A glass splinter, its preparation method and application

By using inorganic glass springs instead of epoxy resin adhesives, the problems of short lifespan and low strength of encapsulation materials in fiber Bragg grating sensors were solved, resulting in high-strength fiber Bragg grating sensors with low coefficient of thermal expansion, thus extending the sensor's lifespan and stability.

CN116655240BActive Publication Date: 2026-05-29ZHONGAN ZHENGHUI SENSING TECHNOLOGY (SHANDONG) CO LTD

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
ZHONGAN ZHENGHUI SENSING TECHNOLOGY (SHANDONG) CO LTD
Filing Date
2023-05-31
Publication Date
2026-05-29

AI Technical Summary

Technical Problem

The epoxy resin adhesive encapsulation material used in existing fiber Bragg grating sensors has a short lifespan, low strength, a large coefficient of thermal expansion affected by ambient temperature, and is prone to damage and aging, thus affecting the lifespan and accuracy of the sensor.

Method used

Inorganic glass springs are used instead of epoxy resin adhesives to encapsulate fiber Bragg gratings on the surface of the glass springs, forming a substrate that carries the fiber Bragg gratings. Silica, aluminum oxide, sodium oxide, and other raw materials are melted at high temperatures to form molten glass, which is then drawn into shape to form a high-strength glass plate with a low coefficient of thermal expansion.

Benefits of technology

This technology achieves high lifespan, high strength, and low expansion coefficient in fiber Bragg grating sensors, improving sensor durability and stability and extending sensor lifespan.

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Abstract

The application provides a glass bullet, a preparation method and application thereof. The glass bullet comprises the following raw materials: silicon dioxide, aluminum oxide, sodium oxide, boron trioxide, potassium oxide, magnesium oxide, zirconium dioxide, sodium sulfate and cerium oxide. The inorganic glass bullet of the application encapsulates a fiber grating on the surface to form a substrate carrying the fiber grating, and is applied to the field of fiber grating sensors. Compared with an epoxy resin adhesive encapsulation material, the inorganic glass bullet has the advantages of long service life, high strength, low expansion coefficient and the like.
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Description

Technical Field

[0001] This invention relates to the field of fiber optic grating sensor technology, and in particular to a glass spring, its preparation method, and its application. Background Technology

[0002] Currently, there are many manufacturers engaged in fiber Bragg grating (FBG) sensing technology both domestically and internationally. However, both domestic and imported products currently employ a fabrication scheme of fiber Bragg gratings + encapsulation materials + sensor substrate. Therefore, in the actual industrial field of FBG sensing technology, the components of a FBG sensor include the FBG element, the sensor substrate, and the encapsulation body that bonds the FBG element to the sensor substrate. Currently, the encapsulation body primarily uses epoxy resin adhesive. The lifespan of FBG sensors is severely limited by the effective time of the encapsulation body; epoxy resin typically ages and fails within 2-3 years, or even a few months under humid and hot conditions. This not only alters the performance parameters of the FBG sensor, making accurate measurement impossible, but also significantly shortens the sensor's lifespan.

[0003] Given the existing problems of short lifespan, low strength, and large expansion coefficient of epoxy resin adhesive encapsulation materials in fiber Bragg gratings, which are prone to damage and aging due to environmental temperature, it is necessary to improve these technologies. Summary of the Invention

[0004] To address the shortcomings of existing epoxy resin adhesive encapsulation materials in fiber Bragg gratings (FBGs), such as short lifespan, low strength, and high coefficient of thermal expansion due to environmental temperature, which makes them prone to damage and aging, this invention develops an inorganic glass spring sheet. This spring sheet encapsulates the surface of the FBG, forming a substrate that supports the FBG. Applied to the field of FBG sensors, this invention offers advantages such as long lifespan, high strength, and low coefficient of thermal expansion compared to epoxy resin adhesive encapsulation materials.

