CN115847763A - Method for preparing gradient plastic optical fiber by co-extrusion physical doping method - Google Patents
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- CN115847763A CN115847763A CN202211529932.6A CN202211529932A CN115847763A CN 115847763 A CN115847763 A CN 115847763A CN 202211529932 A CN202211529932 A CN 202211529932A CN 115847763 A CN115847763 A CN 115847763A
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Abstract
The invention discloses a method for preparing a gradient plastic optical fiber by a co-extrusion physical doping method, which comprises the following steps: step one, adopting a co-extrusion die to set corresponding layer areas according to the number of layers of optical fiber materials to form strip-shaped extrudates with concentric circle interfaces in a multi-layer structure; step two, extruding the strip-shaped extrudate, and then passing the extruded strip-shaped extrudate through a thermal forming diffusion zone with the temperature of 100-240 ℃, wherein the retention time of the strip-shaped extrudate in the diffusion zone is 1-10 min; the refractive index of the multilayer structure is gradually reduced from inside to outside to form gradient distribution, and each layer in the multilayer structure is formed by extruding a polymer physically doped inert dopant; compared with the prior art, the invention adopts physical doping, does not carry out chemical reaction, only changes the micromolecule substance of the refractive index, basically stops the diffusion process at the temperature lower than the vitrification temperature, can quickly diffuse at the temperature higher than the vitrification temperature, greatly reduces the requirements on reaction equipment and the like, reduces the production cost and improves the market competitiveness.
Description
Technical Field
The invention relates to the technical field of optical fiber preparation, in particular to a method for preparing a gradient plastic optical fiber by a co-extrusion physical doping method.
Background
Plastic Optical Fibers (POFs), also known as Polymer Optical fibers (Polymer Optical fibers), have a high refractive index polymeric optically transparent material as the core and a low refractive index polymeric optically transparent material as the cladding. The POF has the characteristics of no electromagnetic interference and radiation, strong anti-interference capability, strong reliability and confidentiality, light weight, flexibility, large core diameter, easy coupling and the like, and is widely applied to the fields of industrial control, consumer electronics, sensors, automobile industry, decorative lighting and the like.
According to the refractive index profile of the optical fiber, there are classified into a step-type (SI POF) plastic optical fiber and a gradient-type (GI POF) plastic optical fiber. Because the gradient refractive index distribution that the refractive index is gradually reduced from the fiber core to the cladding is adopted by the gradient plastic optical fiber, the modal dispersion is reduced, the problem of low bandwidth of the step plastic optical fiber is solved, and the signal transmission bandwidth can transmit 2.5Gbit/s within the range of 100 m; the gradient plastic optical fiber has high bandwidth characteristic, and can be applied to optical fiber access networks, local area networks, large-capacity data exchange centers, automobile automatic driving control and the preparation of optical devices such as polymer self-focusing lenses, collimators and the like.
The production method of the gradient plastic optical fiber at home and abroad at present mainly comprises the following steps:
1. drawing method for interface gel prefabricated rod
The interfacial gel method is that mixed liquid of MMA monomer and dopant (the refractive index of the dopant is larger than that of MMA) is filled into a PMMA tube, the PMMA tube is heated to polymerize, and at the initial stage of reaction, the mixed monomer swells the surface of the PMMA tube to form a gel layer in the PMMA tube. Due to the gel effect, the polymerization reaction mainly takes place in the gel layer, whereas due to the diffusion effect, the copolymerization reaction of the MMA monomer and the dopant takes place in the gel layer. The copolymerization reaction proceeds from the inner wall of the PMMA tube toward the tube core. In the early formed copolymer, MMA monomer is more than dopant, along with the progress of copolymerization reaction, the MMA content in the copolymer is less and less, and the dopant content is more and more, therefore, the refractive index of the produced copolymer is gradually increased to form gradient distribution, a prefabricated bar is formed after polymerization is finished, and then the rod drawing process is adopted to prepare the gradient type plastic optical fiber. The disadvantages of this method are: (1) Bubbles or vacuum bubbles are difficult to eliminate fundamentally and local opaqueness phenomenon exists; (2) It is difficult to prepare a large-diameter long-length gradient preform; (3) The polymerization reaction time is long, the production efficiency is low, and the industrial production is difficult to realize.
