Synthetic quartz bar deposition device and method

Abstract

The invention relates to a synthetic quartz bar deposition device and method.The device comprises a reaction cavity used for deposition and a rotary lifting suspender stretching into an inner cavity of the reaction cavity, the upper end of the rotary lifting suspender is connected with a vertical lifting mechanism and a rotary chuck, and the lower end of the rotary lifting suspender is connected with a glass target bar; the device is characterized in that the blow lamp assembly comprises a horizontal moving support, an inclined telescopic rod is arranged at the upper end of the horizontal moving support, and the front end of the inclined telescopic rod is connected with a blow lamp capable of swinging up and down. According to the method, the spraying range can be expanded, the deposition uniformity can be improved, the temperature distribution of a deposition area can be more uniform, the axial uniformity and the radial uniformity of a deposited bar can be improved at the same time, and therefore the deposition stability and the quality of the deposited bar are improved.

Description

Technical Field

[0001] The invention relates to a synthetic quartz rod deposition device and method, belonging to the technical field of glass material manufacturing. Background Art

[0002] Semiconductors, optical communications, photovoltaics, optics, electric light sources and other industries and fields are important areas of development of emerging industries, and high-purity quartz is widely used in these industries and fields. In today's rapidly developing information society, synthetic quartz materials have become increasingly indispensable. There are many ways to prepare synthetic quartz materials. The most common one is the one-step synthesis method, which is to introduce hydrogen, oxygen, and evaporated silicon tetrachloride liquid into a special burner. After being heated by the burner, the raw materials are melted near a specific target material in a certain area. After a long period of continuous firing, solid cylindrical glass products are finally formed.

[0003] However, the quartz products made by this one-step synthesis technology contain a high content of water vapor molecules or ions (i.e., hydroxyl content), which limits the infrared and near-infrared bands of the material when used later; and for doped synthetic quartz, such as titanium-containing and fluorine-containing synthetic quartz, it is difficult to meet the uniformity requirements inside optical products in the general way; it is necessary to develop a device and method for preparing large-sized quartz powder materials, which have high purity and low optical non-uniformity for pure synthetic quartz materials. The means to solve the above problems is a two-step synthesis technology, that is, the first step is to make solid silica powder, and then a second treatment is carried out within a certain temperature range, and then it is fired to make it transparent. Therefore, the continuous and stable preparation of the powder must be achieved first.

[0004] Japanese patent JP2000007350A realizes the preparation of larger powder rods by designing a new type of burner. The diameter of the burner reaches 120mm or 130mm, which is difficult to process glass products. In addition, it requires an evaporation rate of 115-130g / min of silicon tetrachloride, which makes the supporting evaporation equipment and supply system very expensive. The cost of a single device is high, which is not conducive to large-scale production.

[0005] Japanese patent JP2006232638A prepares powder vertically upward by placing a blowtorch just below the target rod. Since the flame of this method directly pushes above the powder rod, dust pollution will be caused in the deposited area above, affecting the quality of the product. Summary of the invention

[0006] The technical problem to be solved by the present invention is to provide a synthetic quartz rod deposition device and method in view of the deficiencies in the above-mentioned prior art, which can not only realize the preparation of large-size synthetic quartz rods, but also can deposit stably and evenly, and the product quality is good.

[0007] The device technical solution adopted by the present invention to solve the above-mentioned problems is:

[0008] The invention comprises a reaction chamber for deposition and a rotating lifting rod extending into the inner cavity of the reaction chamber, wherein the upper end of the rotating lifting rod is connected to a vertical lifting mechanism and a rotating chuck, the lower end of the rotating lifting rod is connected to a glass target rod, and a blowtorch assembly is arranged below the inner cavity of the deposition chamber corresponding to the glass target rod. The invention is characterized in that the blowtorch assembly comprises a horizontal movable support, an oblique telescopic rod is arranged at the upper end of the horizontal movable support, and a blowtorch which can swing up and down is connected to the front end of the oblique telescopic rod.

