extension line of the cross-sectional diameter of the quartz glass tube/rod.
In some embodiments, the electrodes are respectively arranged at positions close to the heating source, the two electrodes and the heating source are on the same cross section of the quartz glass tube/rod, and an angle formed by a connecting line of the two electrodes and the circle center of the cross section of the quartz glass tube/rod is less than 180 degrees.
Neither electrode is in contact with the quartz glass tube/rod.
In some embodiments, the power supply operates to ionize air between the two electrodes to produce an arc discharge while heating the quartz glass tube/rod at a temperature of 1700 ℃ to 1900 ℃. When the air is ionized, the ionization will occur along the minimum path of the two electrodes, i.e. the arc will form a side enclosure of the glass tube that is less than a semicircle.
In some embodiments, the power supply means provides an alternating current power supply, for example with its live wire connected to one of the electrodes and its neutral wire connected to the other electrode; the reverse is also possible. The material of the electrode may be tungsten wire/rod to prevent impurities from intruding into the glass tube from the electrode.
In some embodiments, the power supply input is alternating current, and the voltage is 380V; the output is alternating current, the voltage is 50-200kv, and the current is 10-200 mA. The power supply device raises 380V voltage to 200KV maximum voltage and 200mA maximum current through the high-voltage transmitting device by the control units such as rectification filtering, voltage regulation, an inversion loop and the like; the method comprises the steps that a constant current principle is adopted, the highest 200kV high voltage is instantly generated when a power supply works, air between electrodes is ionized, and then electric arcs are generated; the voltage value is pulled down to control the current value within the set value range, and the arc is stably discharged under the stable constant current state.
In some embodiments, the rectifying and filtering unit is used for outputting 540V direct current through rectifying and filtering input 380V alternating current; the DC-DC voltage regulating unit is used for carrying out DC-DC voltage regulation on the 540V direct current output by the rectifying and filtering unit and outputting adjustable 540V direct current; the DC-AC inversion module is used for inverting the 540V direct current into low-voltage alternating current with the alternating frequency of about 2 kHz; the transformer is used for converting low-voltage alternating current into high-voltage direct current with the maximum voltage of 200 kilovolts (50-200kv) and outputting the high-voltage direct current. The 200kv high voltage dc ionizes the air between the two electrodes, creating an arc discharge. By the heated flow of the conductive gas, the contaminating alkali metal ions in the glass tube can be purified without bringing the two electrodes into contact with the glass tube.
The control unit is used for controlling the DC-DC voltage regulating unit and the DC-AC inversion module according to the voltage and current parameters output by the transformer and simultaneously realizing overcurrent protection and arc discharge delay protection. In some embodiments, after the arc is generated, the voltage value is pulled down, the current loop works to control the current value within a set value range, and the arc can be stably discharged under a stable constant current state. Wherein, the voltage is controlled at 50-200 kilovolts, and the current is controlled at 80-200 mA. The arc is essentially a discharge phenomenon of gas between two electrodes under the action of a strong electric field, and is high-temperature plasma, and the plasma is an ionized gas-like substance consisting of atoms after part of electrons are deprived and positive and negative ions generated after the atoms are ionized. Charged particles in the plasma gas move directionally between the electrodes under the action of the electric field. The power supply continuously supplies electric energy, and new charged particles are continuously supplemented to form continuous and stable electric arcs.
In some embodiments, the alternating current is denoted by i, the instantaneous value of which varies with time t, crosses zero twice per cycle, the arc self-extinguishes when the dynamic alternating arc current i is 0, and then reignites.
In some embodiments, since the glass tube is heated by the heating source, the temperature rises, and thereby the diffusion coefficient of the impurity alkali metal ions contained in the glass tube rises, it becomes easy to move in a direction in which the voltage gradient is negative.
