Glass tube, preparation method and application in intelligent sensor

Abstract

The invention relates to a glass tube, a preparation method of the glass tube and application of the glass tube in an intelligent sensor, belongs to the technical field of preparation of sensor glass tubes, and aims at solving the problems that a traditional glass tube is insufficient in dielectric property, poor in thermal expansion characteristic adaptability, prone to environmental erosion and the like. The modified barium strontium silicate is prepared through the steps of raw material pretreatment, stepped heating calcination, surface modification and the like, the glass tube is prepared through raw material mixing, high-temperature melting, forming and processing treatment, and the glass tube can be applied to the fields of reed switch sensor packaging, liquid level measurement transparent elements, anti-theft sensor triggering structures and the like. The modified barium strontium silicate is introduced to construct a dielectric functional unit, so that the fidelity of high-frequency signals is optimized, the long-term environmental stability and the structural integrity under thermal shock are improved, and the application in high-end intelligent sensors can be expanded.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of sensor glass tube preparation, and particularly relates to a glass tube, a preparation method and application in an intelligent sensor. BACKGROUND

[0002] As a core perception unit of modern information technology, intelligent sensors have been deeply integrated into many fields such as industrial automation, automobile electronics, smart home, medical equipment, etc., and their function implementation relies on the stable operation of core components. The glass tube plays an important role in sensor packaging, signal transmission channel, trigger structure and sensitive element protection due to its excellent insulation, light transmission, chemical stability and structural strength. With the rapid development of intelligent sensors towards high frequency, integration, miniaturization and long service life, the performance of glass tubes is required to be more precise. They not only need to provide physical support as basic structural components, but also need to cooperate to ensure the signal accuracy and operation stability of the sensor in complex working conditions, which is an important carrier to improve the overall performance of the sensor.

[0003] There are many bottlenecks in the current technology: the dielectric performance of traditional glass tubes is insufficient, which easily leads to electromagnetic aggregation in high-frequency signal transmission, affecting the impedance matching and signal fidelity of the sensor; the thermal expansion characteristics of the glass matrix and other materials are poorly adapted, which easily produces stress concentration during temperature cycling, leading to fracture; it is easily eroded by the environment, accelerating the aging of the device performance and shortening the service life. These problems jointly restrict the application expansion of glass tubes in high-end intelligent sensors, and new glass tube materials with more excellent performance are urgently needed. SUMMARY

[0004] In view of the above situation, in order to overcome the defects of the prior art, the application provides a glass tube, a preparation method and application in an intelligent sensor, which effectively solves the problems of insufficient dielectric performance, poor thermal expansion characteristic adaptability and easy environmental erosion of the intelligent sensor glass tube on the market.

[0005] The technical scheme adopted by the application is as follows: the application provides a glass tube, a preparation method and application in an intelligent sensor, which comprises the following raw materials by weight: 65-70 parts of silicon dioxide, 5-7 parts of aluminum hydroxide, 3-3.5 parts of modified barium strontium silicate, 2-3 parts of sodium silicate, 1-3 parts of boric acid, 2-3 parts of lithium carbonate, 3-5 parts of potassium carbonate, 5-6 parts of barium carbonate, 2.8-3.5 parts of ferric sesquioxide, 2-3 parts of strontium carbonate, and 0.3-0.5 parts of silicon carbide. The preparation method of the modified barium strontium silicate comprises the following steps: SrCO3, BaCO3, SiO2 are subjected to drying and dehydration treatment to avoid water from causing splashing during calcination, and then are sieved to remove agglomerated particles and impurities, so as to ensure uniformity and reactivity of the raw materials; the components are weighed and mixed, and are placed in a high-temperature furnace for stepwise calcination, and nitrogen is replaced by air after protection, to generate pure-phase barium strontium silicate crystals; after the reaction is completed, the sintered block is naturally cooled, and after being crushed, fine grinding is performed to obtain superfine powder; the powder is immersed in an ethanol solution containing a silane coupling agent, and after dispersion and drying, modified barium strontium silicate is obtained.

[0006] Further, the molar ratio of SrCO3, BaCO3, SiO2 is (35-50): (50-65): 100.

[0007] Further, the temperature rising program is set as a first stage, a second stage, a third stage and a fourth stage.

[0008] Further, the first stage is a material dehydration stage, and the program is set to heat to 550-650 DEG C at a heating rate of 3 DEG C / min, and the holding time is 50-70 min.

[0009] Further, the second stage is a carbonate decomposition stage, and the program is set to heat to 1000-1200 DEG C at a heating rate of 5 DEG C / min, and the holding time is 80-100 min, for decomposing carbonates.

