Patent Publication Number: US-2021163337-A1

Title: Method for producing porous glass fine particle body and method for producing optical fiber preform

Description:
CROSS-REFERENCE TO RELATED APPLICATIONS 
     The present application claims priority from International Patent Application No. PCT/2019/016024 filed Apr. 12, 2019, which claims priority from Japanese Patent Application No. 2018-112188 filed Jun. 12, 2018. The content of both applications are incorporated herein in their entirety. 
    
    
     TECHNICAL FIELD 
     The present invention relates to a method for producing a porous glass fine particle body and a method for producing an optical fiber preform. 
     BACKGROUND 
     In the related art, as shown in Patent Literature 1, a method for producing a porous glass fine particle body has been known in which glass fine particles are deposited on a starting base material such as a glass rod to form soot. By sintering this type of porous glass fine particle body, an optical fiber preform for producing an optical fiber or the like can be obtained. 
     Further, in the producing method of Patent Literature 1, a plurality of burners arranged side by side are reciprocated relative to the starting base material. Then, from the start of deposition of the glass fine particles (soot) on the starting base material to deposition of several layers, the return position of the reciprocating movement is fixed, and thereafter the return position is moved every time of reciprocating movement. It is disclosed that this structure suppresses the deviation generated at the interface between the starting base material and the soot. 
     PATENT LITERATURE 
     
         
         [Patent Literature 1] 
       
    
     Japanese Unexamined Patent Application, First Publication No. 2016-44087 
     In the porous glass fine particle body obtained by the producing method of Patent Literature 1, the boundary surface between the soot layers in the longitudinal direction and the boundary surface between the starting base material and the soot layer intersect each other. In this way, when the two boundary surfaces intersect, defects such as interface shift, clouding, and inclusion of bubbles are likely to occur at the intersections. 
     The above defects can be improved by, for example, reciprocating a single burner to deposit the soot, but in this case, the time required to deposit the soot increases and the production efficiency decreases. 
     SUMMARY 
     One or more embodiments provide a method for producing a porous glass fine particle body which suppresses the occurrence of defects at the boundary surface between the soot layer and the starting base material while maintaining the production efficiency. 
     A method according to one or more embodiments of the present invention is a method for producing a porous glass fine particle body in which a plurality of soot layers are formed on a surface of a starting base material by moving a burner group relative to the starting base material along a longitudinal direction of the rotating starting base material and releasing a raw material gas into a flame of the burner group. The method comprises: a first layer formation step of forming a first soot layer on the surface of the starting base material; and an outer layer formation step of forming a plurality of soot layers on an outside of the first soot layer, in which in the first layer formation step, the first soot layer is continuously formed without a break in the longitudinal direction, and in which in the outer layer formation step, the burner group is moved in a reciprocating manner in the longitudinal direction relative to the starting base material while the raw material gas is supplied to each burner included in the burner group to form the soot layers. 
     According to one or more embodiments of the present invention, it is possible to provide a method for a producing porous glass fine particle body which suppresses the occurrence of defects at the boundary surface between the soot layer and the starting base material while maintaining the production efficiency. 
    
    
     
       BRIEF DESCRIPTION OF DRAWINGS 
         FIG. 1A  is a diagram illustrating a method for producing porous glass fine particle body according to a first embodiment. 
         FIG. 1B  is a diagram showing a step following  FIG. 1A . 
         FIG. 1C  is a diagram showing a step that follows  FIG. 1B . 
         FIG. 1D  is a diagram showing a step following  FIG. 1C . 
         FIG. 2  is a view of porous glass fine particle body obtained by the producing method according to the first embodiment. 
         FIG. 3A  is a diagram illustrating a method for producing porous glass fine particle body according to a second embodiment. 
         FIG. 3B  is a diagram showing a step following  FIG. 3A . 
         FIG. 3C  is a diagram showing a step following  FIG. 3B . 
         FIG. 3D  is a diagram showing a step following  FIG. 3C . 
         FIG. 3E  is a diagram showing a step following  FIG. 3D . 
         FIG. 3F  is a diagram showing a step following  FIG. 3E . 
         FIG. 4  is a view of porous glass fine particle body obtained by the producing method according to the second embodiment. 
     
