Modified inorganic glue and preparation method thereof, and rod assembling device of hollow-core optical fiber preform rod

Abstract

The invention provides a modified inorganic adhesive, a preparation method thereof and a rod assembling device of a hollow-core optical fiber preform rod, and the preparation method comprises the following steps: S1, uniformly mixing a solution and a two-component soluble silicate material according to a weight ratio of 1: (1-2) to obtain a solution A; s2, adding 3-5wt% of an organosilane coupling agent into the solution A for reaction to obtain a solution B; s3, standing the solution B at normal temperature for 4-6 hours to obtain modified inorganic glue; the process is simple, a modified inorganic adhesive preparation method with the synergistic effect of a two-component soluble silicate material and an organic silane coupling agent is adopted, and the purpose of improving the hydrophobicity and bonding strength of the adhesive is achieved by optimizing the composition and the preparation process of the adhesive, tight bonding between an optical fiber nested tube and a sleeve is achieved, falling is not prone to occurring, and the service life of the optical fiber nested tube is prolonged. The actual requirements in the preparation and subsequent treatment processes of the hollow-core optical fiber preform are met, and the production cost is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of hollow fiber preforms, and particularly to a modified inorganic adhesive, a preparation method thereof, and an assembly device for hollow fiber preforms. Background Art

[0002] With the rapid development of optical fiber communication and optical fiber sensing technologies, hollow fibers, as an innovative type of optical fiber, have demonstrated extraordinary potential in multiple fields such as optical signal transmission and optical fiber sensing, relying on their unique transmission performance and application value. Hollow fibers, as a new type of optical fiber structure, can better meet the growing high-performance requirements compared to traditional solid-core fibers. Among them, hollow photonic bandgap fibers and hollow anti-resonant fibers are particularly remarkable. Especially for hollow anti-resonant fibers, their uniqueness lies in the use of the anti-resonant effect and the suppression of coupling between the cladding and core modes to confine a large amount of optical power in the hollow core for transmission. This special structure endows it with excellent optical properties.

[0003] However, in the production and processing process of hollow fibers, especially in the preparation and subsequent processing stages of hollow fiber preforms, the problem of tight bonding between the fiber embedding sleeve and the sleeve has become a technical bottleneck that urgently needs to be overcome. Traditional inorganic adhesives, such as single-component silicate adhesives, although can complete the bonding between fiber sleeves to a certain extent, their bonding strength is often unsatisfactory. During long-term use and transportation, these adhesives are prone to phenomena such as colloid shedding or cracking, thus seriously affecting the performance stability and service life of hollow fibers.

[0004] In addition, traditional inorganic adhesives have poor hydrophobicity and are easily affected by environmental humidity, resulting in a decline in colloid performance, further exacerbating the problem of loose bonding between fiber sleeves. This not only affects the transmission efficiency of hollow fibers but also increases the risk of damage during transportation and use.

[0005] To address these challenges, the industry has started actively seeking the use of modified inorganic adhesives to improve the bonding strength and hydrophobicity between fiber sleeves. However, unfortunately, most of the existing modified inorganic adhesives adopt single modification means, such as adding organic resins or inorganic nanoparticles, etc. Although the performance of the adhesives has been improved to a certain extent, there are often deficiencies such as limited modification effect, high cost, or cumbersome preparation process.

[0006] The disclosure of the above background art content is only used to assist in understanding the inventive concept and technical solution of the present invention, and it does not necessarily belong to the prior art of this patent application, nor does it necessarily provide technical guidance; without clear evidence indicating that the above content was publicly available before the filing date of this patent application, the above background art should not be used to evaluate the novelty and inventiveness of this application. Summary of the Invention

[0007] In order to solve technical problems such as how to have both high-intensity bonding force and good hydrophobicity in modified inorganic adhesives, etc., the present invention proposes a modified inorganic adhesive and its preparation method, and a rod-assembling device for a hollow optical fiber preform. Its process is simple. A preparation method of a modified inorganic adhesive using the synergistic effect of a two-component soluble silicate material and an organosilane coupling agent is adopted. The aim is to optimize the composition and preparation process of the adhesive, improve the hydrophobicity and bonding strength of the adhesive, achieve tight bonding between the optical fiber embedding sleeve and the sleeve, which is not easy to fall off, meet the actual requirements in the preparation and subsequent processing of the hollow optical fiber preform, and reduce the production cost.

[0008] In order to achieve the above object, the technical solution of the present invention is as follows:

[0009] The present invention provides a preparation method of a modified inorganic adhesive, including the following steps:

[0010] S1 Mix the solution and the two-component soluble silicate material evenly according to a weight ratio of 1:(1-2) to obtain solution A;

[0011] S2 Add 3-5 wt% of an organosilane coupling agent to solution A for reaction to obtain solution B;

[0012] S3 Let solution B stand at room temperature for 4-6 h to obtain the modified inorganic adhesive.