[0010] Further, the third stage is a solid phase reaction stage, and the program is set to heat to 1100-1300 DEG C at a heating rate of 2 DEG C / min, and the holding time is 100-140 min, for solid phase reaction.

[0011] Further, the fourth stage is a cooling stage, and the program is set to cool to 20-30 DEG C.

[0012] Further, the silane coupling agent is one of KH-550, KH-560 and KH-570.

[0013] Further, the raw materials are weighed, mixed and stirred uniformly; are placed in a combustion furnace for high-temperature melting, and the melting temperature is 1200-1600 DEG C; are formed by a Danla Law tube; and the glass tube is obtained after cutting and processing.

[0014] Further, it can be used in the fields of reed switch sensor packaging, liquid level measurement transparent element, anti-theft sensor triggering structure, temperature sensor protection, precision detection instrument, etc.

[0015] The beneficial effects achieved by the application with the above structure are as follows: By introducing modified barium strontium silicate, the ordered arrangement of dielectric functional units is induced inside the glass matrix, which affects the electromagnetic wave propagation path by changing the local electric field distribution state. When high-frequency current passes through the packaging system, the dielectric units couple with the electromagnetic field, weaken the invalid accumulation of charges between the electrodes, reduce the capacitive delay in the signal transmission process, and improve the signal response speed and fidelity of the device, and improve the high-frequency response.

[0016] Modified barium strontium silicate exhibits selective adsorption properties for alkali metal ions. The oxygen vacancy defects at the grain boundaries are partially filled to form a stable charge balance. When aggressive ions in the environment penetrate, the migrating ions are captured by ion exchange and solidified into inert compounds, blocking their diffusion path to the sensitive area of the die. The thermal expansion compatibility of the strontium barium silicate microcrystalline phase with the matrix reduces the interfacial thermal stress accumulation and delays the performance degradation of the material in a hot and humid environment.

[0017] Modified barium strontium silicate induces local energy dissipation through lattice distortion in temperature cycling. When the packaging system undergoes thermal shock, the interface between the strontium barium silicate microcrystalline phase and the glass matrix undergoes reversible bond length stretching, converting thermal stress into vibration energy. This process is accompanied by dislocation slip generated by the small amount of phase change, which promotes the release of energy in the stress concentration area through phonon scattering, avoiding the directional transmission of stress in the glass network, thereby maintaining the structural integrity of the material under severe temperature changes. It is suitable for packaging protection of high-power devices. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 A comparison chart of dielectric performance test results of a glass tube, a preparation method and an application in a smart sensor proposed by the present application.

[0019] Figure 2 A comparison chart of salt spray exposure test results of a glass tube, a preparation method and an application in a smart sensor proposed by the present application.

[0020] Figure 3 A comparison chart of temperature cycling test results of a glass tube, a preparation method and an application in a smart sensor proposed by the present application.

[0021] Figure 4 A comparison chart of thermal shock cycling test results of a glass tube, a preparation method and an application in a smart sensor proposed by the present application.

[0022] Figure 5 A damage degree image of a glass tube, a preparation method and an application in a smart sensor proposed by the present application. The left image is Example 1, and the right image is Comparative Example 2.

[0023] The accompanying drawings are included to provide a further understanding of the application, and are incorporated in and constitute a part of the specification, illustrate embodiments of the application, and are used to explain the present application, but are not intended to limit the present application. DETAILED DESCRIPTION

[0024] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative efforts fall within the scope of the present application. Embodiment 1

[0025] First, modified barium strontium silicate is prepared. SrCO3, BaCO3 and SiO2 are dehydrated in an oven at 120℃ for 2 hours to avoid water from causing splashing during calcination. The impurities are removed by sieving through a 200-mesh sieve to remove lumps and foreign matter. The components are weighed and mixed according to the molar ratio of 35:65:100. The mixture is placed in a high-temperature furnace for stepwise calcination. The first stage is dehydration, with the temperature raised to 550℃ at a rate of 3℃ / min, and the holding time is 50 min. The second stage is decomposition of carbonates, with the temperature raised to 1000℃ at a rate of 5℃ / min, and the holding time is 80 min. The third stage is solid-phase reaction, with the temperature raised to 1100℃ at a rate of 2℃ / min, and the holding time is 100 min. The fourth stage is cooling to 20℃. Nitrogen is introduced for protection in the first and second stages, and natural air is introduced in the third stage to generate pure-phase barium strontium silicate crystals. After the reaction is completed, the sintered block is naturally cooled, and the sintered block is broken into particles with a particle size of 0.8-1.2μm by a crusher. The particles are finely ground after being crushed to obtain ultra-fine powder. The powder is immersed in an ethanol solution containing 5wt% silane coupling agent, and ultrasonic dispersion is performed for 20 min. The modified barium strontium silicate is obtained after drying at 80℃.