    
    
     DETAILED DESCRIPTION 
     First Embodiment 
     Hereinafter, the method for producing the porous glass fine particle body of the first embodiment will be described with reference to the drawings. The porous glass fine particle body obtained according to the present embodiment can be applied to, for example, an Outside Vapor Deposition method (OVD method) or a Vapor phase Axial Deposition method (VAD method) to obtain an optical fiber preform. The present invention is not limited to the embodiments below. 
     In the OVD method, glass fine particles are deposited on the outer surface of a starting base material such as a glass rod to form a soot layer, a porous glass fine particle body is obtained, and then the soot layer is sintered by heating to obtain an optical fiber preform. 
     The VAD method, deposition of glass fine particles is started from the tip end portion of a starting base material such as a glass rod to form a columnar soot layer, the porous glass fine particle body is obtained, and then the soot layer is sintered by heating to obtain an optical fiber preform. 
     However, the application of the porous glass fine particle body obtained in the present embodiment is not limited to the production of the optical fiber preform. 
     As shown in  FIG. 1A , porous glass fine particle body producing apparatus  10  of the present embodiment include a burner group  2  having a plurality of burners  2   a  to  2   d , a fixed base  3 , and a gas supply device (not shown). The number of burners included in the burner group  2  may be changed appropriately. 
     The plurality of burners  2   a  to  2   d  are arranged side by side along the longitudinal direction X of the starting base material  1 . The starting base material  1  is a glass rod made of silica glass or the like. Both ends (first end  1   a  and second end  1   b ) of the starting base material  1  are supported by a pair of rotary chucks (not shown). The starting base material  1  is rotated in the reaction container (not shown) by the rotary chuck. 
     (Direction Definition) 
     In this specification, the longitudinal direction of the starting base material  1  is simply referred to as the longitudinal direction X. Along the longitudinal direction X, the side closer to the burner  2   a  is called +X side, and the side closer to the burner  2   d  is called −X side. That is, the burner  2   a  (first burner), the burner  2   b  (second burner), the burner  2   c  (third burner), and the burner  2   d  (fourth burner) are arranged in this order from the +X side to the −X side. 
     The plurality of burners  2   a  to  2   d  are fixed to the fixed base  3  and are arranged at equal intervals in the longitudinal direction X. The fixed base  3  is movable in the longitudinal direction X along a rail (not shown). That is, the burner group  2  is movable relative to the starting base material  1  along the longitudinal direction X of the starting base material  1 . 
     In the present embodiment, the burner group  2  moves so as to reciprocate in the longitudinal direction X. However, the starting base material  1  may be reciprocated along the longitudinal direction X while the burner group  2  is stationary. That is, the burner group  2  may be able to reciprocate relative to the starting base material  1  along the longitudinal direction X. 
     A gas supply device (not shown) is connected to each of the burners  2   a  to  2   d . The gas supply device supplies the burners  2   a  to  2   d  with fuel for the pilot fire F 2 , raw material gas, oxygen gas, or the like. The supply device for the fuel of the pilot fire F 2  and the supply device for a raw material gas may be different. 
     Here, in this specification, the flame when the raw material gas is supplied to the burners  2   a  to  2   d  and the glass fine particles are generated is referred to as a generated flame F 1 . Further, the flame in a state in which the raw material gas is not supplied to the burners  2   a  to  2   d  and the glass fine particles are not generated is referred to as a pilot fire F 2 . Further, when simply referring to “flame”, both the generated flame F 1  and the pilot fire F 2  are included. 
     The setting of the heat power of the flame (generated flame F 1  or pilot fire F 2 ) may be different or may be common to the burners  2   a  to  2   d . Further, the setting may be changed according to the number of reciprocating movements of the burner group  2 . 