[0009] According to the above solution, the oblique telescopic rod is an electric telescopic rod or a pneumatic telescopic rod.

[0010] According to the above solution, the oblique telescopic rod has a synchronous telescopic extension rod extending backward.

[0011] According to the above solution, the included angle between the axis of the oblique telescopic rod and the rotary lifting boom is 20 to 60 degrees.

[0012] According to the above scheme, the blowtorch that can swing up and down includes a blowtorch whose rear end is hinged to an oblique telescopic rod, and whose side surface is hinged to a transverse telescopic rod.

[0013] According to the above scheme, the transverse telescopic rod is an electric telescopic rod or a pneumatic telescopic rod, and the lower side of the driving head (motor or cylinder) of the transverse telescopic rod is connected to the rear end of the synchronous telescopic extension rod through a support rod.

[0014] According to the above scheme, the moving track of the horizontal moving support, the moving track of the oblique telescopic rod and the up and down swinging track of the blowtorch are all located in the same vertical radial plane relative to the axis of the rotating lifting boom.

[0015] According to the above scheme, the swing angle of the blowtorch that can swing up and down is 0-40°.

[0016] According to the above scheme, the blowtorch is connected to a raw material control system, and the raw material included in the raw material control system is a gas raw material after evaporation of liquid silicon tetrachloride, or a mixed raw material of liquid silicon tetrachloride, liquid titanium tetrachloride and fluorine-containing gas after evaporation.

[0017] The technical solution of the synthetic quartz rod deposition preparation method of the present invention is:

[0018] Open the deposition chamber, fix the glass target rod at the clamping position at the lower end of the rotating lifting rod, start the rotating lifting rod, and move the rod to the initial position;

[0019] Light the blowtorch, rotate the lifting boom to drive the glass target rod to start rotating, and the upward lifting speed of the boom is zero at this time;

[0020] The raw material control system is turned on. The raw material control system supplies the blowtorch according to the set value of the flow meter. The blowtorch burns and sprays the raw material. The hydrolysis product after the hydrolysis reaction begins to be deposited at the preset position of the glass target rod. In the initial stage of deposition, the rotating lifting boom is pulled up from the starting position at an initial pulling speed lower than the stable section until it reaches the preset speed, that is, the constant speed of the stable section. The deposition enters a continuous stable stage, and the rotating lifting boom is pulled up at a constant speed; the blowtorch continues to spray until the deposition reaches a predetermined length.

[0021] According to the above scheme, the initial stage of the deposition process is divided into four stages according to the change of the preset target diameter of the deposition:

[0022] The first stage, deposition stage: the blowtorch moves backwards through the oblique telescopic rod along the opposite direction of the flame at a preset speed, the speed is M1;

[0023] Second deposition stage: Based on the first deposition stage, the blowtorch performs horizontal reciprocating deposition through a horizontal moving support at a certain preset speed, and the reciprocating motion speed is N1;

[0024] The third deposition stage: based on the movement in the second stage, the speed of the horizontal reciprocating movement of the blowtorch changes from N1 to N2, and at the same time, the swing angle θ1 and the angular velocity ω1 are superimposed to perform up and down reciprocating swing deposition; until the preset deposition diameter is reached, that is, the deposition in the initial stage is completed;

[0025] The fourth deposition stage: when the preset deposition diameter is reached, the blowtorch retreats a distance in the opposite direction of the flame through the oblique telescopic rod, and then reciprocates horizontally at a speed N3 for deposition. At the same time, the blowtorch reciprocates up and down at a swing angle θ2 and an angular velocity ω2 for deposition, and the rotating lifting boom is pulled up at a constant speed until the deposition is completed.

[0026] In the fourth stage, the deposition can be carried out by reciprocating up and down swinging at the maximum swing angle. The maximum swing angle θ is calculated by the formula θ=(90-93)*D / L degrees, where D is the diameter of the blowtorch used, unit: mm, and L is the length of the intersection of the center point of the blowtorch swing arm through the flame center axis and the target rod axis, unit: mm.