2. Plasma state method
Firstly preparing a polymer rod, and then replacing hydrogen or other atoms in the polymer by adopting a plasma state method process, so that the gradient change of the refractive index is formed from the surface of the polymer to the center of the polymer due to different substitution degrees. In order to ensure the low refractive index of the outer surface of the prepared gradient plastic optical fiber rod, fluorine is generally adopted for substitution. The disadvantages of this method are therefore: (1) the industrial production cost of the fluorine chemical process is high; and (2) the fluorination time is long, resulting in low production efficiency.
3. Multilayer coextrusion process
The method comprises the steps of firstly preparing optical high-transparency polymer materials with different refractive indexes, respectively melting and extruding the polymer materials with different refractive indexes through a plurality of extruders according to the distribution principle that the refractive index at the center is highest and gradually decreases along the radial direction, melting and extruding through a multi-layer co-extrusion die, and carrying out traction and stretching forming. The disadvantages of this method are: (1) The optical fiber belongs to a multi-order plastic optical fiber, the refractive index distribution is in a step shape, and the bandwidth is not as high as that of the gradient plastic optical fiber; (2) the fewer the number of layers, the lower the bandwidth; (3) Because the thickness of each layer is usually only 5-30 um, the more the number of layers is, the greater the control difficulty is, the lower the yield is, and the high-bandwidth gradient plastic optical fiber which is qualified in batch is difficult to stably produce.
In order to solve the above problems, the patent document with the application number of CN200910059259.2 discloses a method for preparing a gradient plastic optical fiber by a continuous reaction co-extrusion thermal diffusion method, which comprises adding an inert dopant with a refractive index higher than that of a main monomer as a core layer material into the main monomer, polymerizing an optical fiber core layer melt with a light transmittance of more than 93% in a pre-polymerization reaction device, sending the optical fiber core layer melt into a core layer region of a double-layer co-extrusion mold, simultaneously melting and extruding a polymer formed by polymerizing a material with the same composition as the main monomer as a cladding material into a cladding region of the double-layer co-extrusion mold, melting and compounding the two in the double-layer co-extrusion mold into a double-layer round-section optical fiber, controlling and diffusing the optical fiber into a forming region by a temperature of 100-240 ℃ after being extruded from the double-layer co-extrusion mold, and staying for 10-20 min, wherein the inert dopant is gradually diffused from a high concentration at the center to the cladding polymer along the radial direction of the optical fiber to form the gradient plastic optical fiber with a gradient distribution of high refractive index at the center and a gradually low refractive index at the periphery. In the method for preparing the gradient plastic optical fiber by the continuous reaction co-extrusion thermal diffusion method, the main monomer, the inert doping agent, the flexibility increasing modifier, the free radical initiator and the chain transfer agent are subjected to chemical reaction, so that the requirement on reaction conditions is higher, the production cost is increased, and the market competitiveness is reduced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing a gradient plastic optical fiber by a co-extrusion physical doping method, so as to solve the problem that the requirements on reaction conditions are higher due to the adoption of chemical reactions among a main monomer, an inert doping agent, a flexibility-increasing modifier, a free radical initiator and a chain transfer agent in the method for preparing the gradient plastic optical fiber by a continuous reaction co-extrusion thermal diffusion method in the prior art, so that the production cost is increased, and the market competitiveness is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for preparing a gradient plastic optical fiber by a co-extrusion physical doping method comprises the following steps:
step one, adopting a co-extrusion die to set corresponding layer areas according to the number of layers of optical fiber materials to form strip-shaped extrudates with concentric circle interfaces in a multi-layer structure;
step two, extruding the strip-shaped extrudate, and then passing the extruded strip-shaped extrudate through a thermal forming diffusion zone with the temperature of 100-240 ℃, wherein the retention time of the strip-shaped extrudate in the diffusion zone is 1-10 min;
the refractive index of the multilayer structure is gradually reduced from inside to outside to form gradient distribution, and each layer in the multilayer structure is formed by extruding the polymer physically doped with inert dopant.
Further, the multilayer structure is at least 3 layers, and the cladding layer and the rest layers in the multilayer structure adopt different types of polymers.
Further, the polymer in the clad layer in the multilayer structure is at least one of polymethyl methacrylate and fluororesin.
Further, the polymer in the clad in the multilayer structure is a fluororesin.