     In the method for producing the porous glass fine particle body according to the present embodiment, the pilot fire F 2  is constantly generated even when the generated flame F 1  is not generated. Thereby, when the raw material gas is supplied to the burners  2   a  to  2   d , the generation of glass fine particles can be started smoothly. However, the pilot fire F 2  may be extinguished before supplying the raw material gas, and the pilot fire F 2  may be generated immediately before supplying the raw material gas. Further, the heat power of the pilot fire F 2  may be changed in such a manner as that the heat power of the pilot fire F 2  is weakened before supplying the raw material gas, and the heat power of the pilot fire F 2  is strengthened immediately before supplying the raw material gas. 
     The burners  2   a  to  2   d  generate the pilot fire F 2  with a mixed gas of combustible gas (for example, hydrogen gas, methane, or the like) and oxygen. The raw material gas is released into the pilot fire F 2  to generate a generated flame F 1 , and glass fine particles are formed by an oxidation reaction or a hydrolysis reaction. The glass fine particles are deposited on the surface of the starting base material  1  to form soot, whereby the porous glass fine particle body  20  is obtained. 
     As the raw material gas, for example, silicon tetrachloride (SiCl 4 ) or a silicon-containing organic compound can be used. As the silicon-containing organic compound, an alkyl siloxane such as cyclic siloxane D 3  (hexamethylcyclotrisiloxane), D 4  (octamethylcyclotetrasiloxane, OMCTS), D 5  (decamethylcyclopentasiloxane) can be used. Here, “D” of the above-described silicon-containing organic compound means a unit of [(CH 3 ) 2 —Si]—O—, and for example, D 4  means a structure in which four D units are connected in a ring. Since the silicon-containing organic compound does not form hydrochloric acid even when subjected to an oxidation reaction, it contributes to a reduction in environmental load and a reduction in production cost due to the elimination of hydrochloric acid treatment equipment. In particular, D 4  is widely used industrially, is relatively inexpensive and is easily available. 
     Next, a specific method for producing the porous glass fine particle body  20  will be described. 
     (First Layer Formation Step) 
     First, the first layer formation step shown in  FIGS. 1A and 1B  is performed. More specifically, as shown in  FIG. 1A , the raw material gas is supplied to the burner  2   a  in a state where the burner  2   a  is located at the predetermined first boundary position B 1 . Thus, the generated flame F 1  is generated by the burner  2   a , and the formation of glass fine particles is started. At this time, the raw material gas is not supplied to the burners  2   b  to  2   d , and the pilot fire F 2  is generated. 
     Next, as shown in  FIG. 1B , the burner group  2  (fixed base  3 ) is moved to the +X side with respect to the starting base material  1 . Thus, the glass fine particles formed by the generated flame F 1  of the burner  2   a  are deposited on the starting base material  1  to form the first soot layer  11 . The first soot layer  11  is a soot layer deposited first on the starting base material  1 . 
     In the first layer formation step, the raw material gas is continuously supplied to the burner  2   a  to form glass fine particles until the burner  2   a  reaches the second boundary position B 2  from the first boundary position B 1 . Thus, the first soot layer  11  is continuously formed in the longitudinal direction X without a break. 
     In the first layer formation step, by generating the pilot fire F 2  on the burners  2   b  to  2   d , the formed first soot layer  11  can be heated. 
     (Outer Layer Formation Step) 
     After the first layer formation step, the outer layer formation step shown in  FIGS. 1C and 1D  is performed. In the outer layer formation step, a plurality of soot layers  12  to  14  (see  FIG. 2 ) are formed on the outside of the first soot layer  11 . Although shown in a simplified manner in  FIG. 2 , the number of soot layers formed in the outer layer formation step is, for example, about 50 to 1000, and the thickness per layer is, for example, about 0.01 to 1.0 mm. 
     In the outer layer formation step, first, as shown in  FIG. 1C , the raw material gas is also supplied to the burners  2   b  to  2   d  to generate the flame F 1  therein. Then, as shown in  FIG. 1D , the burner group  2  is moved to the −X side with respect to the starting base material  1 . Thus, a second soot layer  12  is formed. At this time, the glass fine particles formed by the burners  2   a  to  2   d  are separately deposited on the first soot layer  11 . Therefore, the second soot layer  12  is formed by being divided into regions  12   a  to  12   d . Then, in the second soot layer  12 , boundary surfaces between the regions are formed at intervals in the longitudinal direction X. 