[0026] The raw materials are weighed as follows: 65-70 parts of silicon dioxide, 5-7 parts of aluminum hydroxide, 3-3.5 parts of modified barium strontium silicate, 2-3 parts of sodium silicate, 1-3 parts of boric acid, 2-3 parts of lithium carbonate, 3-5 parts of potassium carbonate, 5-6 parts of barium carbonate, 2.8-3.5 parts of ferric tetroxide, 2-3 parts of strontium carbonate, 0.3-0.5 parts of silicon carbide, which are mixed and stirred uniformly. The mixture is placed in a combustion furnace for high-temperature melting, and the melting temperature is 1200℃. The Danlafala tube is formed, and the glass tube is obtained after cutting and processing the tube. Embodiment 2

[0027] Firstly, the modified barium strontium silicate is prepared. SrCO3, BaCO3 and SiO2 are dehydrated in an oven at 120°C for 2 hours to avoid water from causing splashing during calcination. The mixture is sieved through a 200-mesh sieve to remove impurities, lumps and foreign matter. The components are weighed according to the molar ratio of 42:58:100, and mixed thoroughly. The mixture is placed in a high-temperature furnace for stepwise calcination. The first stage is dehydration, with the temperature raised to 600°C at a rate of 3°C / min, and the holding time is 60 min. The second stage is decomposition of the carbonate, with the temperature raised to 1100°C at a rate of 5°C / min, and the holding time is 90 min. The third stage is solid-phase reaction, with the temperature raised to 1200°C at a rate of 2°C / min, and the holding time is 120 min. The fourth stage is cooling to 25°C. Nitrogen is introduced for protection in the first and second stages, and natural air is used in the third stage to generate pure-phase barium strontium silicate crystals. After the reaction is completed, the sintered block is cooled naturally, and the sintered block is crushed to a particle size of 0.8-1.2 μm using a crusher. The crushed product is finely ground to obtain an ultra-fine powder. The powder is immersed in an ethanol solution containing 5wt% silane coupling agent, and ultrasonically dispersed for 20 min. The modified barium strontium silicate is obtained after drying at 80°C.

[0028] The raw materials are weighed as follows: 68 parts of silicon dioxide, 6 parts of aluminum hydroxide, 3.2 parts of modified barium strontium silicate, 2.5 parts of sodium silicate, 2 parts of boric acid, 2.5 parts of lithium carbonate, 4 parts of potassium carbonate, 5.5 parts of barium carbonate, 3.2 parts of ferric tetroxide, 2.5 parts of strontium carbonate, 0.4 parts of silicon carbide, mixed and stirred uniformly. The mixture is placed in a combustion furnace for high-temperature melting, with the melting temperature being 1400°C. The Danlafala tube is used for forming, and the glass tube is obtained after cutting and processing. Example 3

[0029] Firstly, the modified barium strontium silicate is prepared. SrCO3, BaCO3 and SiO2 are dehydrated in an oven at 120℃ for 2 hours to avoid water from causing splashing during calcination, screened through a 200 mesh sieve to remove impurities and remove lumps and foreign matter. The components are weighed according to the molar ratio of 50:50:100, and each component is mixed thoroughly. The mixture is placed in a high-temperature furnace for stepwise calcination. The first stage is dehydration, the temperature is raised to 650℃ at a rate of 3℃ / min, and the holding time is 70 min. The second stage is decomposition of carbonate, the temperature is raised to 1200℃ at a rate of 5℃ / min, and the holding time is 100 min. The third stage is solid-phase reaction, the temperature is raised to 1300℃ at a rate of 2℃ / min, and the holding time is 120 min. The fourth stage is cooling to 30℃. Nitrogen is introduced in the first and second stages for protection, and natural air is replaced in the third stage to generate pure-phase barium strontium silicate crystals. After the reaction is completed, the sintered block is naturally cooled, the sintered block is broken into particles with a particle size of 0.8-1.2μm using a crusher, and the crushed particles are finely ground to obtain ultra-fine powder. The powder is immersed in an ethanol solution containing 5wt% silane coupling agent, ultrasonically dispersed for 20 min, and dried at 80℃ to obtain the modified barium strontium silicate.