In some embodiments, by the rotation of the glass tube, a voltage can be applied throughout the entire range of the glass tube, effectively promoting the movement of the impurity alkali metal ions, and at the same time, the impurity alkali metal ions can be segregated over a large range of the outer peripheral surface of the glass tube. Accordingly, the impurity alkali metal ions can be segregated in a shallow region in the vicinity of the outer peripheral surface of the glass tube, and the region of high purity in the glass tube can be effectively enlarged.
In some embodiments, both electrodes are moved simultaneously at a speed of 40-100mm/min in the radial direction of the glass tube, and the arc generated by the electrodes also purifies the glass tube in the radial direction.
In some embodiments, after the ionization step, the outer peripheral surface of the glass tube may be subjected to a surface removal operation to remove a region of a predetermined depth, for example, 2mm, so that the impurity alkali metal ions segregated on the outer peripheral surface side of the glass tube can be removed, and a glass tube in which only a portion having been highly purified remains can be obtained. The surface removal operation may be a grinding process, a chemical etching process, or a flame grinding process, among others.
The effects of the present application will be described below by way of specific examples and comparative examples.
Example 1
Firstly, carrying out a high-purity step, heating a quartz glass tube, wherein a heating source is a oxyhydrogen flame burner, the heating temperature is 1900 ℃, the quartz glass tube rotates by taking a mandrel of the quartz glass tube as a rotating shaft, and the rotating speed is 45 r/min; continuous and stable electric arcs are generated outside the quartz glass tube through the two electrodes, alternating current electric arcs generated by alternating voltage is applied to the electrodes, the alternating voltage is 180 kilovolt, the current is 120mA, the electrodes and the blast burner horizontally move in the direction parallel to the axial direction of the quartz glass tube at the outer side of the quartz glass tube, the horizontal moving speed is 60mm/min, and alkali metal ions contained in the quartz glass tube move to the outer wall of the quartz glass tube.
After the high-purity step, the tube expansion is carried out, the tube expansion temperature is 1860 ℃, the rotating speed is 130r/min, and the horizontal moving speed of the blast burner is 60 mm/min.
Comparative example 1
Otherwise, as in example 1, the purification step was replaced by heating a quartz glass tube at a temperature of 1350 ℃ by a oxyhydrogen flame burner at a rotation speed of 45r/min with its mandrel as a rotation shaft; an electrode is arranged on the inner wall of the quartz glass tube, a click is oppositely arranged on the outer wall, the two electrodes are electrified with direct current, the applied voltage is 40KV, the electrode and the blast lamp horizontally move in the direction parallel to the axial direction of the quartz glass tube on the outer side of the quartz glass tube, the horizontal moving speed is 60mm/min, and alkali metal ions contained in the quartz glass tube move to the outer wall of the quartz glass tube.
Example 2
Firstly, a tube expanding step is carried out, wherein the tube expanding temperature is 1800 ℃, the rotating speed is 85r/min, and the horizontal moving speed of a blast lamp is 50 mm/min.
A high purification step after tube expansion, wherein a quartz glass tube is heated by a oxyhydrogen flame burner at the heating temperature of 1880 ℃, and the quartz glass tube rotates by taking a mandrel thereof as a rotating shaft at the rotating speed of 45 r/min; a continuous and stable arc is generated outside the quartz glass tube through two electrodes, an alternating current arc generated by applying an alternating voltage to the electrodes is 150 kilovolts, the current is 100mA, the electrodes and the blast burner horizontally move in the direction parallel to the axial direction of the quartz glass tube at the outer side of the quartz glass tube, the horizontal moving speed is 80mm/min, and alkali metal ions contained in the quartz glass tube move to the outer wall of the quartz glass tube.
Comparative example 2 otherwise the same as in example 2, the purification step was replaced with heating a quartz glass tube at 1460 ℃ with a mandrel as a rotating shaft and at 45r/min by using a oxyhydrogen flame burner as a heating source; an electrode is arranged on the inner wall of the quartz glass tube, a click is oppositely arranged on the outer wall, the two electrodes are electrified with direct current, the applied voltage is 50KV, the electrode and the blast lamp horizontally move in the direction parallel to the axial direction of the quartz glass tube on the outer side of the quartz glass tube, the horizontal moving speed is 60mm/min, and alkali metal ions contained in the quartz glass tube move to the outer wall of the quartz glass tube.