     Thereafter, the burner group  2  is reciprocated relative to the starting base material  1  along the longitudinal direction X between the first boundary position B 1  and the second boundary position B 2 . Thus, soot layers are sequentially deposited as shown in  FIG. 2 , and the porous glass fine particle body  20  are obtained. 
     (Method for Producing Optical Fiber Preform) 
     When producing the optical fiber preform, the porous glass fine particle body  20  are dehydrated (dehydration step) and sintered (sintering step). The sintering step may be performed after the dehydration step or may be performed simultaneously with the dehydration step. 
     In the dehydration step, water contained in the soot layer of the porous glass fine particle body  20  is removed by using dehydration gas. By removing the water, it is possible to reduce the light transmission loss of the optical fiber obtained from the porous glass fine particle body  20 . An inert gas containing a dehydrating agent can be used as the dehydration gas. As the dehydrating agent, chlorine (Cl 2 ) or a chlorine compound such as thionyl chloride (SOCl 2 ) can be used. A dehydrating agent such as carbon monoxide other than a chlorine compound may be used. 
     In the dehydration step, for example, the porous glass fine particle body  20  is installed and heated in an atmosphere of dehydration gas. At this time, dehydration gas enters the pores of the porous glass fine particle body  20  to dehydrate the inside of the porous glass fine particle body  20 . Therefore, the smaller the density of the glass fine particle body in the soot layer, the easier the dehydration gas enters, and the more efficient dehydration can be performed. 
     In the sintering step, the porous glass fine particle body  20  is heated at a high temperature (for example, 1400° C.) to vitrify the soot layer. Thus, the soot layer becomes a transparent glass body, and the optical fiber preform is obtained. 
     Further, the optical fiber can be produced by melting and drawing the optical fiber preform. 
     Incidentally, at the boundary surface between the starting base material  1  and the first soot layer  11 , defects such as interface shift, inclusion of bubbles, and clouding may occur. In order to suppress the occurrence of these defects, for example, it is conceivable to increase the temperature when forming the first soot layer  11  and firmly adhere the first soot layer  11  to the starting base material  1 . However, when the temperature at which the first soot layer  11  is formed is increased, the density of the glass fine particle body in the first soot layer  11  increases. When the density of the glass fine particle body increases, it becomes difficult for the dehydration gas to enter the pores in the above-described dehydration step. As a result, the efficiency of the dehydration step may be reduced or the dehydration may be insufficient. 
     The reduction in the efficiency of the dehydration step may lead to a reduction in the production efficiency of the optical fiber preform and the optical fiber and an increase in cost. Insufficient dehydration may lead to an increase in transmission loss due to water in the optical fiber (for example, an increase in loss at a wavelength of 1383 nm). 
     Under these circumstances, it is required to suppress the occurrence of defects at the boundary surface between the first soot layer  11  and the starting base material  1  without increasing the temperature when forming the first soot layer  11 . 
     The method for producing porous glass fine particle body of the present embodiment includes a first layer formation step for forming a first soot layer  11  on the surface of a starting base material  1 , and an outer layer formation step for forming a plurality of soot layers on the outside of the first soot layer  11 . Then, in the first layer formation step, the first soot layer  11  is continuously formed in the longitudinal direction X without a break. 
     As described above, by continuously forming the first soot layer  11  without breaks, it is possible to suppress the occurrence of defects such as an interface shift, inclusion of bubbles, and clouding at the interface between the first soot layer  11  and the starting base material  1 . Since the above effect can be obtained without increasing the temperature when forming the first soot layer  11 , the density of the glass fine particle body in the first soot layer  11  can be suppressed to be small, and the dehydration step can be performed efficiently and more reliably. Then, in the outer layer formation step, while reciprocating the burner group  2  relative to the starting base material  1  in the longitudinal direction X, the glass fine particles formed by the burners  2   a  to  2   d  are deposited. Thereby, the production efficiency of the porous glass fine particle body  20  can be improved. 