[0030] The raw materials are weighed as follows: 70 parts of silicon dioxide, 7 parts of aluminum hydroxide, 3.5 parts of modified barium strontium silicate, 3 parts of sodium silicate, 3 parts of boric acid, 3 parts of lithium carbonate, 5 parts of potassium carbonate, 6 parts of barium carbonate, 3.5 parts of ferric oxide, 3 parts of strontium carbonate, and 0.5 parts of silicon carbide. The mixture is mixed and stirred uniformly, placed in a combustion furnace for high-temperature melting, and the melting temperature is 1600℃. The Danlafala tube is formed, and the glass tube is obtained after cutting and processing.

[0031] Comparative Example 1 The raw materials are weighed as follows: 65-70 parts of silicon dioxide, 5-7 parts of aluminum hydroxide, 2-3 parts of sodium silicate, 1-3 parts of boric acid, 2-3 parts of lithium carbonate, 3-5 parts of potassium carbonate, 5-6 parts of barium carbonate, 2.8-3.5 parts of ferric oxide, 2-3 parts of strontium carbonate, and 0.3-0.5 parts of silicon carbide. The mixture is mixed and stirred uniformly, placed in a combustion furnace for high-temperature melting, and the melting temperature is 1200℃. The Danlafala tube is formed, and the glass tube is obtained after cutting and processing.

[0032] Comparative Example 2 The raw materials are weighed as follows: 69 parts of silicon dioxide, 6 parts of aluminum hydroxide, 15 parts of sodium carbonate, 1.5 parts of boric acid, 6.5 parts of lithium carbonate, 4.0 parts of potassium carbonate, 7.9 parts of barium carbonate, 3.1 parts of ferric oxide, 1 part of strontium oxide, and 0.5 parts of C powder. The mixture is mixed and stirred uniformly, placed in a combustion furnace for high-temperature melting, and the melting temperature is 1200℃. The Danlafala tube is formed, and the glass tube is obtained after cutting and processing.

[0033] Comparative Example 3 Take the following weight parts of raw materials: barium carbonate 50 parts, strontium carbonate 0.5 parts, calcium carbonate 7.5 parts, lead oxide 0.5 parts, titanium dioxide 30 parts, yttrium oxide 0.1 parts, silicon dioxide 0.1 parts, manganese chloride 0.5 parts, bismuth oxide 0.1 parts, mix and stir uniformly; put in the combustion furnace for high temperature smelting, the smelting temperature is 1200℃; use the Danlafala pipe to form; cut the pipe and process to obtain the glass tube.

[0034] Experimental example 1 Take 6 groups of glass tube samples from examples 1-3 and comparative examples 1-3 respectively, cut the glass tube into 10mmx10mmx1mm thin slices, polish the surface, 3 repeated samples per group; prepare a vector network analyzer, place the sample in a parallel plate electrode, scan the 1-10GHz frequency band, record the dielectric constant (ε) and loss tangent (tanδ) indicators and compare, conduct three tests and take the average value.

[0035] Table 1 dielectric performance test results

[0036] As Figure 1 and Table 1, the test data of each example and the comparison group show that the glass samples of examples 1-3 with modified barium strontium silicate all exhibit better dielectric stability at 10GHz high frequency, among which example 2 achieves the lowest dielectric loss and signal distortion rate, significantly better than comparative examples 1-3 without adding modifier, with the increase of modifier content, the dielectric constant shows a trend of first decreasing and then increasing, while the loss characteristics continue to improve, which confirms that the modified barium strontium silicate effectively optimizes the high frequency response characteristics of the material by constructing a nano dielectric network.

[0037] Experimental example 2 Group the example and comparative example samples for salt spray exposure test, simulate high corrosion environment by hanging in the salt spray chamber, use neutral salt solution for continuous spraying treatment, after exposure, gently clean the surface deposited salt and dry, record the weight change data after re-equilibrium, conduct three tests and take the average value.

[0038] As Figure 2 shown, in the 48-hour neutral salt spray exposure test, the example samples (1-3) containing modified barium strontium silicate show significantly better surface integrity than the comparative examples, the example group only shows slight pitting on the surface, without large area peeling or discoloration, with small weight loss; while the comparative example group (especially comparative example 3) shows obvious corrosion degradation, with surface powdering, local collapse and significant mass loss, the experiment shows that the introduction of modified barium strontium silicate effectively inhibits the material degradation in high corrosion environment.

[0039] Experimental example 3 Temperature cycling experiments were conducted on the examples and comparative samples in groups. Extreme hot and cold alternation conditions were achieved through programmed control. Multiple cycles were performed in the low and high temperature ranges to simulate thermal shock. Each cycle included a rapid heating and cooling process and maintained a stable temperature range. After the experiment, the samples were rebalanced to release thermal stress. Changes in material weight or size were recorded. Three experiments were conducted, and the average value was taken.