[0013] The present invention proposes a modified inorganic adhesive and its preparation method, and a rod-assembling device for a hollow optical fiber preform. Its process is simple. A preparation method of a modified inorganic adhesive using the synergistic effect of a two-component soluble silicate material and an organosilane coupling agent is adopted. The aim is to optimize the composition and preparation process of the adhesive, improve the hydrophobicity and bonding strength of the adhesive, achieve tight bonding between the optical fiber embedding sleeve and the sleeve, which is not easy to fall off, meet the actual requirements in the preparation and subsequent processing of the hollow optical fiber preform, and reduce the production cost.

[0014] As a preferred technical solution, the two-component soluble silicate material includes: sodium silicate and alumina, and the weight ratio of sodium silicate to alumina is 3:1.

[0015] As a preferred technical solution, the organosilane coupling agent is γ-aminopropyltriethoxysilane or methyltriethoxysilane.

[0016] As a preferred technical solution, in step S2, 3-5 wt% of an organosilane coupling agent is added to solution A and stirred at room temperature for 5-8 h for reaction, and the stirring speed is 450-550 r / min.

[0017] The present invention also provides a modified inorganic adhesive prepared according to the preparation method of the modified inorganic adhesive described in any one of the above.

[0018] The present invention also provides a method for assembling a hollow fiber preform, including: the modified inorganic glue as described above and several fiber embedding sleeves. The several fiber embedding sleeves are assembled into a rod by the modified inorganic glue. The modified inorganic glue is evenly coated on the outer surface of the fiber embedding sleeve to form a modified inorganic glue layer. The fiber embedding sleeve is bonded to the quartz glass part and the sleeve through the modified inorganic glue layer respectively.

[0019] As a preferred technical solution, at least 5 fiber embedding sleeves are provided. The fiber embedding sleeve has a double nested structure. The sleeve is arranged outside the fiber embedding sleeve. The sleeve is connected to a rotary fixator. The quartz glass part includes: a quartz glass tube and multiple quartz glass sheets. The quartz glass sheets are evenly arranged on the outer circumference of the quartz glass tube and connected to the quartz glass tube. The quartz glass sheets are arranged between every two adjacent fiber embedding sleeves. The fiber embedding sleeve is correspondingly arranged with a rotatable syringe. The infrared sensor is correspondingly arranged with the fiber embedding sleeve.

[0020] As a preferred technical solution, several fiber embedding sleeves are assembled into a rod by the modified inorganic glue, specifically including the following steps:

[0021] S1 Assemble several fiber embedding sleeves in a sleeve, and fix the positions of the internal fiber embedding sleeves with the help of a quartz glass part;

[0022] S2 Load the modified inorganic glue into a rotatable syringe. The rotation speed of the fiber embedding sleeve is adapted to the rotation speed of the rotatable syringe. The rotatable syringe is positioned by the infrared sensor, and the fiber embedding sleeve is spin-coated to form a modified inorganic glue coating;

[0023] S3 After bonding both ends of the preform with the modified inorganic glue coating, let it stand at room temperature for 23 - 25h, then dry it at 75 - 85°C for 2 - 3h, and naturally cool down to room temperature to obtain a hollow fiber preform.

[0024] As a preferred technical solution, in step S2, the rotatable syringe rotates counterclockwise or clockwise along the tube wall of the fiber embedding sleeve to coat the end face of the fiber embedding sleeve. The injection speed of the rotatable syringe is 0.4 - 0.6 mL / min, the rotation speed of the rotatable syringe is 4 - 6 r / min, and the rotation speed of the embedding sleeve is 1 - 3 r / min.

[0025] As a preferred technical solution, the thickness of the modified inorganic glue coating is 0.5 - 1 mm.

[0026] A modified inorganic glue, its preparation method, and an assembling device for a hollow fiber preform provided by the present invention have the following beneficial effects:

[0027] 1) Its process is simple. It is a method for preparing a modified inorganic adhesive by the synergistic action of a two-component soluble silicate material and an organosilane coupling agent. The aim is to optimize the composition and preparation process of the adhesive, improve the hydrophobicity and bonding strength of the adhesive, achieve tight bonding between the fiber optic embedding sleeve and the sleeve, which is not easy to fall off, meet the actual requirements in the preparation and subsequent processing of the hollow fiber preform, and reduce the production cost;