[0005] The technical solution of this invention is as follows:

[0006] In a first aspect, the present invention provides a glass spring comprising the following raw materials in weight percentages: 60-70% silicon dioxide, 8-14% aluminum oxide, 10-15% sodium oxide, 3-8% boron trioxide, 0.5-4% potassium oxide, 0.5-4% magnesium oxide, 0.5-3% zirconium dioxide, 0.1-0.8% sodium sulfate, and 0.1-0.5% cerium oxide.

[0007] Preferably, in the glass spring, the sum of the mass percentages of sodium oxide and potassium oxide is not less than 12%.

[0008] Preferably, the glass spring contains 62-66% silicon dioxide by mass.

[0009] Preferably, the glass spring contains aluminum oxide at a mass percentage of 8-12%.

[0010] Preferably, the boron trioxide content in the glass spring is 3-6% by mass.

[0011] Preferably, the magnesium oxide content in the glass spring is 2-4% by mass.

[0012] Preferably, the zirconium dioxide in the glass spring is 0.5% to 1% by mass;

[0013] The sum of the mass percentages of sodium sulfate and cerium oxide is 0.5% to 1.1%.

[0014] Secondly, the present invention also provides a method for preparing the aforementioned glass spring, comprising the following steps:

[0015] The following ingredients are mixed and stirred to obtain a mixture: silicon dioxide, aluminum oxide, sodium oxide, boron trioxide, potassium oxide, magnesium oxide, zirconium dioxide, sodium sulfate, and cerium oxide.

[0016] The mixture is melted at 1550–1650°C to obtain molten glass;

[0017] The molten glass is drawn down at 750-1300℃ to form a glass plate;

[0018] After annealing the glass plate at 600-700℃ to room temperature, a glass spring is obtained.

[0019] Preferably, in the method for preparing the glass spring, the thickness of the glass spring is 0.3 to 1.8 mm.

[0020] Thirdly, the present invention also provides an application of the glass spring described above or the glass spring prepared by the described preparation method in a fiber optic grating sensor.

[0021] The glass spring sheet, its preparation method, and its application of the present invention have the following advantages over the prior art:

[0022] The glass spring of the present invention comprises the following raw materials: silicon dioxide, aluminum oxide, sodium oxide, boron trioxide, potassium oxide, magnesium oxide, zirconium dioxide, sodium sulfate, and cerium oxide. The inorganic glass spring of the present invention encapsulates a fiber optic grating on its surface to form a substrate that carries the fiber optic grating. It is applied in the field of fiber optic grating sensors and has advantages such as high lifespan, high strength, and low coefficient of expansion compared to epoxy resin adhesive encapsulation materials. Detailed Implementation

[0023] The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0024] It should be noted that the order of description of the following embodiments is not intended to limit the preferred order of embodiments. Furthermore, in the description of this application, the term "comprising" means "including but not limited to". Various embodiments of the present invention may exist in the form of a range; it should be understood that the description in the form of a range is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the invention; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single numerical values ​​within that range. For example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., and single digits within the range, such as 1, 2, 3, 4, 5, and 6, regardless of the range. Additionally, whenever a numerical range is indicated herein, it means including any referenced number (fraction or integer) within the indicated range.

[0025] This application provides a glass spring comprising the following raw materials by mass percentage: 60-70% silicon dioxide, 8-14% aluminum oxide, 10-15% sodium oxide, 3-8% boron trioxide, 0.5-4% potassium oxide, 0.5-4% magnesium oxide, 0.5-3% zirconium dioxide, 0.1-0.8% sodium sulfate, and 0.1-0.5% cerium oxide.