Example 3
Firstly, carrying out a high-purity step, heating a quartz glass tube, wherein a heating source is a oxyhydrogen flame burner, the heating temperature is 1880 ℃, the quartz glass tube rotates by taking a mandrel thereof as a rotating shaft, and the rotating speed is 55 r/min; a continuous and stable arc is generated outside the quartz glass tube through two electrodes, an alternating current arc generated by applying an alternating voltage to the electrodes is 180 kilovolts, the current is 160mA, the electrodes and the blast burner horizontally move in the direction parallel to the axial direction of the quartz glass tube at the outer side of the quartz glass tube, the horizontal moving speed is 85mm/min, and alkali metal ions contained in the quartz glass tube move to the outer wall of the quartz glass tube/rod.
Then, the tube expansion is carried out, the tube expansion temperature is 1790 ℃, the rotating speed is 145r/min, and the horizontal moving speed of the blast burner is 60 mm/min.
Carrying out a high-purity step again after pipe expansion, heating the quartz glass pipe by using a oxyhydrogen flame burner at the heating temperature of 1880 ℃, and rotating the quartz glass pipe by using a mandrel of the quartz glass pipe as a rotating shaft at the rotating speed of 55 r/min; continuous and stable electric arcs are generated outside the quartz glass tube through the two electrodes, alternating current electric arcs generated by alternating voltage is applied to the electrodes, the alternating voltage is 180 kilovolt, the current is 160mA, the electrodes and the blast burner horizontally move in the direction parallel to the axial direction of the quartz glass tube at the outer side of the quartz glass tube, the horizontal moving speed is 85mm/min, and alkali metal ions contained in the quartz glass tube move to the outer wall of the quartz glass tube.
Comparative example 3 otherwise the same as in example 3, the purification step was replaced with heating a quartz glass tube at 1460 ℃ with a mandrel as a rotating shaft and at 45r/min by using a oxyhydrogen flame burner as a heating source; an electrode is arranged on the inner wall of the quartz glass tube, a click is oppositely arranged on the outer wall, the two electrodes are electrified with direct current, the applied voltage is 50KV, the electrode and the blast lamp horizontally move in the direction parallel to the axial direction of the quartz glass tube on the outer side of the quartz glass tube, the horizontal moving speed is 60mm/min, and alkali metal ions contained in the quartz glass tube move to the outer wall of the quartz glass tube.
Example 4
Performing a high-purity step, heating a quartz glass rod, wherein a heating source is a oxyhydrogen flame burner, the heating temperature is 1800 ℃, the quartz glass rod rotates by taking a mandrel of the quartz glass rod as a rotating shaft, and the rotating speed is 45 r/min; a continuous stable arc is generated outside the quartz glass rod through two electrodes, an alternating current arc generated by applying an alternating voltage to the electrodes is 180 kilovolts, the current is 120mA, the electrodes and the torch move horizontally in the direction parallel to the axial direction of the quartz glass rod at the outer side of the quartz glass rod, the horizontal moving speed is 60mm/min, and alkali metal ions contained in the quartz glass rod move to the outer wall of the quartz glass rod.