     Further, in the first layer formation step, by heating the first soot layer  11  with the pilot fire F 2  of the burners  2   b  to  2   d , the temperature decrease of the first soot layer  11  can be suppressed. By suppressing the temperature decrease of the first soot layer  11  in this way, it is possible to suppress the occurrence of defects due to temperature unevenness (temperature distribution, temperature change, or the like) during production. More specifically, when temperature unevenness occurs, since the first soot layer  11  and the starting base material  1  have different linear expansion coefficients, cracks or the like originating from the interface between the first soot layer  11  and the starting base material  1  is likely to occur. On the other hand, by heating the first soot layer  11  with the pilot fire F 2  of the burners  2   b  to  2   d  as described above, it is possible to stabilize the temperature of the first soot layer  11  and suppress the occurrence of cracks or the like. 
     Further, in the outer layer formation step, after the first layer formation step is completed, supply of the raw material gas to the burners  2   b  to  2   d  different from the burner  2   a  on which the first soot layer  11  is formed is started. With this configuration, the diameter of the porous glass fine particle body  20  can be stabilized in the longitudinal direction X. 
     Second Embodiment 
     Next, a second embodiment according to the present invention will be described, but the basic configuration is the same as that of the first embodiment. Therefore, the same reference numerals are given to similar components, the explanation thereof will be omitted, and only differences will be described. 
     In the first embodiment, the outer layer formation step is performed after the first layer formation step is completed. On the other hand, in the present embodiment, the first layer formation step and the outer layer formation step are performed simultaneously. 
     First, as shown in  FIG. 3A , the raw material gas is supplied to the burner  2   a  in a state where the burner  2   a  is located at the predetermined first boundary position B 1 . Thus, the generated flame F 1  is generated by the burner  2   a , and the formation of glass fine particles is started. At this time, the raw material gas is not supplied to the burners  2   b  to  2   d , and the pilot fire F 2  is generated. The heat power of the pilot fire F 2  does not need to be constant and may be changed as appropriate. Further, the pilot fire F 2  may be extinguished or weakened until the raw material gas is supplied to the burners  2   b  to  2   d , and the pilot fire F 2  may be ignited or the heat power may be strengthened immediately before the raw material gas is supplied. 
     Next, as shown in  FIGS. 3B to 3C , the burner group  2  (fixed base  3 ) is moved to the +X side with respect to the starting base material  1 . Thus, the first soot layer  11  is formed. Then, when the burner  2   b  reaches the first boundary position B 1 , the raw material gas is supplied to the burner  2   b . Thus, the generated flame F 1  is generated by the burner  2   b , the formation of glass fine particles is started, and the second soot layer  12  is formed on the surface of the first soot layer  11 . 
     Similarly thereafter, as shown in  FIGS. 3C and 3D , when the burners  2   c  and  2   d  reach the first boundary position B 1 , the raw material gas is supplied to the respective burners  2   c  and  2   d . That is, in the present embodiment, when the plurality of burners  2   a  to  2   d  reach the first boundary position B 1 , the supply of the raw material gas to the reached burners  2   a  to  2   d  is started. Therefore, while forming the first soot layer  11 , the second to fourth soot layers  12  to  14  are simultaneously formed. That is, the first layer formation step and the outer layer formation step are performed simultaneously. 
     As shown in  FIGS. 3E to 3F , when the burner  2   a  reaches the predetermined second boundary position B 2 , the fixed base  3  starts a turn-back movement toward the −X side. At this time, the burner  2   a  forms the second soot layer  12  on the first soot layer  11 . That is, the second soot layer  12  is formed separately in the portion formed by the burner  2   a  and the portion formed by the burner  2   b.    
     Similarly, the third to fourth soot layers  13  and  14  are formed by being divided in the longitudinal direction X by the burners  2   a  to  2   d.    
     On the other hand, the first soot layer  11  is continuously formed by the burner  2   a  without a break. Therefore, as in the first embodiment, an action effect by continuously forming the first soot layer  11  without a break can be obtained. 