Further, the polymer in each layer except the clad layer in the multilayer structure is at least one of polymethyl methacrylate, polystyrene, and polycarbonate.
Further, the inert dopant includes at least one of diphenyl sulfide, bromobenzene, butyl benzyl phthalate, benzyl benzoate and biphenyl.
Further, the light transmittance of the polymethyl methacrylate is greater than 93%, and the refractive index of the polymethyl methacrylate is equal to 1.49; the light transmittance of the polystyrene is more than 92%, and the refractive index of the polystyrene is equal to 1.59; the light transmittance of the polycarbonate is more than 92%, and the refractive index of the polycarbonate is equal to 1.58.
Further, the refractive index of diphenyl sulfide is 1.633, the refractive index of bromobenzene is 1.56, the refractive index of butyl benzyl phthalate is 1.54, the refractive index of benzyl benzoate is 1.568, and the refractive index of biphenyl is 1.587.
Further, the fluororesin is a copolymer obtained by copolymerizing at least two of THV, PVDF, ETFE, and PTFE.
Further, the fluororesin is a copolymer obtained by copolymerizing THV and PVDF.
Compared with the prior art, the invention has the following beneficial effects:
1. the method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method adopts a polymer as a main monomer to physically dope an inert dopant, and the polymer is extruded by a co-extrusion die to form the gradient plastic optical fiber with the refractive index gradient distribution, wherein the refractive index gradient distribution has high central refractive index and gradually low peripheral refractive index, and the gradient plastic optical fiber is gradually diffused from the high central concentration along the radial direction of the optical fiber to the polymer direction of a cladding;
2. in the invention, the polymer and the inert doping agent are physically doped, chemical reaction is not carried out, only the small molecular substance with the refractive index is changed, the diffusion process is basically stopped at the temperature lower than the vitrification temperature, the small molecular substance can be rapidly diffused at the temperature higher than the vitrification temperature, the requirements on reaction equipment and the like are greatly reduced, the production cost is reduced, and the market competitiveness is improved.
Drawings
FIG. 1 is a schematic structural diagram of a five-layer gradient plastic optical fiber prepared in an embodiment of the present invention;
fig. 2 is a schematic view of the refractive index profile of a gradient plastic optical fiber having a five-layer structure prepared in the embodiment of the present invention.
Detailed Description
The present invention will be described in further detail below by way of specific embodiments:
the gradient plastic optical fiber prepared by the method at least comprises three layers of materials, wherein the innermost layer is the inert doping agent which is formed by physically doping a high transparent polymer with high refractive index, and the concentration of the inert doping agent is relatively high; then the second layer is also high-transparency polymer doped high-refractive index inert dopant, the concentration of the inert dopant is relatively reduced, the subsequent materials are also high-transparency polymer doped high-refractive index inert dopant, only the concentration of the inert dopant is further reduced, the last layer of high-transparency polymer is used as a cladding, and the refractive index of the last layer of high-transparency polymer is lower than that of the physically doped high polymer in the inner layer;
the polymers of each layer are melted and extruded by an extruder and converged to a co-extrusion die, the co-extrusion die is provided with corresponding layer areas according to the number of layers of optical fiber materials to form strip-shaped extruded materials with a multi-layer structure concentric circle interface, the strip-shaped extruded materials pass through a thermal forming diffusion area with the temperature of 100-240 ℃ after being extruded, the residence time of the extruded materials in the diffusion area is 1-10 min, and therefore the physically-doped high-refractive index inert doping agent is gradually diffused from the center high concentration along the radial direction of the optical fiber to the direction of the cladding polymer to form the gradient plastic optical fiber with the refractive index gradient distribution with the high center refractive index and the gradually low peripheral refractive index.
The highly transparent polymer can be a highly transparent polymer material such as polymethyl methacrylate (PMMA, light transmittance >93%, refractive index n = 1.49), polystyrene (PS, light transmittance 92%, refractive index n = 1.59), polycarbonate (PC, light transmittance >92%, refractive index n = 1.58), and the like, and PMMA with light transmittance >93% and refractive index n =1.49 is preferable in the invention.
The inert dopant diphenyl sulfide (DPS, refractive index n = 1.633), bromobenzene (BB, refractive index n = 1.56), butyl benzyl phthalate (BBP, refractive index n = 1.54), benzyl benzoate (BEN, refractive index n = 1.568), biphenyl (DP, refractive index n = 1.587), preferably bromobenzene (BB, n = 1.56).