Table 1 comparison of the effects of the embodiment
Figure RE-GDA0002835303410000111
Figure RE-GDA0002835303410000121
In addition, referring to fig. 1 to 5, an embodiment of the present disclosure further provides a high-purity processing apparatus for a quartz glass tube/rod, which includes a base 12, a fixing mechanism 13, a heating mechanism 14, a molding mechanism 15, an ionization mechanism 16, and a controller 17; wherein the content of the first and second substances,
two sets of fixing mechanisms 13 are arranged on the top surface of the base 12, and are used for installing and fixing the quartz glass tube/rod 11 and driving the quartz glass tube/rod 11 to rotate by taking the axis of the quartz glass tube/rod as a shaft;
the heating mechanism 14 is arranged on the top surface of the base station 12, is positioned between the two groups of fixing mechanisms 13 and is used for heating the quartz glass tube/rod 11, and the heating mechanism 14 can move along the axial direction of the quartz glass tube/rod 11;
the shaping mechanism 15 is fixedly arranged on the heating mechanism 14 and is used for shaping the part of the quartz glass tube/rod 11 which expands outwards under the action of centrifugal force after being heated;
an ionization means 16 fixedly provided to the heating means 14 and generating an alternating current arc in a radial direction of the quartz glass tube/rod 11;
and a controller 17 disposed on a side surface of the base 12, wherein the fixing mechanism 13, the heating mechanism 14, the molding mechanism 15, and the ionization mechanism 16 are electrically connected to the controller 17.
In this embodiment, two sets of fixing mechanisms 13 are respectively used for fixing two ends of the quartz glass tube/rod 11, and the quartz glass tube/rod 11 is driven to rotate by a synchronous driving device. In order to make the distance between the two sets of fixing means 13 adaptable to quartz glass tubes/rods 11 of various lengths, one set of fixing means 13 may be arranged to be fixed and the other set may be arranged to be movable in the axial direction of the quartz glass tube/rod 11. By moving one set of fixing means 13, the distance between the two sets of fixing means 13 is adjusted to suit the length dimension of the quartz glass tube/rod 11. The movable fixing mechanism 13 can be realized by arranging an electric wheel on the bottom surface of the fixing mechanism 13 and arranging a sliding groove on the top surface of the base station 12, and the electric wheel is matched with the sliding groove. The application range of the device is improved.
The heating mechanism 14 can heat the quartz glass tube/rod 11. Under the action of centrifugal force formed by high-speed rotation of the quartz glass tube/rod 11, the heated and softened part of the quartz glass tube/rod 11 is expanded outwards, the tube wall becomes thinner, the outer diameter is increased, and the tube expanding processing is completed. The heating mechanism 14 can move along one end of the quartz glass tube/rod 11 to the other end, so as to realize the sectional heating and tube expanding of the quartz glass tube/rod 11.
The shaping mechanism 15 in cooperation with the heating mechanism 14 can restrict the tube expansion size of the silica glass tube/rod 11 to obtain the silica glass tube/rod 11 having a desired outer diameter size.
The ionization mechanism 16 ionizes the air outside the quartz glass tube/rod 11 to generate an arc discharge. And impurities in the quartz glass tube/rod 11 are cleaned, and the quality of the product is ensured.
In a preferred embodiment, as shown in fig. 1 and 2, the fixing mechanism 13 includes a supporting platform 31 fixedly disposed on the top surface of the base platform 12, an electric bearing 32 is fixedly disposed on the top surface of the supporting platform 31, a fixing ring 33 is fixedly disposed on an inner annular surface of the electric bearing 32, at least 2 telescopic driving components 34 are uniformly embedded in the fixing ring 33 along an annular direction, a telescopic end 35 of each telescopic driving component 34 extends to the center of the fixing ring 33, and a fixing plate 36 is fixedly connected to an end of each telescopic end 35.
In the present embodiment, the arc-shaped surfaces of the fixing plates 36 are located on the same circumference, and the telescopic ends 35 of the telescopic driving parts 34 are synchronously driven in a telescopic manner, so that the fixing plates 36 can be matched with and fixedly hold the quartz glass tube/rod 11. The telescopic driving part 34 may be a common automatic control telescopic device such as a cylinder, a hydraulic telescopic rod or an electric telescopic rod.
To ensure an effective clamping of the quartz glass tube/rod 11, the holding plate 36 preferably conforms to the arcuate configuration of the quartz glass tube/rod 11. The smaller the number of the telescopic driving members 34, the less the fixing effect on the silica glass tube/rod 11 and the more uneven the force applied to the silica glass tube/rod 11 in the circumferential direction. The number of the telescopic driving parts 34 is preferably set to 4-6. To further increase the fixing effect, an anti-slip layer is disposed on the surface of the fixing plate 36 away from the telescopic end 35.