     Further, in the present embodiment, the generated flame F 1  is generated by the burners  2   b  to  2   d  different from the burner  2   a  forming the first soot layer  11  during the first layer formation step, so that the first soot layer  11  is heated. Therefore, similarly to the first embodiment, it is possible to suppress the temperature decrease of the first soot layer  11  and suppress the occurrence of defects due to temperature unevenness. 
     Further, in the present embodiment, the supply of the raw material gas to the burners  2   a  to  2   d  is started when the burners  2   a  to  2   d  reach the first boundary position B 1 . Therefore, for example, as compared with the case where the supply is started when the burners  2   a  to  2   d  are located between the boundary positions B 1  and B 2 , it is possible to prevent the glass fine particles formed in an unstable state in the initial reaction of the raw material gas from being deposited on the intermediate portion in the longitudinal direction X of the porous glass fine particle body  20 . Therefore, the yield of the porous glass fine particle body  20  can be improved by increasing the proportion of the portion that can be used as the non-defective part. 
     In particular, when a silicon-containing organic compound is used as the raw material gas, defects are likely to occur due to the unstable mixing ratio of the raw material gas and the oxygen gas. Then, at the beginning of the supply of the raw material gas, the mixing ratio of the oxygen gas and the raw material gas is unlikely to be stabilized, so that the above-described defects are likely to occur. Therefore, the configuration of the present embodiment is suitable when the silicon-containing organic compound is used as the raw material gas. 
     In the porous glass fine particle body  20  obtained by the producing method of the present embodiment, as shown in  FIG. 4 , the number of soot layers formed changes in the longitudinal direction X. However, since the thickness of one soot layer is about 0.01 to 1.0 mm, the influence on the diameter stability of the porous glass fine particle body  20  is small. 
     Further, for example, the amount of glass fine particles formed by each of the burners  2   a  to  2   d  and deposited on the starting base material  1  may be changed such that the diameter of the porous glass fine particle body  20  becomes more stable in the longitudinal direction X. The amount of glass fine particles deposited on the starting base material  1  can be adjusted by various conditions such as the flow rate of the raw material gas, the moving speed of the burner group  2  with respect to the starting base material  1 , and the air flow in the reaction container. 
     It should be noted that the technical scope of the present invention is not limited to the above-described embodiments, and various modifications can be made without departing from the spirit of the present invention. 
     For example, in the above-described embodiment, the return position in the reciprocating movement of the burner group  2  when forming the second and subsequent layers of soot is fixed, but the return position may be gradually shifted. This can prevent the diameter of the porous glass fine particle body  20  from varying in the longitudinal direction X. 
     Further, the boundary positions B 1  and B 2  when forming the first soot layer  11  and the boundary positions B 1  and B 2  when forming the outer soot layer may be different. 
     Further, although the burners  2   a  to  2   d  are arranged at equal intervals in the above-described embodiments, the burners  2   a  to  2   d  may not be arranged at equal intervals. 
     In addition, without departing from the spirit of the present invention, it is possible to appropriately replace the constituent elements in the above-described embodiments with well-known constituent elements, and the above-described embodiments and modification examples may be appropriately combined. 
     Furthermore, although the disclosure has been described with respect to only a limited number of embodiments, those skilled in the art, having benefit of this disclosure, will appreciate that various other embodiments may be devised without departing from the scope of the present invention. Accordingly, the scope of the invention should be limited only by the attached claims. 
     REFERENCE SIGNS LIST 
     
         
         
           
               1  Starting base material 
               2  Burner group 
               2   a  to  2   d  Burner 
               11  First soot layer 
               12  to  14  Outer soot layer 
             B 1  First boundary position (boundary position) 
             X Longitudinal direction