[0027] According to the above scheme, the speed of the horizontal reciprocating movement is N=D*OD / (L*T), T is the time used for the four stages of deposition, unit: minute, OD is the diameter of the deposited product to be achieved, unit: mm, L is the length of the intersection of the center point of the blowtorch swing arm through the center axis of the flame and the axis of the target rod, unit: mm.

[0028] According to the above scheme, the blowtorch can swing up and down with an angle of 0 to 40°, an angular velocity ω of 0.5 to 5° / min, ω1 and ω2 are both taken at ω, and ω1<ω2.

[0029] According to the above scheme, the horizontal reciprocating speed N of the blowtorch is 0.1-5.0 mm / min, N1, N2, and N3 are all taken at N, and N1<N2<N3.

[0030] According to the above scheme, the displacement adjustment speed M1 of the blowtorch along the axis where the flame of the blowtorch is located is 0.1-2mm / min, and the stroke is 0-200mm.

[0031] According to the above scheme, the diameter D of the blowtorch is 40-100 mm.

[0032] According to the above scheme, the diameter of the prepared loose matrix of synthetic quartz material is 100-500mm.

[0033] According to the above scheme, when the blowtorch moves to the lower end of the target rod, the center of the blowtorch flame always falls on the area near the outer side of the powder rod.

[0034] The beneficial effects of the present invention are as follows: 1. By arranging an oblique telescopic rod and connecting a blowtorch that can swing up and down at the front end of the oblique telescopic rod, the blowtorch can move back and forth and swing up and down along the flame spraying direction, which can not only expand the spraying range and improve the uniformity of deposition, but also make the temperature distribution in the deposition area more uniform, and can improve the axial uniformity and radial uniformity of the deposited rod at the same time, thereby improving the stability of deposition and the quality of the deposited rod; 2. During deposition, different methods are used in stages according to different target diameters to perform spray deposition, which can not only improve the efficiency of deposition, but also further improve the uniformity of deposition; the role of the first stage is mainly to ensure that the distance from the blowtorch to the deposition surface is always maintained at a certain distance during the deposition process, Thereby, the temperature gradient of the deposition surface is ensured; the second stage mainly serves to ensure uniform adhesion of particles of each layer of powder in the deposition area; the third stage mainly serves to compensate for the insufficient flame area after the powder rod size is enlarged, so that the temperature of the entire deposition surface of the powder rod is more uniform; the fourth stage mainly serves to ensure that the powder rod can obtain a larger size, and the deposition temperature field within the maximum outer diameter surface is uniform, and high-purity and high-uniformity doped synthetic quartz materials can be obtained when the raw material mixed titanium and fluorine compounds are deposited; 3. The deposited rods of the present invention have lower optical non-uniformity, and can be used for the doped deposition of titanium tetrachloride in silicon tetrachloride to prepare high-purity and high-uniformity titanium-doped synthetic quartz materials and high-purity and high-uniformity fluorine-doped synthetic quartz materials, and are suitable for large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 The figure is a schematic diagram of the overall structure of an embodiment of the present invention.

[0036] Figure 2 The figure is a schematic diagram of the structure of a blowtorch according to an embodiment of the present invention.

[0037] Figure 3 This is a comparison diagram of the radial refractive index distribution of the transparent glass mother material prepared by the present invention. DETAILED DESCRIPTION

[0038] The present invention is further described below in conjunction with embodiments and drawings.