[0026] The functions of each component in the glass spring of the present invention are as follows:

[0027] Silica: It forms the framework of glass springs and has good chemical stability, thermal stability, and transparency;

[0028] Aluminum oxide: a network intermediate for glass, which increases the mechanical strength and chemical strengthening properties of glass;

[0029] Sodium oxide and potassium oxide: excellent fluxes for glass, and also important substances for the chemical strengthening of glass;

[0030] Magnesium oxide: overcomes the tendency to crystallize, widens the temperature range, and is beneficial for molding operations;

[0031] Zirconium dioxide can inhibit the migration of alkali metals and alkaline earth metals, while also improving the hardness and elastic modulus of glass.

[0032] Boron trioxide: reduces the coefficient of glass expansion and also reduces the difficulty of melting;

[0033] Cerium oxide and sodium sulfate (Glauber's salt): act as composite clarifying agents, and high-temperature clarification facilitates the removal of bubbles.

[0034] This invention targets the field of fiber Bragg grating (FBG) sensors, employing glass to replace traditional metal substrates and adhesives to achieve fully glass-encapsulated FBG sensors. Without compromising the core performance characteristics of the substrate, such as strength, stiffness, and elasticity, or increasing manufacturing costs, it achieves excellent corrosion resistance and long lifespan, completely solving the durability and stability issues of fiber optic sensors. This represents a completely new sensor technology and product for the engineering field. Currently, the use of organic plastics for FBG springs results in short lifespans, low strength, and large expansion coefficients due to changes in ambient temperature. Developing glass, with its high lifespan, high strength, and low expansion coefficient, is undoubtedly the best choice. The inorganic glass spring of this invention encapsulates the FBG on its surface, forming a substrate that supports the FBG. Applied to the field of FBG sensors, it offers advantages such as high lifespan, high strength, and low expansion coefficient compared to epoxy resin adhesive encapsulation materials.

[0035] In some embodiments, the sum of the mass percentages of sodium oxide and potassium oxide is not less than 12%.

[0036] In some embodiments, the mass percentage of silicon dioxide is 62-66%.

[0037] In some embodiments, the mass percentage of aluminum oxide is 8-12%.

[0038] In some embodiments, the mass percentage of boron trioxide is 3-6%.

[0039] In some embodiments, the mass percentage of magnesium oxide is 2-4%.

[0040] In some embodiments, the mass percentage of zirconium dioxide is 0.5% to 1%;

[0041] In some embodiments, the sum of the mass percentages of sodium sulfate and cerium oxide is 0.5% to 1.1%.

[0042] The above formula components are suitable for float glass, overflow glass, and slot-pull glass production processes, and the produced glass thickness is 0.3-1.8mm. It can be chemically ion-strengthened and has advantages such as long service life, high strength, and low coefficient of thermal expansion.

[0043] Based on the same inventive concept, the present invention also provides a method for preparing the above-mentioned glass spring, comprising the following steps:

[0044] S1. Mix and stir silicon dioxide, aluminum oxide, sodium oxide, boron trioxide, potassium oxide, magnesium oxide, zirconium dioxide, sodium sulfate, and cerium oxide to obtain a mixture;

[0045] S2. Melt the mixture at 1550-1650℃ to obtain molten glass;

[0046] S3. Pull the molten glass down at 750-1300℃ to form a glass plate;

[0047] S4. Anneal the glass plate at 600-700℃ to room temperature to obtain a glass spring.

[0048] In some embodiments, the thickness of the glass spring is 0.3 to 1.8 mm.

[0049] Step S2 is as follows: Place the mixture into a platinum-rhodium crucible, and then place it in a glass melting furnace to melt at 1550-1630℃ for 6-12 hours to obtain molten glass; in the middle and later stages of melting, use a platinum rod to stir slowly, which is beneficial to the clarification, homogenization and debubbling of the molten glass (remember not to stir too fast as it will introduce air and affect the quality of the molten glass).