The highly transparent polymer of the clad may be PMMA, a fluororesin, preferably a fluororesin having a refractive index at least 5% lower than that of the core layer, and a fluororesin which is a copolymer of VDF, TFE, HFP such as THV, PVDF, ETFE, PTFE, further preferably THV and PVDF.
The refractive index dopant of the invention is an inert dopant with the refractive index larger than that of a high transparent polymer, and is characterized in that the dopant does not react with a main material, only small molecular substances with the refractive index are changed, the diffusion process is basically stopped at the temperature lower than the glass transition temperature, and the dopant can be rapidly diffused at the temperature higher than the glass transition temperature.
The gradient plastic optical fiber at least comprises three layers of materials, and preferably adopts a five-layer structure in order to ensure that a production line and a co-extrusion die are relatively simple and the refractive index gradient distribution is closer to a parabolic curve.
The five-layer structure material comprises the following components:
the PMMA material is doped with an inert dopant BB, is fully mixed after being proportioned according to a corresponding proportion by adopting a physical doping mode, and is added into a hopper of an extruder.
The PMMA and the fluororesin are dried for more than 4 hours.
The inert dopant BB described above requires purification processes such as water washing, distillation, etc. to remove impurities and bromine.
The five-component polymer material is melted and extruded by an extruder to be converged into a five-layer co-extrusion die, and the co-extrusion die is provided with five layer regions to form a strip-shaped extrudate with a concentric circle interface of a five-layer structure.
The above-mentioned polymeric materials of layers 1 to 3 are further melt physically mixed in an extruder.
And thirdly, after the polymer is extruded from the five-layer co-extrusion die, the outer diameter of the five-layer polymer is gradually reduced from large to small through a diffusion area with controllable temperature, meanwhile, the refractive index is gradually diffused along with the temperature from inside to outside, and finally, the polymer is shaped, drawn and wound on a disc to complete the production.
The temperature of the polymer in the temperature-controllable diffusion zone is controlled to be 100-240 ℃, preferably 120-180 ℃, and the retention time is 1-10 min, preferably 5min, so as to ensure the time required by the diffusion of the dopant and ensure certain production efficiency. Because the concentration of the inert dopant in the center of the extrudate is the highest, according to the principle of thermal diffusion, the dopant small molecules with high refractive index diffuse from the high concentration region to the low concentration region until the optical fiber cools, and the diffusion process stops. By diffusion, the dopant concentration forms a gradient-type profile. If the inert dopant BB is added at 15% as in the present invention, a polymer with a central refractive index of at most 1.50 can be obtained, and with the decrease of the inert dopant BB addition of the subsequent layers and the influence of thermal diffusion, the dopant diffuses inward and outward in the radial direction of the concentric circle cross section in the extrudate, and the concentration of the dopant BB is decreased from 15% to 0%, and the corresponding refractive index is decreased from 1.50 to 1.49, then to 1.42, and finally to 1.35, so as to form a gradient distribution of the refractive index, which is close to a quadratic parabolic distribution. The bandwidth of the fiber with the gradient-type distribution of the refractive index can exceed 1GHz 100m. In addition, the rolled optical fiber can be placed into an oven with the temperature of more than 80 ℃ for constant-temperature curing for a certain time, so that the diffusion of the inert dopant is further enhanced, the gradient distribution of the refractive index is optimized, the refractive index is closer to the quadratic parabolic distribution, and the bandwidth is maximized.
The PMMA material with the light transmittance of 93 percent is selected and dried, and the inert dopant BB is also subjected to purification processes such as washing, distillation and the like, so that the entering of impurities is reduced to the maximum extent, the loss of the produced gradient plastic optical fiber is less than 0.3dB/m, and the gradient plastic optical fiber can be used for high-bandwidth short-distance communication application.
The method of the invention can be used for continuous and stable mass production, has high production efficiency, simple and convenient production and lower production cost.