[0028] 2) Organosilane coupling agents (such as γ-aminopropyltriethoxysilane or methyltriethoxysilane) play a key synergistic role in the two-component soluble silicate material. These coupling agent molecules contain hydrolyzable silyl groups and organic functional groups, which can form good bonds with both inorganic and organic materials. During the hydrolysis process, the organosilane coupling agent releases silanol groups (Si-OH). These silanol groups can undergo condensation reactions with the inorganic components in the aluminosilicate adhesive and the hydroxyl groups on the surfaces of the fiber optic embedding sleeve and the sleeve, forming chemical bonds. This chemical bonding significantly enhances the bonding strength between the adhesive and the substrate;

[0029] During the curing process of the colloid, the silicon atoms in the organosilane coupling agent combine with oxygen atoms to form silicon-oxygen bonds (Si-O-Si). These silicon-oxygen bonds not only enhance the density of the aluminosilicate network but also improve the strength and durability of the adhesive. At the same time, the formation of silicon-oxygen bonds helps to improve the hydrophobic properties of the adhesive, enabling it to better resist the erosion of moisture and humid environments; the organosilane coupling agent, as a "molecular bridge", connects inorganic materials (such as the aluminosilicate adhesive and the inorganic layers on the surfaces of the fiber optic embedding sleeve and the sleeve) with organic materials (such as the organic components in the adhesive and the organic coating inside the fiber optic sleeve). Through chemical bonding, the silane coupling agent significantly improves the interfacial bonding strength between the inorganic matrix and the adhesive, making the connection between the two more firm and stable; due to the hydrophobic nature of the silicon-oxygen bond, the adhesive containing silicon-oxygen bonds exhibits excellent hydrophobic properties. This hydrophobic property helps prevent moisture from penetrating into the adhesive, thus protecting the connection between the fiber optic embedding sleeve and the sleeve from damage. In a humid environment, the hydrophobic adhesive can maintain its performance and stability, ensuring the normal operation of the fiber optic communication system.

[0030] 3) In the solution, sodium silicate ionizes to produce silicate ions, and alumina is partially dissolved or exists in the form of its particles, providing aluminum ions. The silicate ions and aluminum ions undergo a chemical reaction to form a silicoaluminate complex. The silicoaluminate complexes are connected together through shared oxygen atom bridges to form a three-dimensional framework structure. The weight ratio of sodium silicate to alumina is 3:1. This ratio is selected based on the requirements of the chemical reaction and the optimization of the properties of the inorganic glue. Through an appropriate ratio, it can ensure that sodium silicate and alumina react fully to form a stronger inorganic silicoaluminate network structure. This network structure is composed of silicon-oxygen tetrahedrons and aluminum-oxygen tetrahedrons, which are interconnected through oxygen atom bridges to form a strong inorganic silicoaluminate network structure. The strong inorganic silicoaluminate network structure endows the modified inorganic glue with high strength, enabling it to withstand large stresses and environmental changes. The inorganic silicoaluminate network structure has excellent chemical stability and thermal stability and can maintain stable performance in high-temperature, humid, or corrosive environments. The silicon-oxygen bonds and aluminum-oxygen bonds in the inorganic silicoaluminate network structure can form good bonds with a variety of substrates and are suitable for the bonding and sealing of various materials.

[0031] 4) Both γ-aminopropyltriethoxysilane and methyltriethoxysilane are organosilane reagents with a bifunctional group structure. Their R parts can react with the active groups in the organic polymer to form covalent bonds. After the X part hydrolyzes, it forms silanol groups, which can undergo a condensation reaction with the hydroxyl groups on the surface of the inorganic material to form strong chemical bonds. This property enables the organosilane coupling agent to act as a bridge between organic and inorganic materials, significantly improving the bonding and mechanical properties of the materials.

[0032] 5) The modified inorganic glue is uniformly coated on the outer surface of the optical fiber ferrule tube, forming a strong modified inorganic glue layer. This modified inorganic glue layer not only firmly bonds the individual optical fiber ferrule tubes together but also ensures a stable and durable connection between them. This stable connection helps reduce signal attenuation during the transmission of optical fibers and improves the transmission performance of the optical fibers. Through the modified inorganic glue layer, a tight bond is formed between the optical fiber ferrule tube and the quartz glass part and the sleeve. This tight bond not only enhances the overall strength of the optical fiber preform but also enables it to better resist external environmental interference and damage. For example, during the preparation and subsequent processing of the optical fiber preform, this enhanced strength helps prevent deformation or fracture of the optical fiber ferrule tube due to uneven stress. The quartz glass part is arranged between every two adjacent optical fiber ferrule tubes, playing a role of isolation and protection, while the sleeve is arranged outside the optical fiber ferrule tube, providing not only additional protection but also facilitating the installation and fixation of the optical fiber preform. This structural design helps optimize the performance of the optical fiber preform and makes it more adaptable to the requirements of various application scenarios.