[0050] Step S3 specifically involves drawing molten glass down to a shape at 750-1300℃, using processes including but not limited to float glass, overflow glass, and slit glass drawing, to obtain a glass sheet. In step S4, the glass sheet is annealed at 600-700℃ to room temperature, and then cut to obtain the desired glass springs. Specifically, the glass sheet is annealed at 600-700℃ for 1.5-3 hours to room temperature, and then cut and polished to a thickness of 0.3-1.8 mm. Finally, the physicochemical properties of the glass springs made from each batch of materials are tested, and the relevant parameters are recorded. The physicochemical property tests include Young's modulus and coefficient of thermal expansion.

[0051] Based on the same inventive concept, the present invention also provides an application of the glass spring sheet described above or the glass spring sheet prepared by the above preparation method in a fiber optic grating sensor.

[0052] The specific application mentioned above is as follows: encapsulating fiber Bragg gratings on the surface of a glass spring to form a substrate that carries the fiber Bragg gratings, which is then applied in the field of fiber Bragg grating sensors.

[0053] The following detailed embodiments further illustrate the glass spring of this application, its preparation method, and its application. This section further explains the invention in conjunction with specific embodiments, but should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the embodiments are conventional means well known to those skilled in the art. Unless otherwise specified, the reagents, methods, and equipment used in this invention are conventional reagents, methods, and equipment in the art.

[0054] Example 1

[0055] This application provides a glass spring sheet comprising the following raw materials by mass percentage: SiO2 64.5%, Al2O3 10%, Na2O 12.5%, B2O3 5%, K2O 3.4%, MgO 3.3%, ZrO2 0.8%, Na2SO4 0.3%, and CeO2 0.2%.

[0056] The method for preparing the above-mentioned glass spring includes the following steps:

[0057] S1. According to the above mass percentage ratio, mix and stir SiO2, Al2O3, Na2O, B2O3, K2O, MgO, ZrO2, Na2SO4, and CeO2 to obtain 200g of mixture;

[0058] S2. Place 200g of the mixture into a platinum-rhodium crucible and melt it in a glass melting furnace at 1600℃ for 9 hours to obtain molten glass.

[0059] S3. The molten glass is pulled down at 1000℃ to form a glass plate;

[0060] S4. Anneal the glass plate at 650℃ for 2 hours to room temperature, then cut and polish the glass plate to obtain a glass spring with a thickness of 1.3mm.

[0061] Example 2

[0062] This application provides a glass spring sheet comprising the following raw materials by mass percentage: SiO2 64.5%, Al2O3 9.5%, Na2O 12.5%, B2O3 5%, K2O 3.4%, MgO 3.8%, ZrO2 0.8%, Na2SO4 0.3%, and CeO2 0.2%.

[0063] The method for preparing the above-mentioned glass spring includes the following steps:

[0064] S1. According to the above mass percentage ratio, mix and stir SiO2, Al2O3, Na2O, B2O3, K2O, MgO, ZrO2, Na2SO4, and CeO2 to obtain 200g of mixture;

[0065] S2. Place 200g of the mixture into a platinum-rhodium crucible and melt it in a glass melting furnace at 1600℃ for 9 hours to obtain molten glass.

[0066] S3. The molten glass is pulled down at 1000℃ to form a glass plate;

[0067] S4. Anneal the glass plate at 650℃ for 2 hours to room temperature, then cut and polish the glass plate to obtain a glass spring with a thickness of 1.3mm.

[0068] Example 3

[0069] This application provides a glass spring sheet comprising the following raw materials by mass percentage: SiO2 63.5%, Al2O3 11%, Na2O 13%, B2O3 5%, K2O 2.9%, MgO 3.3%, ZrO2 0.8%, Na2SO4 0.3%, and CeO2 0.2%.

[0070] The method for preparing the above-mentioned glass spring includes the following steps:

[0071] S1. According to the above mass percentage ratio, mix and stir SiO2, Al2O3, Na2O, B2O3, K2O, MgO, ZrO2, Na2SO4, and CeO2 to obtain 200g of mixture;

[0072] S2. Place 200g of the mixture into a platinum-rhodium crucible and melt it in a glass melting furnace at 1600℃ for 9 hours to obtain molten glass.