The fixing ring 33 is fixedly mounted to the inner circumferential surface of the electric bearing 32 by interference fit for mounting the respective telescopic driving parts 34. The quartz glass tube/rod 11 held by the holding plate 36 is driven to rotate by the electric bearing 32, and the rotation speed is 30 to 70r/min for high-purity operation and 80 to 200r/min for tube expansion operation, so that centrifugal force is generated. The electric bearings 32 of the two sets of fixing mechanisms 13 are driven to rotate synchronously, so that the quartz glass tube/rod 11 is ensured to rotate stably.
In a preferred embodiment, as shown in fig. 1, 3 and 4, the heating mechanism 14 includes a track groove 41 disposed on the top surface of the base 12 between the two sets of fixing mechanisms 13, the track groove 41 is disposed along the axial direction of the quartz glass tube/rod 11, a moving block 42 is disposed above the track groove 41, a driving part 43 embedded in the track groove 41 is disposed on the bottom surface of the moving block 42, mounting plates 44 are symmetrically disposed on the top surface of the moving block 42 on both sides of the quartz glass tube/rod 11, a heating source 45 is disposed on the plate surface of the mounting plate 44 close to the quartz glass tube/rod 11, the heating source 45 is disposed at the same height as the quartz glass tube/rod 11, and the heating source 45 is a plasma torch, a oxyhydrogen flame torch or a laser.
In this embodiment, the driving part 43 drives the moving block 42 to move along the axial direction of the quartz glass tube/rod 11 at a speed of 40-100mm/min to expand the quartz glass tube/rod 11. The drive member 43 may be a drive mechanism such as a motorized roller, track, or chain. The heating sources 45 are symmetrically distributed on both sides of the quartz glass tube/rod 11 to ensure that the quartz glass tube/rod 11 is uniformly heated. The heating source 45 operates at a temperature of 1700 c to 1900 c to heat the quartz glass tube/rod 11.
In a preferred embodiment, as shown in fig. 3 to 5, the shaping mechanism 15 comprises an expanding idler 54 which can move in a direction close to or away from the quartz glass tube 11, the expanding idler 54 is coaxially arranged below the quartz glass tube 11, and the expanding idler 54 is a graphite wheel for limiting the position of the quartz glass tube 11 during the tube expanding operation.
In this embodiment, the component for driving the tube expanding roller 54 to move may be a molding cylinder 51, and is fixedly disposed on the top surface of the moving block 42 below the quartz glass tube 11. The shaping piston rod 52 of the shaping cylinder 51 is vertically arranged upwards, the top end of the shaping piston rod 52 is fixedly connected with a mounting frame 53, and the mounting frame 53 is rotatably provided with an expanding supporting roller 54 through a bearing, and the top surface of the expanding supporting roller 54 protrudes out of the mounting frame 53, so that the top surface of the expanding supporting roller can be in contact with the quartz glass tube 11.
Similarly, the shaping cylinder 51 can be replaced by a hydraulic telescopic rod or an electric telescopic rod.
The controller 17 controls the extension and contraction of the shaping piston rod 52 of the shaping cylinder 51, so that the distance between the top surface of the pipe expanding riding wheel 54 and the axis of the quartz glass pipe 11 can be adjusted. This distance is the radial dimension of the quartz glass tube 11 after the tube expansion. It is ensured that the tube expansion dimension of the silica glass tube 11 is controllable.
In a preferred embodiment, as shown in fig. 4, the ionization mechanism 16 includes an ac power source and a first electrode 61 and a second electrode 62 electrically connected to the ac power source, wherein the first electrode 61 and the second electrode 62 are respectively fixedly disposed on the heating mechanism 14, symmetrically distributed on two sides of the quartz glass tube/rod 11, and disposed close to the quartz glass tube/rod 11.