[0033] 6) The optical fiber embedding sleeve adopts a double-nested structure, which further enhances its stability within the sleeve and improves the overall mechanical strength;

[0034] The infrared sensor is arranged corresponding to the optical fiber embedding sleeve, ensuring that the rotatable syringe can precisely coat the end face of the optical fiber embedding sleeve. The application of this technology improves production efficiency and ensures the stability of coating quality;

[0035] The rotation speed of the embedding sleeve is adapted to the rotation speed of the rotatable syringe, ensuring the smooth progress of the coating process. This adaptability design reduces the failure rate during production and improves the overall production efficiency. Description of the Drawings

[0036] Figure 1 It is a schematic structural diagram of the rod assembling device for the hollow optical fiber preform provided by the present invention;

[0037] Figure 2 It is a schematic cross-sectional structure diagram of the hollow optical fiber preform;

[0038] Figure 3 It is a schematic cross-sectional structure diagram of the quartz glass part;

[0039] Figure 4 It is a flowchart of the rod assembling process of the rod assembling device for the hollow optical fiber preform;

[0040] Among them: 1 - optical fiber embedding sleeve; 2 - sleeve; 3 - modified inorganic glue layer; 4 - quartz glass part; 41 - quartz glass tube; 42 - quartz glass sheet; 5 - rotation fixator; 6 - infrared sensor; 7 - rotatable syringe; 8 - syringe rotation fixator. Detailed Embodiment

[0041] The preferred embodiments of the present invention will be described in detail below with reference to the drawings.

[0042] As Figure 3 shown, the present invention provides a preparation method for a modified inorganic glue, including the following steps:

[0043] S1 Mix the solution and the two-component soluble silicate material evenly according to a weight ratio of 1:(1 - 2) to obtain solution A;

[0044] S2 Add 3 - 5wt% of the organosilane coupling agent to solution A for reaction to obtain solution B;

[0045] S3 Let solution B stand at room temperature for 4 - 6h to obtain the modified inorganic glue.

[0046] The present invention provides a modified inorganic adhesive, a preparation method thereof, and an assembly device for a hollow fiber preform. The process is simple. The modified inorganic adhesive is prepared by the synergistic effect of a two-component soluble silicate material and an organosilane coupling agent. The aim is to optimize the composition and preparation process of the adhesive to improve the hydrophobicity and bonding strength of the adhesive, achieve tight bonding between the fiber embedding sleeve and the sleeve, which is not easy to fall off, meet the actual requirements in the preparation and subsequent processing of the hollow fiber preform, and reduce the production cost.

[0047] Organosilane coupling agents (such as γ-aminopropyltriethoxysilane or methyltriethoxysilane) play a key synergistic role in the two-component soluble silicate material. These coupling agent molecules contain hydrolyzable silyl groups and organic functional groups, and can form good bonds with both inorganic materials and organic materials. During the hydrolysis process of the organosilane coupling agent, silanol groups (Si-OH) are released. These silanol groups can undergo condensation reactions with the inorganic components in the aluminosilicate adhesive and the hydroxyl groups on the surfaces of the fiber embedding sleeve and the sleeve to form chemical bonds. This chemical bonding significantly enhances the bonding strength between the adhesive and the substrate.

[0048] During the curing process of the colloid, the silicon atoms in the organosilane coupling agent combine with oxygen atoms to form silicon-oxygen bonds (Si-O-Si). These silicon-oxygen bonds not only enhance the density of the aluminosilicate network but also improve the strength and durability of the adhesive. At the same time, the formation of silicon-oxygen bonds helps to improve the hydrophobic properties of the adhesive, enabling it to better resist the erosion of moisture and humid environments. The organosilane coupling agent, as a "molecular bridge", connects inorganic materials (such as aluminosilicate adhesives and the inorganic layers on the surfaces of the fiber embedding sleeve and the sleeve) and organic materials (such as the organic components in the adhesive and the organic coating inside the fiber sleeve). Through chemical bonding, the silane coupling agent significantly improves the interfacial bonding strength between the inorganic matrix and the adhesive, making the connection between the two more firm and stable. Due to the hydrophobic nature of the silicon-oxygen bond, the adhesive containing silicon-oxygen bonds exhibits excellent hydrophobic properties. This hydrophobic property helps prevent moisture from penetrating into the adhesive, thereby protecting the connection between the fiber embedding sleeve and the sleeve from damage. In a humid environment, the hydrophobic adhesive can maintain its performance and stability, ensuring the normal operation of the optical fiber communication system.

[0049] Preferably, the two-component soluble silicate material includes sodium silicate and alumina, and the weight ratio of sodium silicate to alumina is 3:1.

[0050] Preferably, the organosilane coupling agent is γ-aminopropyltriethoxysilane or methyltriethoxysilane.