The gradient plastic optical fiber with a five-layer structure is prepared as shown in fig. 1, and the specific material formula of each layer of material is as follows:
and drying the PMMA and the fluororesin for at least more than 4 hours by using a vacuum oven, fully removing the water in the material, and simultaneously purifying and filtering the inert doping agent bromobenzene BB by adopting reduced pressure distillation so as to ensure that the purity of the BB reaches more than 99.99 percent. Then the raw materials are proportioned according to the proportion of each component, the mixture is added into a hopper of each extruder after being fully mixed, each extruder is set with a proper production temperature to ensure that the mixed polymer is fully melted and plasticized, the extrudate of each extruder is converged into a five-layer co-extrusion die, the co-extrusion die is provided with five layer regions to form a strip extrudate of a five-layer structure concentric circle interface, the strip extrudate passes through a temperature control diffusion forming region to enable an optical fiber to stay for 5min, the refractive index is distributed from the center 1.497 to 1.49, then to 1.42, and finally to the edge 1.365 in a gradient mode (the distribution of the specific refractive index is shown in figure 2), and the optical fiber is drawn and stretched into a diameter of 0.75mm and then wound on a disc. The temperature of the temperature control diffusion forming area is controlled in three sections, namely 180 ℃, 150 ℃ and 120 ℃. And finally, placing the coiled optical fiber into an oven at 80 ℃ for constant temperature treatment for 30min to further form refractive index gradient diffusion, thus preparing a high-bandwidth gradient plastic optical fiber product. The production line can continuously produce for 24 hours, and greatly improves the production efficiency.
The main indexes of the gradient plastic optical fiber produced by the method are as follows:
loss: <0.25dB/m @650nm
Outer diameter: phi 0.75mm
Diameter fluctuation: plus or minus 6 percent
Maximum numerical aperture: 0.16
Theoretical bandwidth: 1GHz 100m
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. A method for preparing a gradient plastic optical fiber by a co-extrusion physical doping method is characterized by comprising the following steps:
step one, adopting a co-extrusion die to set corresponding layer areas according to the number of layers of optical fiber materials to form strip-shaped extrudates with concentric circle interfaces in a multi-layer structure;
step two, extruding the strip-shaped extrudate, and then passing the extruded strip-shaped extrudate through a thermal forming diffusion zone with the temperature of 100-240 ℃, wherein the retention time of the strip-shaped extrudate in the diffusion zone is 1-10 min;
the refractive index of the multilayer structure is gradually reduced from inside to outside to form gradient distribution, and each layer in the multilayer structure is formed by extruding the polymer physically doped with inert dopant.
2. The method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method according to claim 1, which is characterized in that: the multilayer structure has at least 3 layers, and the cladding layer and the rest layers in the multilayer structure adopt different types of polymers.
3. The method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method according to claim 2, characterized in that: the polymer in the cladding in the multilayer structure is at least one of polymethyl methacrylate and fluororesin.
4. The method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method according to claim 3, wherein the method comprises the following steps: the polymer in the cladding in the multilayer structure is a fluororesin.
5. The method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method according to claim 2, characterized in that: the polymer in each layer except the cladding layer in the multilayer structure is at least one of polymethyl methacrylate, polystyrene and polycarbonate.
6. The method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method according to claim 1, which is characterized in that: the inert dopant includes at least one of diphenyl sulfide, bromobenzene, butyl benzyl phthalate, benzyl benzoate and biphenyl.
7. The method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method according to claim 5, wherein the method comprises the following steps: the light transmittance of the polymethyl methacrylate is greater than 93%, and the refractive index of the polymethyl methacrylate is equal to 1.49; the light transmittance of the polystyrene is more than 92%, and the refractive index of the polystyrene is equal to 1.59; the light transmittance of the polycarbonate is more than 92%, and the refractive index of the polycarbonate is equal to 1.58.
8. The method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method according to claim 6, wherein the method comprises the following steps: the refractive index of diphenyl sulfide is 1.633, the refractive index of bromobenzene is 1.56, the refractive index of butyl benzyl phthalate is 1.54, the refractive index of benzyl benzoate is 1.568, and the refractive index of biphenyl is 1.587.
9. The method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method according to claim 4, wherein the method comprises the following steps: the fluororesin is a copolymer formed by copolymerizing at least two of THV, PVDF, ETFE and PTFE.
10. The method for preparing the gradient plastic optical fiber by the co-extrusion physical doping method according to claim 9, wherein the method comprises the following steps: the fluororesin is a copolymer formed by copolymerizing THV and PVDF.
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