Ceramic ferrule for core-adjustment-free ultra-low-loss high-end connector and preparation method of ceramic ferrule

Abstract

The invention discloses a preparation method of a ceramic ferrule for a core-adjustment-free ultra-low-loss high-end connector, which comprises the following steps: S1, dissolving rare earth metal alkoxide and a zirconium source in an ethanol aqueous solution, adding a hydrolysis catalyst for hydrolysis reaction, forming gel, drying and grinding to obtain rare earth modified nano zirconium oxide; s2, 5, 5 '-dioxodibenzothiophene-3, 7-diamine and benzo [1, 2-B: 3, 4-B': 5, 6-B '] trithiophene-2, 5, 8-trialdehyde are subjected to a D-A reaction, and a conductive COF organic carrier of the micro-nano structure is obtained; s3, mixing the materials with a binder and an auxiliary agent; and S4, after injection molding, degreasing, sintering and finish machining are performed to obtain the core-adjustment-free ultra-low-loss ceramic ferrule. According to the method, core-adjustment-free design is achieved, assembly is simplified, efficiency is improved, meanwhile, optical signal transmission loss is remarkably reduced, signal integrity is improved, and the low-loss and high-precision assembly requirements of a high-end connector are met.

Description

Technical Field

[0001] This invention relates to the technical field of ceramic ferrules, and more particularly to a ceramic ferrule for a high-end connector that requires no adjustment and has ultra-low loss, and its preparation method. Background Technology

[0002] In the field of high-end connectors, ceramic ferrules are key components whose performance directly affects the quality and stability of signal transmission. Traditional methods for manufacturing ceramic ferrules present numerous challenges. On the one hand, precise adjustment of the core wire position is required during assembly. This adjustment process is not only time-consuming and labor-intensive but also demands a high level of skill from operators, leading to low production efficiency. On the other hand, optical signals suffer significant losses during transmission due to surface reflection and scattering of the ferrule, as well as the inherent loss characteristics of the material itself, affecting signal integrity and transmission efficiency. Furthermore, ceramic ferrules lack sufficient thermal stability at high temperatures, making it difficult to meet the long-term stable use requirements of high-end connectors in complex environments. These problems limit the performance of ceramic ferrules in high-end applications and urgently require solutions through improved manufacturing methods. Summary of the Invention

[0003] In view of the technical problems of complex core adjustment and high loss in ceramic ferrules for high-end connectors in the existing technology, the present invention provides a method for preparing ceramic ferrules for high-end connectors with ultra-low loss and no core adjustment. It aims to solve the problems of low assembly efficiency caused by the need for precise adjustment of the core wire position during assembly of ceramic ferrules prepared by traditional methods, as well as the problems of high loss during optical signal transmission affecting signal integrity and transmission efficiency.

[0004] To achieve the above objectives, the technical solution adopted by the present invention is as follows: A method for manufacturing a ceramic ferrule for a high-end connector that requires no core adjustment and has ultra-low loss, the method comprising the following steps: S1: Rare earth metal alkoxides and zirconium sources are dissolved in an ethanol-water solution. Then, an appropriate amount of hydrolysis catalyst is slowly added under stirring. The hydrolysis reaction is then carried out at 60–80°C for 1–3 hours, followed by stirring at room temperature for 12–24 hours to promote condensation and form a gel. Finally, the gel is dried at 60–80°C for 12–24 hours and ground into powder to obtain rare earth-modified nano-zirconia. This invention, prepared via a sol-gel method, solves the problems of uneven particle size, agglomeration, and poor compatibility with the matrix that may occur in traditional nano-zirconia preparations. The introduction of rare earth metal alkoxides effectively improves the surface properties of nano-zirconia and enhances its bonding force with subsequent organic carriers and other components, thereby improving the overall mechanical properties and stability of the ceramic ferrule. Simultaneously, precisely controlled hydrolysis and condensation reaction conditions ensure uniform and fine nano-zirconia particle size, contributing to improved compactness and optical properties of the ceramic ferrule, and providing a high-quality inorganic filler base for the subsequent preparation of high-performance ceramic ferrules.