[0051] Preferably, in step S2, 3-5 wt% of an organosilane coupling agent is added to solution A and stirred at room temperature for 5-8 h. The stirring speed is 450-550 r / min. The weight percentages of the organosilane coupling agent added to solution A in step S2 are preferably 3 wt%, 4 wt%, and 5 wt%. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the above range. The reaction time of stirring at room temperature is preferably 5 h, 6 h, 7 h, and 8 h. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the above range. The stirring speed is preferably 450 r / min, 500 r / min, and 550 r / min. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the above range. By adjusting the stirring speed and reaction time, the hydrolysis and condensation reaction rates of the organosilane coupling agent can be controlled. An appropriate reaction rate helps to obtain an ideal bonding effect and material properties. Reacting at room temperature avoids the use of extreme conditions such as high temperature or high pressure, thereby reducing energy consumption and production costs.

[0052] As Figure 1-2 shown, the present invention also provides a method for assembling a hollow fiber preform, including: the modified inorganic glue as described above and several fiber embedding tubes 1. The several fiber embedding tubes 1 are assembled into a rod by the modified inorganic glue. The modified inorganic glue is uniformly coated on the outer surface of the fiber embedding tube 1 to form a modified inorganic glue layer 3. The fiber embedding tube 1 is bonded to the quartz glass part 4 and the sleeve 2 respectively through the modified inorganic glue layer 3.

[0053] Preferably, as Figure 1-2 shown, at least 5 fiber embedding tubes 1 are provided. The fiber embedding tube 1 is a double-nested structure. The sleeve 2 is arranged outside the fiber embedding tube 1. The sleeve 2 is connected to the rotary fixator 5. The quartz glass part 4 is arranged between every two adjacent fiber embedding tubes 1. The fiber embedding tube 1 is correspondingly arranged with the rotatable syringe 7. The infrared sensor 6 is correspondingly arranged with the fiber embedding tube 1.

[0054] Preferably, as Figure 3 shown, several fiber embedding tubes 1 are assembled into a rod by the modified inorganic glue, specifically including the following steps:

[0055] S1 Assemble several fiber embedding tubes 1 in a sleeve 2 and fix the positions of the internal fiber embedding tubes 1 with the help of the quartz glass part 4;

[0056] S2 Load the modified inorganic glue into the rotatable syringe 7. The rotation speed of the fiber embedding tube 1 is adapted to the rotation speed of the rotatable syringe 7. The rotatable syringe 7 is positioned by the infrared sensor 6, and the fiber embedding tube 1 is spin-coated to form a modified inorganic glue coating 3;

[0057] After both ends of the preform are bonded with the modified inorganic glue coating 3, it is left standing at room temperature for 23 - 25 h, then dried at 75 - 85 °C for 2 - 3 h, and naturally cooled to room temperature to obtain a hollow fiber preform.

[0058] In step S3, the standing time at room temperature is preferably 23 h, 24 h, and 25 h. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the said range. The drying temperature is preferably 75 °C, 80 °C, and 85 °C. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the said range. The drying holding time is 2 h and 3 h. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the said range.

[0059] Preferably, in step S2, the syringe rotary fixer 8 drives the rotatable syringe 7 to rotate counterclockwise or clockwise along the tube wall of the optical fiber embedding tube 1 to perform coating treatment on the end face of the optical fiber embedding tube 1. The injection speed of the rotatable syringe 7 is 0.4 - 0.6 mL / min. The injection speed of the rotatable syringe 7 is preferably 0.4 mL / min, 0.5 mL / min, and 0.6 mL / min. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the said range. The rotation speed of the rotatable syringe 7 is 4 - 6 r / min. The rotation speed of the rotatable syringe 7 is preferably 4 r / min, 5 r / min, and 6 r / min. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the said range. The rotation speed of the optical fiber embedding tube 1 is 1 - 3 r / min. The rotation speed of the optical fiber embedding tube 1 is preferably 1 r / min, 2 r / min, and 3 r / min. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the said range.

[0060] Preferably, the thickness of the modified inorganic glue coating 3 is 0.5 - 1 mm. The thickness of the modified inorganic glue coating 3 is preferably 0.5 mm and 1 mm. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the said range.