[0040] like Figure 3 As shown, after 10 cycles of extreme temperatures from -40°C to 85°C, the sample samples of the examples (1-3) exhibited excellent dimensional stability and crack resistance, with minimal length changes and only microcracks or no visible cracks on the surface; while the comparative group (1-3) showed significant thermal stress failure, manifested as permanent length growth and multiple cracks. This experiment confirms that modified barium strontium silicate significantly improves the deformation buffering capacity and structural durability of the material under alternating hot and cold conditions.

[0041] Experiment Example 4 The examples and comparative samples were grouped and subjected to thermal shock cycling tests. The glass tube samples were placed in a muffle furnace and heated thoroughly before being rapidly immersed in liquid nitrogen to achieve extreme temperature difference shock. After each cycle, the cracking or breakage of the samples was recorded in detail until the preset number of cycles was completed. Three tests were conducted and the average value was taken.

[0042] like Figure 4 and Figure 5 As shown, the examples with modified barium strontium silicate exhibited a significant improvement in structural integrity under thermal shock conditions. Compared to the unmodified control group samples, the experimental group samples containing the modifier showed a significantly enhanced ability to maintain airtightness under extreme temperature cycling, and no through-cracks appeared on the surface. As the amount of modifier added increased, the number of cycles before thermal shock failure increased, while the comparative samples generally showed brittle fracture characteristics, confirming that modified barium strontium silicate improved the stress buffering capacity of the glass tube.

[0043] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0044] While embodiments of the application have been shown and described, it is to be understood that the application is not limited to the details of the embodiments described, since various modifications can be made by those skilled in the art, without departing from the spirit and scope of the application, which is defined by the appended claims and their equivalents.

[0045] The above description of the application and its embodiments is not restrictive, and the embodiments shown in the drawings are only one of the embodiments of the application, and the actual structure is not limited thereto. In general, if a person skilled in the art is inspired by it, without departing from the purpose of the application, without creative design, similar structure and embodiments of the technical solution should belong to the protection scope of the application.

Claims

1. A glass tube, characterized in that: The raw materials include the following parts by weight: 65-70 parts silicon dioxide, 5-7 parts aluminum hydroxide, 3-3.5 parts modified barium strontium silicate, 2-3 parts sodium silicate, 1-3 parts boric acid, 2-3 parts lithium carbonate, 3-5 parts potassium carbonate, 5-6 parts barium carbonate, 2.8-3.5 parts iron(III) oxide, 2-3 parts strontium carbonate, and 0.3-0.5 parts silicon carbide; The preparation method of the modified barium strontium silicate includes the following steps: SrCO3, BaCO3, and SiO2 were dried and dehydrated, and then sieved to remove impurities. The components were weighed and thoroughly mixed, placed in a high-temperature furnace, and calcined by stepwise heating. Nitrogen gas was introduced for protection, and then replaced with air to generate pure-phase barium strontium silicate crystals. After the reaction was completed, the sintered block was naturally cooled, crushed, and then finely ground to obtain ultrafine powder. The powder was immersed in an ethanol solution containing a silane coupling agent, dispersed, and dried to obtain modified barium strontium silicate.

2. A glass tube according to claim 1, characterized in that: The molar ratio of SrCO3, BaCO3, and SiO2 is (35-50):(50-65):

100.

3. A glass tube according to claim 2, characterized in that: The heating program is set to a first stage, a second stage, a third stage, and a fourth stage.

4. A glass tube according to claim 3, characterized in that: The first stage of the heating program involves heating to 550-650℃ at a rate of 3℃ / min and holding for 50-70 minutes.

5. A glass tube according to claim 4, characterized in that: The second stage of the heating program involves heating to 1000-1200℃ at a rate of 5℃ / min and holding for 80-100min.

6. A glass tube according to claim 5, characterized in that: The third stage heating program involves heating to 1100-1300℃ at a rate of 2℃ / min and holding for 100-140min.

7. A glass tube according to claim 6, characterized in that: The fourth stage of the heating process involves cooling down to 20-30℃.

8. A glass tube according to claim 7, characterized in that: The silane coupling agent is one of KH-550, KH-560, and KH-570.

9. A method for preparing a glass tube according to claims 1-8, characterized in that: Weigh the raw materials, mix them and stir evenly; place them in a combustion furnace for high-temperature melting at a temperature of 1200-1600℃; shape them into tubes using the Denrafa method; cut the tubes and process them to obtain glass tubes.

10. The application of a glass tube in a smart sensor according to claim 9, characterized in that: It can be used in fields such as reed switch sensor packaging, transparent elements for liquid level measurement, triggering structures for anti-theft sensors, temperature sensor protection, and precision testing instruments.

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