[0005] S2: 5,5'-dioxodibenzothiophene-3,7-diamine and benzo[1,2-B:3,4-B':5,6-B']trithiophene-2,5,8-trialdehyde are dissolved in a polar solvent at a specific molar ratio. Then, an appropriate amount of catalyst is slowly added under stirring. The DA reaction is then carried out for 6–12 hours within a temperature range of room temperature to 60°C. After separation, washing, and drying, a micro / nano-structured conductive COF organic carrier is obtained. The COF organic carrier obtained by the DA reaction in this invention not only endows COF with excellent conductivity but also optimizes its micro / nano structure. This effectively reduces surface reflectivity, decreases scattering and loss of light signals during transmission, thereby improving signal integrity and transmission efficiency. Furthermore, it simultaneously improves the antistatic properties of the ceramic ferrule, reducing signal interference and equipment damage caused by static electricity. In addition, the COF organic carrier of this invention can form a stable network structure during high-temperature sintering, synergistically interacting with the zirconia ceramic matrix to improve the thermal stability of the ceramic ferrule and ensure stable performance of the ferrule under complex environments. The micro-nano structure of COF organic carriers can also optimize the microstructure of zirconia ceramics, improve the density and uniformity of ceramics, further reduce the scattering and loss of optical signals during transmission, and further improve the transmission efficiency and quality of optical signals.

[0006] S3: The rare earth modified nano-zirconia obtained in step S1, the micro-nano structure conductive COF organic carrier obtained in step S2, and the binder and additives are mixed in proportion and stirred in a high-speed mixer for 30 to 60 minutes at a stirring speed of 500 to 1000 rpm to obtain a gel-like substance. S4: The gel-like substance obtained in step S3 is injection molded, and then degreased, sintered and finished to obtain the ceramic ferrule for the self-aligning ultra-low loss high-end connector.

[0007] As a preferred technical solution, the rare earth metal alkoxide is at least one of yttrium isopropoxide, lanthanum isopropoxide, and cerium isopropoxide; the zirconium source is a zirconium alkoxide.

[0008] As a preferred technical solution, the polar solvent is at least one of dimethyl sulfoxide, N,N-dimethylformamide, acetonitrile, and tetrahydrofuran.

[0009] As a preferred technical solution, the adhesive is at least one of paraffin wax, polyethylene wax, polypropylene wax, and ethylene-vinyl acetate wax.

[0010] As a preferred technical solution, the additives include surfactants, plasticizers, and sintering aids.

[0011] As a preferred technical solution, the injection molding temperature is 150-200℃ and the injection pressure is 0.5-0.6MPa.

[0012] As a preferred technical solution, the degreasing process includes two steps: supercritical carbon dioxide-assisted solvent degreasing and thermal degreasing.

[0013] As a preferred technical solution, the sintering temperature is 1200-1300℃ and the sintering time is 2-4 hours.

[0014] As a preferred technical solution, the finishing process is to perform internal hole machining using a five-axis linkage air static pressure grinding system, and to achieve the concentration control of internal hole machining accuracy through online compensation using a laser interferometer, and to integrate an AI vision inspection module for closed-loop correction of three-dimensional parameters such as outer diameter, concentricity, and exit angle.

[0015] As a preferred technical solution, the mechanical structure parameters of the ceramic ferrule are as follows: the inner hole straightness is ≤0.1um / m, the inner diameter concentration is 0.1250-0.1255mm, the outer diameter accuracy is 2.49900±0.00025mm, the concentricity is <0.3μm, and the emission angle is <2°.

[0016] Another aspect of the present invention is to provide a ceramic ferrule for a non-aligning ultra-low loss high-end connector, wherein the ceramic ferrule is prepared by the above-described method for preparing a ceramic ferrule for a non-aligning ultra-low loss high-end connector.