[0073] S3. The molten glass is pulled down at 1000℃ to form a glass plate;

[0074] S4. Anneal the glass plate at 650℃ for 2 hours to room temperature, then cut and polish the glass plate to obtain a glass spring with a thickness of 1.3mm.

[0075] Example 4

[0076] This application provides a glass spring sheet comprising the following raw materials by mass percentage: SiO2 63.5%, Al2O3 10.5%, Na2O 12.4%, B2O3 5%, K2O 3.5%, MgO 3.8%, ZrO2 0.8%, Na2SO4 0.3%, and CeO2 0.2%.

[0077] The method for preparing the above-mentioned glass spring includes the following steps:

[0078] S1. According to the above mass percentage ratio, mix and stir SiO2, Al2O3, Na2O, B2O3, K2O, MgO, ZrO2, Na2SO4, and CeO2 to obtain 200g of mixture;

[0079] S2. Place 200g of the mixture into a platinum-rhodium crucible and melt it in a glass melting furnace at 1600℃ for 9 hours to obtain molten glass.

[0080] S3. The molten glass is pulled down at 1000℃ to form a glass plate;

[0081] S4. Anneal the glass plate at 650℃ for 2 hours to room temperature, then cut and polish the glass plate and the glass block to obtain a glass spring with a thickness of 1.3mm.

[0082] The Young's modulus and coefficient of thermal expansion of the glass sheets obtained in Examples 1 to 4 are shown in Table 1 below.

[0083] Table 1 - Young's modulus and coefficient of thermal expansion of different glass sheets

[0084] Example Example 1 Example 2 Example 3 Example 4 Young's modulus (GPa) 72.3 71.8 71.6 72.1 <![CDATA[Coefficient of thermal expansion (10 -7 / °C)]]> 2.5 2.4 2.7 2.6

[0085] As can be seen from Table 1, the glass springs in the field of fiber gratings provided by this invention have excellent performance in terms of Young's modulus and coefficient of thermal expansion.

[0086] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A glass spring, characterized in that, The raw materials include the following percentages by weight: silicon dioxide 63.5-64.5%, aluminum oxide 9.5-11%, sodium oxide 12.4-13%, boron trioxide 5%, potassium oxide 2.9-3.5%, magnesium oxide 3.3-3.8%, zirconium dioxide 0.8%, sodium sulfate 0.3%, and cerium oxide 0.2%. The method for preparing the glass spring includes the following steps: The following ingredients are mixed and stirred to obtain a mixture: silicon dioxide, aluminum oxide, sodium oxide, boron trioxide, potassium oxide, magnesium oxide, zirconium dioxide, sodium sulfate, and cerium oxide. The mixture is melted at 1600℃ for 6~12h to obtain glass melt; The molten glass is drawn down at 1000℃ to form a glass plate; After annealing the glass plate at 600~700℃ for 1.5~3h to room temperature, a glass spring is obtained.

2. A method for preparing a glass spring as described in claim 1, characterized in that, Includes the following steps: The following ingredients are mixed and stirred to obtain a mixture: silicon dioxide, aluminum oxide, sodium oxide, boron trioxide, potassium oxide, magnesium oxide, zirconium dioxide, sodium sulfate, and cerium oxide. The mixture is melted at 1600℃ for 6~12h to obtain glass melt; The molten glass is drawn down at 1000℃ to form a glass plate; After annealing the glass plate at 600~700℃ for 1.5~3h to room temperature, a glass spring is obtained.

3. The method for preparing the glass spring as described in claim 2, wherein the thickness of the glass spring is 0.3~1.8 mm.

4. The application of a glass spring as described in claim 1 or a glass spring prepared by any of the preparation methods described in claims 2 to 3 in a fiber optic grating sensor.