[0039] An embodiment of the device of the present invention is Figure 1 , 2 As shown, it includes a reaction chamber 8 for deposition and a rotating lifting boom 1 extending into the inner cavity of the reaction chamber, the upper end of the rotating lifting boom is connected to a vertical lifting mechanism 10 and a rotating chuck 9, the lower end of the rotating lifting boom is connected to a glass target rod 2, a blowtorch assembly is arranged below the inner cavity of the deposition chamber corresponding to the glass target rod, the blowtorch assembly includes a horizontally movable support 4, an oblique telescopic rod 5 is arranged on the upper end of the horizontally movable support, the oblique telescopic rod is an electric telescopic rod, the oblique telescopic rod has a synchronous telescopic extension rod extending backward, the angle between the oblique telescopic rod and the axis of the rotating lifting boom is 30-50°, the front end of the oblique telescopic rod is connected to a blowtorch 3 that can swing up and down, the blowtorch that can swing up and down includes a blowtorch whose rear end is hinged to the oblique telescopic rod, the side of the blowtorch is hinged to a transverse telescopic rod 6, the transverse telescopic rod is an electric telescopic rod, the lower side of the driving head of the transverse telescopic rod is hinged to the rear end of the synchronous telescopic extension rod of the oblique telescopic rod through a support rod, and the blowtorch is driven to swing up and down by the telescopic movement of the transverse telescopic rod. The blowtorch is connected to a raw material control system, and the raw material included in the raw material control system is a gas raw material after evaporation of liquid silicon tetrachloride, or a mixed raw material of liquid silicon tetrachloride, liquid titanium tetrachloride and fluorine-containing gas after evaporation.

[0040] The technical scheme of the synthetic quartz rod deposition preparation method of the present invention is: using the above-mentioned device, opening the deposition chamber, fixing the glass target rod at the clamping position at the lower end of the rotating lifting suspension rod, turning on the rotating lifting suspension rod, and moving the suspension rod to the initial position; igniting the blowtorch, the rotating lifting suspension rod drives the glass target rod to start rotating, and at this time the upward lifting speed of the suspension rod is zero; turning on the raw material control system, the raw material control system supplies the blowtorch according to the set value of the flow meter, the blowtorch burns and sprays the raw material, and the hydrolysis product after the hydrolysis reaction begins to be deposited at the preset position of the glass target rod. In the initial stage of deposition, the rotating lifting suspension rod is pulled upward from the starting position at an initial pulling speed lower than the stable section until it reaches the preset speed, that is, the constant speed of the stable section; the rotating lifting suspension rod is pulled upward at a constant speed; the blowtorch continues to spray until the deposition reaches a predetermined length, and finally a large-sized quartz mother material 7 is prepared by deposition.

[0041] At the beginning of the deposition process, the torch operates in four stages according to the change of the preset target diameter of the deposition:

[0042] In the first stage of deposition: the blowtorch 3 moves backwards in the opposite direction of the flame through the oblique telescopic rod 5 at a preset speed of 0.2 mm / min, and the operation time is 600 minutes; then enters the second stage of deposition: on the basis of the first stage, the blowtorch performs horizontal reciprocating motion deposition at a preset speed of 0.2 mm / min under the action of the horizontal movable support 4; then enters the third stage of deposition: on the basis of the movement in the second stage, the horizontal reciprocating speed of the blowtorch is changed from 0.2 mm / min to 0.5 mm / min, and the swing angle is superimposed. The torch is deposited by reciprocating at an angle of 30° (with the initial position of the torch as the origin, and deflected 15° up and down) and an angular velocity of 0.5° / min; until the preset diameter is reached, the fourth stage of stable deposition is carried out: the torch is retreated a distance in the opposite direction of the flame through the oblique telescopic rod, and then the torch is deposited by reciprocating in the horizontal direction at a speed of 1.0mm / min, and at the same time, the torch is deposited by reciprocating at a maximum swing angle of 40° and an angular velocity of 1.0° / min, until the deposition is completed to obtain a diameter of 420mm and a density of 0.38g / cm 3 of loose powder.

[0043] The device and method can also be used for the deposition of a mixed raw material after evaporation of liquid silicon tetrachloride and liquid titanium tetrachloride to prepare a powder matrix material of transparent glass rods with different doped titanium contents; and the deposition of a mixed raw material after evaporation of liquid silicon tetrachloride and a fluorine-containing mixture to prepare a powder matrix material of transparent glass rods with different doped fluorine contents.