[0017] The beneficial effects of this invention are: This invention discloses a method for fabricating ceramic ferrules for ultra-low-loss high-end connectors without the need for core adjustment. By innovatively introducing rare-earth-modified nano-zirconia and a micro / nano-structured conductive COF organic carrier during the fabrication process, it not only achieves high-precision molding and excellent mechanical properties of the ceramic ferrule but also significantly improves its optical and antistatic properties. The addition of rare-earth-modified nano-zirconia effectively improves the surface properties of the ceramic ferrule and enhances its bonding with the organic carrier and other components, thereby improving overall mechanical properties and stability. Simultaneously, the use of the micro / nano-structured conductive COF organic carrier not only endows the ceramic ferrule with excellent conductivity but also optimizes its microstructure, reducing scattering and loss of optical signals during transmission, thus improving signal integrity and transmission efficiency. Furthermore, the COF organic carrier can form a stable network structure during high-temperature sintering, synergistically interacting with the zirconia ceramic matrix to improve the thermal stability of the ceramic ferrule, ensuring stable performance of the ferrule under complex environments. These improvements make the application of ceramic ferrules in high-end connectors more reliable, enabling them to meet the long-term use requirements of high-end connectors in complex environments in various data transmission fields such as main lines of testing equipment, standard test lines, high-end data center computer rooms, medical devices, intelligent driving, and low-altitude flight. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the ceramic ferrule structure obtained in Embodiment 1 of the present invention. Detailed Implementation

[0019] The following description is intended to disclose the invention and enable those skilled in the art to implement it. The preferred embodiments described below are merely examples, and other obvious variations will occur to those skilled in the art.

[0020] Example 1 This embodiment describes a method for preparing ceramic ferrules for ultra-low-loss high-end connectors that do not require core alignment, which includes the following steps: S1: Dissolve 18g of yttrium isopropoxide and 100g of zirconium isopropoxide in 500mL of ethanol aqueous solution (volume ratio 1:1), then slowly add 10g of hydrolysis catalyst (nitric acid) under stirring, and then carry out the hydrolysis reaction at 60℃ for 1 hour. After that, continue stirring at room temperature for 24 hours to promote the condensation reaction and form a gel. Finally, dry the gel at 80℃ for 12 hours and grind it into powder to obtain rare earth modified nano-zirconia.

[0021] S2: 74 g of 5,5'-dioxodibenzothiophene-3,7-diamine (CAS: 6259-19-4) and 99 g of benzo[1,2-B:3,4-B':5,6-B']trithiophene-2,5,8-trialdehyde (CAS: 2243590-42-1) were dissolved in 150 mL of a polar solvent (dimethyl sulfoxide). Then, an appropriate amount of catalyst (p-toluenesulfonic acid) was slowly added under stirring. The DA reaction was then carried out at 60 °C for 12 hours. After separation, washing, and drying, a micro / nano-structured conductive COF organic carrier was obtained. The DA reaction refers to an electron donor-acceptor reaction.

[0022] S3: The rare earth-modified nano-zirconia obtained in step S1, the micro / nano-structured conductive COF organic carrier obtained in step S2, and the binder (paraffin wax) and additives are mixed in a mass ratio of 10:3:1:1. The additives include surfactants (such as ammonium polyphosphate), plasticizers (such as dibutyl phthalate), and sintering aids (such as alumina) in a mass ratio of 1:1:1. The mixture is stirred in a high-speed mixer for 30 minutes at a stirring speed of 1000 rpm to obtain a gel-like substance.

[0023] S4: The gel-like substance obtained in step S3 is injection molded at a temperature of 180℃ and an injection pressure of 0.5MPa. Then, it undergoes degreasing, sintering, and finishing processes in sequence.

[0024] The degreasing process includes two steps: supercritical carbon dioxide-assisted solvent degreasing and thermal degreasing. Supercritical carbon dioxide-assisted solvent degreasing: The injection-molded preform is placed in a supercritical carbon dioxide degreasing device, with the temperature set at 40℃, the pressure at 12MPa, and the treatment time at 4 hours. This process utilizes the high solubility of supercritical carbon dioxide to remove organic binders from the preform.

[0025] Thermal degreasing: The green body, after being degreased with supercritical carbon dioxide, is placed in a thermal degreasing furnace, with the temperature set at 500℃ and the treatment time at 3 hours. This process further removes residual organic matter from the green body through high-temperature decomposition and volatilization.

[0026] Sintering treatment: The degreased green body is placed in a sintering furnace, the temperature is set at 1200℃, and the sintering time is 4 hours. This process densifies the ceramic material, improving its mechanical and optical properties.