[0061] Example 1

[0062] The present invention provides a preparation method of a modified inorganic glue, including the following steps:

[0063] S1 Mix the sodium silicate and the aluminum oxide in a weight ratio of 3:1 to obtain a two-component soluble silicate material;

[0064] S2 Mix the solution and the two-component soluble silicate material evenly in a weight ratio of 1:1 to obtain solution A;

[0065] In S2, 3 wt% of γ-aminopropyltriethoxysilane was added to Solution A and stirred at room temperature for 5 h at a stirring speed of 500 r / min to obtain Solution B;

[0066] In S3, Solution B was left standing at normal temperature for 5 h to obtain the modified inorganic glue;

[0067] The modified inorganic glue prepared by Step S3 was used to form a rod with several optical fiber jacket tubes 1, which specifically included the following steps:

[0068] In S4, several optical fiber jacket tubes 1 were assembled inside a sleeve 2, and the internal optical fiber jacket tubes 1 were fixed in position with the aid of a quartz glass part 4 to ensure that the optical fiber jacket tubes 1 were arranged evenly and stably;

[0069] In S5, the modified inorganic glue was loaded into a rotatable syringe 7. The rotation speed of the optical fiber jacket tube 1 was adapted to the rotation speed of the rotatable syringe 7. The rotatable syringe 7 was positioned by an infrared sensor 6. The angle and position of the optical fiber jacket tube 1 to be coated were adjusted at a speed of 2 r / min by a rotary fixator 5. The syringe rotary fixator 8 drove the rotatable syringe 7 to rotate clockwise along the tube wall of the optical fiber jacket tube 1, and the optical fiber jacket tube 1 was spin-coated at an injection speed of 0.5 mL / min to form a uniform modified inorganic glue coating 3 with a thickness of 0.5 mm;

[0070] In S6, after both ends of the preform were bonded with the modified inorganic glue coating 3, it was left standing at normal temperature for 24 h, then dried at 80 °C for 2 h, and naturally cooled to room temperature to obtain a hollow-core optical fiber preform.

[0071] Example 2

[0072] The present invention provides a method for preparing a modified inorganic glue, which includes the following steps:

[0073] In S1, the sodium silicate and the aluminum oxide were mixed according to a weight ratio of 3:1 to obtain a two-component soluble silicate material;

[0074] In S2, the solution and the two-component soluble silicate material were mixed evenly according to a weight ratio of 1:1 to obtain Solution A;

[0075] In S2, 5 wt% of methyltriethoxysilane was added to Solution A and stirred at room temperature for 5 h at a stirring speed of 500 r / min to obtain Solution B;

[0076] In S3, Solution B was left standing at normal temperature for 5 h to obtain the modified inorganic glue;

[0077] The modified inorganic glue prepared by adopting Step S3 is used to assemble a plurality of optical fiber sheaths 1 into a rod, which specifically includes the following steps:

[0078] S4 Assemble a plurality of optical fiber sheaths 1 in a sleeve 2, and fix the positions of the internal optical fiber sheaths 1 by means of a quartz glass part 4 to ensure that the optical fiber sheaths 1 are arranged evenly and stably;

[0079] S5 Load the modified inorganic glue into a rotatable syringe 7. The rotation speed of the optical fiber sheath 1 is adapted to the rotation speed of the rotatable syringe 7. The rotatable syringe 7 is positioned by an infrared sensor 6, and the angle and position of the optical fiber sheath 1 to be coated are adjusted at a speed of 2 r / min through a rotation fixator. The syringe rotation fixator 8 drives the rotatable syringe 7 to rotate clockwise along the tube wall of the optical fiber sheath 1, and the optical fiber sheath 1 is spin-coated at an injection speed of 0.5 mL / min to form a uniform modified inorganic glue coating 3, and the thickness of the modified inorganic glue coating 3 is 0.5 mm;

[0080] S6 After bonding both ends of the preform with the modified inorganic glue coating 3, leave it standing at room temperature for 24 h, then dry it at 80 °C for 2 h, and naturally cool it to room temperature to obtain a hollow-core optical fiber preform.

[0081] Example 3

[0082] The present invention provides a preparation method of a modified inorganic glue, which includes the following steps:

[0083] S1 Mix the sodium silicate and the aluminum oxide according to a weight ratio of 3:1 to obtain a two-component soluble silicate material;

[0084] S2 Mix the solution and the two-component soluble silicate material evenly according to a weight ratio of 1:1 to obtain Solution A;

[0085] S2 Add 4 wt% methyltriethoxysilane to Solution A and stir at room temperature for 5 h for reaction, and the stirring speed is 500 r / min to obtain Solution B;

[0086] S3 Leave Solution B standing at room temperature for 5 h to obtain the modified inorganic glue;

[0087] The modified inorganic glue prepared by adopting Step S3 is used to assemble a plurality of optical fiber sheaths 1 into a rod, which specifically includes the following steps:

[0088] S4 Assemble a plurality of optical fiber sheaths 1 in a sleeve 2, and fix the positions of the internal optical fiber sheaths 1 by means of a quartz glass part 4 to ensure that the sheaths are arranged evenly and stably;

[0089] S5 Load the modified inorganic glue into the rotatable syringe 7. The rotation speed of the optical fiber jacket 1 is adapted to that of the rotatable syringe 7. The rotatable syringe 7 is positioned by the infrared sensor 6. The angle and position of the optical fiber jacket 1 to be coated are adjusted at a speed of 2 r / min by the rotation fixer 5. The syringe rotation fixer 8 drives the rotatable syringe 7 to rotate clockwise along the wall of the optical fiber jacket 1, and the optical fiber jacket 1 is spin-coated at an injection speed of 0.5 mL / min to form a uniform modified inorganic glue coating 3 with a thickness of 0.5 mm.