In this embodiment, the first electrode 61 and the second electrode 62 can move with the heating mechanism 14, so as to realize ionization purification of the whole quartz glass tube/rod 11. The first electrode 61 and the second electrode 62 may be fixedly mounted to the heating source 45, respectively, or may be directly fixedly mounted to the mounting plate 44.
The voltage of the alternating current power supply is 380V, and the output is alternating current. The 380V voltage of an alternating current power supply is boosted to 50-200kV output voltage and 10-200mA output current through a high-voltage transmitting device through control units such as a rectifying filter, a voltage regulation unit, an inverter loop and the like; the maximum 200kV high voltage is instantaneously generated by adopting a constant current principle when a power supply works, air between two electrodes 61 is ionized, and then electric arcs are generated; the voltage value is pulled down to control the current value within the set value range, and the arc is stably discharged under the stable constant current state. By the heated flow of the conductive gas, it is possible to purify the impurity alkali metal ions and the like in the silica glass tube/rod 11 without bringing the electrode 61 into contact with the silica glass tube/rod 11, and to ensure the processing quality of the silica glass tube/rod 11.
According to the embodiment of the disclosure, the following technical effects are achieved:
the technical scheme disclosed by the invention has the advantages that the purification efficiency is high, the time is saved, the surface of the glass tube/rod cannot be damaged, and the deformation of the glass tube expanding is easy to control and difficult to generate deviation due to relatively short time. The electrode and the glass tube/rod keep a certain distance, so that elements in the electrode cannot pollute the quartz glass tube/rod, higher cleanliness is guaranteed, the high-precision quartz glass tube/rod is suitable for the high-precision application field, meanwhile, the quartz glass tube/rod is not contacted, and the surface quality of the glass tube/rod is superior to the defects caused by contact in the direct current high-purity process. In a word, the technical scheme of the method not only improves the purity of the quartz glass tube/rod, but also improves the generation efficiency, has simple requirements on equipment, and greatly saves the engineering cost.
In the description of the present specification, the terms "connect", "mount", "fix", and the like are to be understood in a broad sense, for example, "connect" may be a fixed connection, a detachable connection, or an integral connection; may be directly connected or indirectly connected through an intermediate. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
In the description of the present application, the description of the terms "one embodiment," "some embodiments," etc. means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (16)

1. A method for purifying a quartz glass tube/rod, comprising: a high-purification step of heating the quartz glass tube/rod while generating a continuous stable arc outside the quartz glass tube/rod to move alkali metal ions contained in the quartz glass tube/rod toward an outer wall of the quartz glass tube/rod.
2. A method for purifying a quartz glass tube/rod according to claim 1, wherein the heating of the quartz glass tube/rod is performed by uniformly distributing one or more heating sources around the circumference of the quartz glass tube/rod, the heating sources being a plasma torch, an oxyhydrogen flame torch or a laser; the quartz glass tube/rod is heated at a temperature of 1700 ℃ to 1900 ℃.
3. A method for purifying a silica glass tube/rod as set forth in claim 1 or 2, wherein the continuous stable arc is an alternating arc generated by arranging a pair of electrodes on the outside of the silica glass tube/rod and applying an alternating voltage of 50 to 200kV and a current of 80 to 200mA to the electrodes.
4. A method for high purity of a silica glass tube/rod as set forth in claim 3, wherein the pair of electrodes are provided on the same cross section or on different cross sections of the silica glass tube/rod.
5. The method for purifying a silica glass tube/rod as set forth in any one of claims 1 to 4, wherein the silica glass tube/rod is rotated with its mandrel as a rotation axis at a rotation speed of 30 to 70 r/min; the electrode and the torch are horizontally moved outside the quartz glass tube/rod in a direction parallel to the axial direction of the quartz glass tube/rod at a horizontal moving speed of 40 to 100 mm/min.