[0027] This embodiment increases the specific surface area of ​​zirconia ceramic powder by ≥16㎡ / g, improves surface activity by 15%, enhances the compactness of the blank, and at the same time improves the porosity of the sintered body by <0.03% and the surface roughness Ra≤5nm, thus providing the source powder with the foundation for high-end products.

[0028] Precision machining: The inner hole is machined using a five-axis linkage air static pressure grinding system. The precision concentration of the inner hole machining is controlled by online compensation through a laser interferometer. An integrated AI vision inspection module (12.8 million pixels + deep learning algorithm) is used to perform closed-loop correction of three-dimensional parameters such as outer diameter, concentricity, and exit angle.

[0029] like Figure 1 As shown, the mechanical structure parameters of the ceramic ferrule in this embodiment include: inner hole straightness ≤ 0.1 μm / m, inner diameter concentration 0.1250-0.1255 mm, outer diameter accuracy 2.49900 ± 0.00025 mm, concentricity < 0.3 μm, emission angle < 2°, front end bevel 35° ± 1', rear end bevel 60° ± 2', and rear end chamfer 0.15 ± 0.05 mm.

[0030] Example 2 The method for preparing ceramic ferrules for ultra-low loss high-end connectors without core adjustment in this embodiment is basically the same as that in Example 1 in terms of raw material composition and preparation steps. The difference is that in the preparation method of this embodiment, lanthanum isopropoxide is used instead of yttrium isopropoxide.

[0031] Example 3 The method for preparing ceramic ferrules for ultra-low loss high-end connectors without core adjustment in this embodiment is basically the same as that in Example 1 in terms of raw material composition and preparation steps. The difference is that cerium isopropoxide is used instead of yttrium isopropoxide in the preparation method of this embodiment.

[0032] Comparative Example 1 The preparation method of the ceramic ferrule for ultra-low loss high-end connectors without core adjustment in this comparative example is basically the same as that in Example 1 in terms of raw material composition and preparation steps. The difference is that step S2 is not included in the preparation method of this comparative example.

[0033] The ceramic ferrules for ultra-low loss high-end connectors without alignment prepared in Examples 1-3 and Comparative Example 1 were subjected to performance tests, and the performance results are shown in Table 1: The insertion loss test includes setting up a test system using a light source and an optical power meter, installing the ceramic ferrule in the test system, measuring the optical power before and after passing through the ceramic ferrule, and calculating the insertion loss. The test uses light sources with wavelengths of 1310nm and 1550nm, and an optical power meter with an accuracy of ≤0.01dB.

[0034] The mechanical strength test procedure includes fixing the ceramic ferrule sample on a three-point bending tester, applying a load until the sample breaks, recording the maximum load at fracture, and calculating the mechanical strength based on the sample dimensions. A three-point bending tester with an accuracy of ≤0.1 MPa is used for the test.

[0035] The thermal stability test procedure includes placing the ceramic ferrule sample in a high-temperature furnace, setting different temperature gradients, holding it at each temperature point for a certain period of time, observing the changes in the physical properties of the sample, and recording the performance changes of the sample at different temperatures to determine its thermal stability.

[0036] The test procedure for antistatic performance is as follows: First, clean the ceramic ferrule sample thoroughly, ensuring the surface is free of dust and stains. Then, place the sample in a standard test environment with a temperature of 23±2℃ and a relative humidity of 50±5%. Use a high-precision surface resistivity meter, calibrating the instrument to standard test conditions. Place the sample on the test platform, ensuring the sample surface is flat. Apply a 100V DC voltage to the sample surface using the test electrodes, wait 1 minute, and record the surface resistivity value. Repeat the measurement three times at different locations on the sample, and take the average value as the final result. Record the surface resistivity value for each measurement and calculate the average value.

[0037] Table 1 project Example 1 Example 2 Example 3 Comparative Example 1 Insertion loss (dB) ≤0.12 ≤0.12 ≤0.12 0.15 Mechanical strength (MPa) ≥300 ≥300 ≥300 290 Thermal stability (°C) ≥1200 ≥1200 ≥1200 ≥1200 Antistatic properties (Ω) <![CDATA[≤5*10 10 ]]> <![CDATA[≤5*10 10 ]]> <![CDATA[≤5*10 10 ]]> <![CDATA[8*10 10 ]]> The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed invention.