[0090] S6 After bonding both ends of the preform with the modified inorganic glue coating 3, let it stand at room temperature for 24 h, then dry it at 80 °C for 2 h, and naturally cool it to room temperature to obtain a hollow-core optical fiber preform.

[0091] Comparative Example 1

[0092] Comparative Example 1 provides a preparation method of a modified inorganic glue, including the following steps:

[0093] S1 Mix the sodium silicate and the aluminum oxide in a weight ratio of 3:1 to obtain a two-component soluble silicate material.

[0094] S2 Mix the solution and the two-component soluble silicate material evenly in a weight ratio of 1:1 to obtain Solution A.

[0095] S3 Let Solution A stand at room temperature for 5 h to obtain the modified inorganic glue.

[0096] Use the modified inorganic glue prepared in step S3 to form a preform with several optical fiber jackets 1, specifically including the following steps:

[0097] S4 Assemble several optical fiber jackets 1 in a sleeve 2, and fix the positions of the internal optical fiber jackets 1 with the help of the quartz glass part 4 to ensure that the optical fiber jackets 1 are arranged evenly and stably.

[0098] S5 Load the modified inorganic glue into the rotatable syringe 7. The rotation speed of the optical fiber jacket 1 is adapted to that of the rotatable syringe 7. The rotatable syringe 7 is positioned by the infrared sensor 6. The angle and position of the optical fiber jacket 1 to be coated are adjusted at a speed of 2 r / min by the rotation fixer 5. The syringe rotation fixer 8 drives the rotatable syringe 7 to rotate clockwise along the wall of the optical fiber jacket 1, and the optical fiber jacket 1 is spin-coated at an injection speed of 0.5 mL / min to form a uniform modified inorganic glue coating 3 with a thickness of 0.5 mm.

[0099] After bonding both ends of the preform with a modified inorganic glue coating, it was left standing at room temperature for 24 h, then dried at 80 °C for 2 h, and naturally cooled to room temperature to obtain a hollow fiber preform.

[0100] The performance of the modified inorganic glue used for the hollow fiber preform sets provided in Examples 1 to 3 and Comparative Example 1 was tested, and the implementation means are as follows:

[0101] The surface drying time is usually detected by the observation method. The observation method is to observe the surface drying condition of the modified inorganic glue with the naked eye and record the time from the start of coating to the formation of a continuous dry film on the surface.

[0102] The tensile strength was tested using a universal material testing machine (or tensile testing machine). The modified inorganic glue sample was prepared into a specimen with standard dimensions, fixed at both ends to the fixture of the testing machine, and then stretched at a constant speed until the specimen broke. Record the maximum tensile force at the break, and calculate the tensile strength based on the cross-sectional area of the specimen. Repeat the above steps 5 times, and calculate the average value of the 5 tensile strengths, which is the tensile strength of the test result.

[0103] The elongation at break was also tested using a universal material testing machine. During the tensile strength test, record the elongation of the specimen from the original length to the break, and then calculate the percentage of the elongation to the original length, which is the elongation at break. Repeat the above steps 5 times, and calculate the average value of the 5 elongations at break, which is the elongation at break of the test result.

[0104] The modified inorganic glue sample was coated on a specific substrate and then immersed in water for 24 hours. After that, observe the bonding condition between the sample and the substrate to judge whether there is any peeling phenomenon. This test can evaluate the stability and adhesion of the modified inorganic glue in a water environment.

[0105] The performance of the modified inorganic glue used for the hollow fiber preform sets provided in Examples 1 to 3 and Comparative Example 1 was tested using the above experimental means, and the results are shown in Table 1.

[0106] Table 1 Test results of the performance of the modified inorganic glue used for the hollow fiber preform sets provided in Examples 1 to 3 and Comparative Example 1

[0107]

[0108]

[0109] As can be seen from Table 1, the modified inorganic adhesives for assembling hollow fiber preforms provided in Examples 1 to 3 of the present invention have more excellent interfacial bonding strength and hydrophobic properties compared with Comparative Example 1. The results of various performance tests show that in Examples 1 to 3, the two-component soluble silicate material was modified by adding an organosilane coupling agent, which strengthened the bonding effect of the hollow fiber preform assembly, improved the bonding strength of the adhesive, and the hydrophobicity was also improved. It has good mechanical properties and water resistance. Among them, the performance of the modified inorganic adhesive for assembling hollow fiber preforms prepared in Example 3 is the best.