6. The method for high-purifying a silica glass tube/rod as set forth in any one of claims 1 to 4, wherein the method for high-purifying a silica glass tube further comprises, after the step of high-purifying: expanding the tube at 1700-1900 deg.c and at 80-200r/min and the horizontal moving speed of the blast burner 40-100 mm/min.
7. The method for high-purifying a silica glass tube/rod as set forth in any one of claims 1 to 4, wherein the method for high-purifying a silica glass tube further comprises, before the step of high-purifying: expanding the tube at 1700-1900 deg.c and at 80-200r/min and the horizontal moving speed of the blast burner 40-100 mm/min.
8. A highly purified quartz glass tube/rod produced by the method as set forth in any one of claims 1 to 7, characterized in that the content of lithium ions in the surface layer of the inner wall is 0.5ppm or less; the lithium ion content of the bulk impurity is 0.1ppm or less.
9. Use of the quartz glass tube/rod according to claim 8 in the fields of optical fibers, semiconductors, photovoltaics.
10. A high-purity device of a quartz glass tube/rod is characterized by comprising a base station, a fixing mechanism, a heating mechanism, a molding mechanism, an ionization mechanism and a controller; wherein the content of the first and second substances,
the two groups of fixing mechanisms are arranged on the top surface of the base station and are used for installing and fixing the quartz glass tubes/rods and driving the quartz glass tubes/rods to rotate by taking the axis of the quartz glass tubes/rods as a shaft;
the heating mechanism is arranged on the top surface of the base station, is positioned between the two groups of fixing mechanisms and is used for heating the quartz glass tube/rod, and the heating mechanism can move along the axial direction of the quartz glass tube/rod;
the shaping mechanism is fixedly arranged on the heating mechanism and is used for shaping the part of the quartz glass tube which expands outwards under the action of centrifugal force after being heated;
the ionization mechanism is fixedly arranged on the heating mechanism and generates an alternating current arc in the radial direction of the quartz glass tube/rod;
the controller is arranged on the side face of the base station, and the fixing mechanism, the heating mechanism, the molding mechanism and the ionization mechanism are all electrically connected with the controller.
11. The high-purity device according to claim 10, wherein the fixing mechanism comprises a supporting table fixedly arranged on the top surface of the base table, an electric bearing is fixedly arranged on the top surface of the supporting table, a fixing ring is fixedly arranged on the inner ring surface of the electric bearing, at least 2 telescopic driving parts are uniformly embedded in the fixing ring along the circumferential direction, the telescopic ends of the telescopic driving parts extend to the center of the fixing ring, and a fixing plate is fixedly connected to the ends of the telescopic ends.
12. The apparatus according to claim 11, wherein the heating means comprises a track groove formed on the top surface of the base plate between two sets of fixing means, the track groove is arranged along the axial direction of the quartz glass tube/rod, a moving block is arranged above the track groove, a driving member embedded in the track groove is arranged on the bottom surface of the moving block, mounting plates are symmetrically arranged on the top surface of the moving block on both sides of the quartz glass tube/rod, heating sources are arranged on the plate surfaces of the mounting plates close to the quartz glass tube/rod, and the heating sources are arranged at the same height as the quartz glass tube/rod.
13. The high-purity apparatus according to claim 12, wherein the heating source is a plasma torch, a oxyhydrogen flame torch, or a laser.
14. The apparatus according to claim 12, wherein said molding mechanism comprises an expander roller movable in a direction close to or away from said silica glass tube, said expander roller being coaxially disposed below said silica glass tube.
15. The high purity processing apparatus of claim 14, wherein the expander roller is a graphite roller.
16. The apparatus according to claim 14, wherein the ionization means comprises an ac power source and a first electrode and a second electrode electrically connected to the ac power source, and the first electrode and the second electrode are respectively fixedly disposed on the heating means, symmetrically disposed on both sides of the quartz glass tube/rod, and disposed adjacent to the quartz glass tube/rod.
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US4759787A (en) * 1984-11-05 1988-07-26 Tsl Group Plc Method of purifying molten silica
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