Claims

1. A method for manufacturing a ceramic ferrule for a high-end connector with ultra-low loss and no need for core adjustment, characterized in that, The preparation method includes the following steps: S1: Dissolve rare earth metal alkoxide and zirconium source in an ethanol aqueous solution, then slowly add an appropriate amount of hydrolysis catalyst under stirring, and then carry out hydrolysis reaction at 60-80℃ for 1-3 hours. After that, continue stirring at room temperature for 12-24 hours to promote condensation reaction and form gel. Finally, dry the gel at 60-80℃ for 12-24 hours and grind it into powder to obtain rare earth modified nano zirconium oxide. S2: 5,5'-dioxodibenzothiophene-3,7-diamine and benzo[1,2-B:3,4-B':5,6-B']trithiophene-2,5,8-trialdehyde are dissolved in a polar solvent at a certain molar ratio. Then, an appropriate amount of catalyst is slowly added under stirring. The DA reaction is then carried out for 6 to 12 hours in the temperature range of room temperature to 60°C. After separation, washing and drying, a micro-nano structured conductive COF organic support is obtained. S3: The rare earth modified nano-zirconia obtained in step S1, the micro-nano structure conductive COF organic carrier obtained in step S2, and the binder and additives are mixed in proportion and stirred in a high-speed mixer for 30 to 60 minutes at a stirring speed of 500 to 1000 rpm to obtain a gel-like substance. S4: The gel-like substance obtained in step S3 is injection molded, and then degreased, sintered and finished to obtain the ceramic ferrule for the self-aligning ultra-low loss high-end connector.

2. The method for preparing ceramic ferrules for ultra-low loss high-end connectors without alignment as described in claim 1, characterized in that, The rare earth metal alkoxide is at least one of yttrium isopropoxide, lanthanum isopropoxide, and cerium isopropoxide; the zirconium source is a zirconium alkoxide.

3. The method for preparing ceramic ferrules for ultra-low loss high-end connectors without alignment as described in claim 1, characterized in that, The binder is at least one of paraffin wax, polyethylene wax, polypropylene wax, and ethylene-vinyl acetate wax.

4. The method for preparing a ceramic ferrule for a high-end connector with no need for alignment as described in claim 1, characterized in that, The additives include surfactants, plasticizers, and sintering aids.

5. The method for preparing a ceramic ferrule for a high-end connector with no need for alignment as described in claim 1, characterized in that, The injection molding temperature is 150–200°C, and the injection pressure is 0.5–0.6 MPa.

6. The method for preparing a ceramic ferrule for a high-end connector with no need for alignment as described in claim 1, characterized in that, The degreasing process includes two steps: supercritical carbon dioxide-assisted solvent degreasing and thermal degreasing.

7. The method for preparing a ceramic ferrule for a high-end connector with no need for alignment as described in claim 1, characterized in that, The sintering temperature is 1200–1300℃, and the sintering time is 2–4 hours.

8. The method for preparing a ceramic ferrule for a high-end connector with no need for alignment as described in claim 1, characterized in that, The finishing process involves machining the inner hole using a five-axis linkage air static pressure grinding system. Online compensation using a laser interferometer enables concentrated control of the machining accuracy of the inner hole, and an integrated AI vision inspection module performs closed-loop correction of three-dimensional parameters such as outer diameter, concentricity, and exit angle.

9. The method for preparing a ceramic ferrule for a high-end connector with no need for alignment as described in claim 1, characterized in that, The mechanical structural parameters of the ceramic ferrule are as follows: the inner hole straightness is ≤0.1um / m, the inner diameter concentration is 0.1250-0.1255mm, the outer diameter accuracy is 2.49900±0.00025mm, the concentricity is <0.3μm, and the emission angle is <2°.

10. A ceramic ferrule for a high-end connector with ultra-low loss and no need for core adjustment, characterized in that, The ceramic ferrule is prepared using the ceramic ferrule preparation method for ultra-low loss high-end connectors without alignment as described in any one of claims 1 to 9.

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