[0110] It can be understood that the present invention is described by some examples. As is known to those skilled in the art, without departing from the spirit and scope of the present invention, various changes or equivalent replacements can be made to these features and examples. In addition, under the teaching of the present invention, these features and examples can be modified to adapt to specific situations and materials without departing from the spirit and scope of the present invention. Therefore, the present invention is not limited by the specific examples disclosed herein, and all changes or equivalent replacements that fall within the scope of the claims of this application. In addition, under the teaching of the present invention, these features and examples can be modified to adapt to specific situations and materials without departing from the spirit and scope of the present invention. Therefore, the present invention is not limited by the specific examples disclosed herein, and all examples that fall within the scope of the claims of this application belong to the scope protected by the present invention.

Claims

1. A method for preparing a modified inorganic glue, characterized in that: The following steps are involved: S1: uniformly mixing the solution and the two-component soluble silicate material in a weight ratio of 1:(1-2) to obtain solution A; S2: adding 3-5 wt% of an organic silane coupling agent to solution A to react and obtain solution B; S3: leaving solution B at room temperature for 4 to 6 hours to obtain a modified inorganic glue.

2. The method for preparing the modified inorganic glue according to claim 1, characterized in that: The two-component soluble silicate material includes sodium silicate and aluminum oxide, and the weight ratio of the sodium silicate to the aluminum oxide is 3:

1.

3. The method for preparing the modified inorganic glue according to claim 1, characterized in that: The organic silane coupling agent is γ-aminopropyltriethoxysilane or methyltriethoxysilane.

4. The method for preparing the modified inorganic glue according to claim 1, characterized in that: In step S2, 3-5 wt% of an organic silane coupling agent is added to solution A and stirred for 5-8 hours at room temperature at a stirring speed of 450-550 r / min.

5. A modified inorganic glue, characterized in that: The modified inorganic glue is prepared according to the preparation method of any one of claims 1-4.

6. A hollow core optical fiber preform assembly device, characterized in that: include: The modified inorganic glue and a plurality of optical fiber nested tubes as described in claim 5, wherein the plurality of optical fiber nested tubes are connected by a modified inorganic glue rod, the modified inorganic glue is evenly coated on the outer surface of the optical fiber nested tube to form a modified inorganic glue layer, and the optical fiber nested tube is bonded to the quartz glass member and the sleeve respectively through the modified inorganic glue layer.

7. The hollow core optical fiber preform assembly device according to claim 6, characterized in that: At least five optical fiber nested tubes are provided, and the optical fiber nested tubes are of a double nested structure. The sleeve is provided on the outside of the optical fiber nested tube, and the sleeve is connected to a rotating fixture. The quartz glass component includes: a quartz glass tube and a plurality of quartz glass sheets, and the quartz glass sheets are evenly provided on the outer circumference of the quartz glass tube and connected to the quartz glass tube. The quartz glass sheets are provided between every two adjacent optical fiber nested tubes, and the optical fiber nested tubes are provided corresponding to the rotatable injector, and the infrared sensor is provided corresponding to the optical fiber nested tube.

8. The hollow core optical fiber preform assembly device according to claim 6, characterized in that: A plurality of optical fiber nested tubes are assembled into rods through modified inorganic adhesive, which specifically includes the following steps: S1 assembles a plurality of optical fiber nested tubes in a sleeve, and fixes the positions of the optical fiber nested tubes inside with the help of quartz glass pieces; S2: loading the modified inorganic glue into a rotatable syringe, the rotation speed of the optical fiber nested tube is adapted to the rotation speed of the rotatable syringe, the rotatable syringe is positioned by an infrared sensor, and the optical fiber nested tube is spin-coated to form a modified inorganic glue coating; S3 uses a modified inorganic adhesive coating to bond the two ends of the preform rod, and then leaves it to stand at room temperature for 23 to 25 hours, and then keeps it at 75 to 85°C for 2 to 3 hours for drying, and naturally cools it to room temperature to obtain a hollow-core optical fiber preform rod.

9. The hollow core optical fiber preform assembly device according to claim 8, characterized in that: In step S2, the rotatable syringe rotates counterclockwise or clockwise along the wall of the optical fiber nested tube to coat the end face of the optical fiber nested tube. The injection speed of the rotatable syringe is 0.4-0.6 mL / min, the rotation speed of the rotatable syringe is 4-6 r / min, and the rotation speed of the nested tube is 1-3 r / min.

10. The hollow core optical fiber preform assembly device according to claim 8, characterized in that: The thickness of the modified inorganic adhesive coating is 0.5 to 1 mm.

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