[0044] After the deposition is completed, it is placed in a high-temperature sintering furnace and a certain proportion of helium, chlorine, oxygen and other gases are introduced at about 1400-1600 degrees Celsius to prepare a transparent quartz material. In this embodiment, a quartz material with a diameter of 420 mm and a density of 0.38 g / cm 3 The loose powder is placed in a high-temperature glass tube at 1550 degrees Celsius. After 40 hours of firing, a transparent glass mother material with a diameter of 232 mm is finally produced.

[0045] Figure 3The transparent glass mother material with a diameter of 230 mm prepared by the above embodiment is tested by a high-precision refractive index testing device. The relative difference of the refractive index value of 1.45732 of pure silica glass in radial test (an important indicator to characterize the uniformity of the prepared glass material) can be seen from the test chart. The glass mother material prepared without the use of the claimed equipment and method of the present invention has a diameter of only 100 mm, and within 80% of the diameter of the product, its radial refractive index difference relative value reaches 0.00024, while the glass mother material prepared with the claimed equipment and method of the present invention has a refractive index relative difference of 0.00007 within 80% of the diameter of the product; within 80% of the diameter of the glass mother material prepared with the claimed equipment and method of the present invention, its refractive index uniformity is improved by about 70.8%, and the glass mother material prepared with the claimed equipment and method of the present invention shows a uniform change trend in the radial direction, which has obvious advantages over the glass mother material prepared without the claimed equipment and method of the present invention.

Claims

1. A synthetic quartz rod deposition device, comprising a reaction chamber for deposition and a rotating lifting rod extending into the inner cavity of the reaction chamber, wherein the upper end of the rotating lifting rod is connected to a vertical lifting mechanism and a rotating chuck, the lower end of the rotating lifting rod is connected to a glass target rod, and a blowtorch assembly is arranged below the inner cavity of the deposition chamber corresponding to the glass target rod, characterized in that The blowtorch assembly comprises a horizontal movable support, an oblique telescopic rod is arranged on the upper end of the horizontal movable support, and the front end of the oblique telescopic rod is connected to the blowtorch which can swing up and down.

2. The synthetic quartz rod deposition device according to claim 2, characterized in that The oblique telescopic rod is an electric telescopic rod or a pneumatic telescopic rod.

3. The synthetic quartz rod deposition device according to claim 1 or 2, characterized in that The oblique telescopic rod has a synchronous telescopic extension rod extending backward.

4. The synthetic quartz rod deposition device according to claim 1 or 2, characterized in that The included angle between the axis of the oblique telescopic rod and the rotating lifting boom is 20-60 degrees.

5. The synthetic quartz rod deposition device according to claim 3, characterized in that The blowtorch capable of swinging up and down comprises a blowtorch whose rear end is hinged to an oblique telescopic rod, and whose side surface is hinged to a transverse telescopic rod.

6. The synthetic quartz rod deposition device according to claim 5, characterized in that The transverse telescopic rod is an electric telescopic rod or a pneumatic telescopic rod, and the lower side of the driving head of the transverse telescopic rod is connected to the rear end of the synchronous telescopic extension rod through a support rod.

7. The synthetic quartz rod deposition device according to claim 1 or 2, characterized in that The moving track of the horizontal moving support, the moving track of the oblique telescopic rod and the up and down swinging track of the blowtorch are all located in the same vertical radial plane relative to the axis of the rotating lifting boom.

8. The synthetic quartz rod deposition device according to claim 1 or 2, characterized in that The swing angle of the blowtorch that can swing up and down is 0-40 degrees.

9. The synthetic quartz rod deposition device according to claim 1 or 2, characterized in that The blowtorch is connected to a raw material control system, and the raw material included in the raw material control system is a gas raw material after evaporation of liquid silicon tetrachloride, or a mixed raw material of liquid silicon tetrachloride, liquid titanium tetrachloride and fluorine-containing gas after evaporation.

10. A method for depositing synthetic quartz rods, using any of the apparatuses described in claims 1 to 9, characterized in that Open the deposition chamber, fix the glass target rod at the clamping position at the lower end of the rotating lifting rod, start the rotating lifting rod, and move the rod to the initial position; Light the blowtorch, rotate the lifting boom to drive the glass target rod to start rotating, and the upward lifting speed of the boom is zero at this time; The raw material control system is turned on. The raw material control system supplies the blowtorch according to the set value of the flow meter. The blowtorch burns and sprays the raw material. The hydrolysis product after the hydrolysis reaction begins to be deposited at the preset position of the glass target rod. In the initial stage of deposition, the rotating lifting boom is pulled up from the starting position at an initial pulling speed lower than the stable section until it reaches the preset speed, that is, the constant speed of the stable section. The deposition enters a continuous stable stage, and the rotating lifting boom is pulled up at a constant speed; the blowtorch continues to spray until the deposition reaches a predetermined length.

11. The method for depositing synthetic quartz rods according to claim 10, characterized in that During the initial stage of the deposition process, the torch operates in four stages according to the change in the preset target diameter of the deposition: The first stage, deposition stage: the blowtorch moves backwards and deposits in the opposite direction of the flame through the oblique telescopic rod at a certain preset speed, the speed is M1; Second deposition stage: Based on the first deposition stage, the blowtorch performs horizontal reciprocating deposition through a horizontal moving support at a preset speed, and the reciprocating speed is N1; The third deposition stage: based on the movement in the second stage, the speed of the horizontal reciprocating movement of the blowtorch changes from N1 to N2, and at the same time, the swing angle θ1 and the angular velocity ω1 are superimposed to perform up and down reciprocating swing deposition; until the preset deposition target diameter is reached, that is, the deposition in the initial stage is completed; The fourth deposition stage: when the preset deposition diameter is reached, the blowtorch retreats a distance in the opposite direction of the flame through the oblique telescopic rod, and then reciprocates horizontally at a speed N3 for deposition. At the same time, the blowtorch reciprocates up and down at a swing angle θ2 and an angular velocity ω2 for deposition, and the rotating lifting boom is pulled up at a constant speed until the deposition is completed.

12. The method for depositing synthetic quartz rods according to claim 11, characterized in that In the fourth stage, the deposition is carried out by reciprocating up and down swinging at the maximum swing angle. The maximum swing angle θ is calculated by the formula θ=(90-93)*D / L degrees, where D is the diameter of the blowtorch used, unit: mm, and L is the length of the intersection of the center point of the blowtorch swing arm through the flame center axis and the target rod axis, unit: mm.

13. The method for depositing synthetic quartz rods according to claim 11, characterized in that The speed of the horizontal reciprocating movement N=D*OD / (L*T), T is the time used for the four stages of deposition, unit: minute, OD is the diameter of the deposited product to be achieved, unit: mm, L is the length of the intersection of the center point of the blowtorch swing arm through the flame center axis and the target rod axis, unit: mm.

14. The method for depositing synthetic quartz rods according to claim 11, characterized in that The blowtorch can swing up and down with a swing angle of 0 to 40 degrees, a swing angular velocity ω of 0.5 to 5 degrees / min, ω1 and ω2 are both taken at ω, and ω1<ω2.

15. The method for depositing synthetic quartz rods according to claim 11, characterized in that The horizontal reciprocating speed N of the blowtorch is 0.1-5.0 mm / min, N1, N2 and N3 are all taken at N, and N1<N2<N3.

16. The method for depositing synthetic quartz rods according to claim 11, characterized in that The range of adjusting speed M1 of the blowtorch along the axis where the flame of the blowtorch is located is 0.1-2mm / min. The stroke is 0-200mm.

17. The method for depositing synthetic quartz rods according to claim 10 or 11, characterized in that The diameter D of the blowtorch is 40-100 mm.

18. The method for depositing synthetic quartz rods according to claim 10 or 11, characterized in that The prepared synthetic quartz material loose matrix has a diameter of 100-500 mm.

19. The method for depositing synthetic quartz rods according to claim 10 or 11, characterized in that When the blowtorch moves to the lower end of the target rod, the center point of the blowtorch flame always falls on the area close to the outer side of the powder rod.

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