A soldering process using a new type of glass soldering sapphire

By using bismuth oxide, boron oxide, and silicon oxide glass powder to prepare glass solder paste, the problem of reduced mechanical properties in sapphire brazing was solved, high-quality sapphire connections were achieved, thermal stress was reduced, and welding strength and stability were improved.

CN119612966BActive Publication Date: 2026-03-17NORTHWESTERN POLYTECHNICAL UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-09
Publication Date
2026-03-17

AI Technical Summary

Technical Problem

Existing sapphire brazing processes result in reduced mechanical properties, especially due to the brittle intermetallic compounds generated during metal brazing and the difference in thermal expansion coefficients between ceramics and metals, which leads to high residual stress at the joint and reduces its mechanical properties.

Method used

Glass powder made primarily from bismuth oxide, boron oxide, and silicon oxide is ball-milled, melted, cooled, and then mixed with butyl acetate to form a glass solder paste. This paste is then coated onto the surface of sapphire to form a sandwich structure. The heating process is controlled to achieve good wetting and low thermal stress welding.

Benefits of technology

It improves the mechanical properties and long-term service stability of welded joints, with narrow and high-strength weld seams, simple process, low equipment investment, and is suitable for large-scale production.

✦ Generated by Eureka AI based on patent content.

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Abstract

This application discloses a novel glass brazing process for sapphire, specifically relating to the field of sapphire brazing. The process includes: ball milling and mixing bismuth oxide powder, boron oxide powder, and silicon oxide powder to obtain a mixture; heating the mixture to obtain molten glass; pouring the molten glass into cold water to obtain glass particles; ball milling the glass particles to obtain glass powder; mixing the glass powder with a binder to obtain glass solder paste; coating the glass solder paste onto the surface of the sapphire, forming a sapphire-glass solder paste-sapphire sandwich structure; and heating the sandwich structure to the brazing temperature to obtain the brazed sapphire. This process reduces thermal stress caused by the anisotropic coefficient of thermal expansion of the sapphire base material, resulting in welds with good mechanical properties and long-term service stability, narrow weld seams, and high strength.
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Description

Technical Field

[0001] This application relates to the field of sapphire brazing, and more particularly to a novel glass brazing process for sapphire. Background Technology

[0002] Sapphire is a modern structural material with good electrical conductivity, mechanical strength, and high-temperature resistance, and has a wide range of applications, with broad prospects in aerospace, automotive, chemical, and nuclear energy fields. However, because sapphire is a compound mainly composed of covalent bonds, its inherent brittleness makes it very difficult to manufacture large and complex-shaped parts. Therefore, these components are usually made using sapphire bonding technology.

[0003] The joining process for sapphire materials mainly needs to address two issues: the wettability of the joining interface and the stress buffering of the joint. Currently, many methods exist for joining sapphire, such as diffusion bonding, mechanical bonding, physical and chemical vapor deposition bonding, and brazing. Among these, brazing offers advantages such as simplicity, low equipment investment, and suitability for production requirements. Currently, sapphire brazing primarily uses specific active brazing filler metals. However, using metal brazing filler metals to braze ceramic joints easily generates continuous brittle intermetallic compounds, reducing the joint quality. Furthermore, the significant difference in the coefficients of linear expansion between ceramics and metals leads to substantial residual stress at the joint, reducing its mechanical properties. Summary of the Invention

[0004] The main objective of this application is to provide a novel glass brazing process for sapphire, which aims to solve the problem that the brazing of sapphire leads to a reduction in its mechanical properties.

[0005] To achieve the above objectives, this application provides a glass powder, the raw materials of which include bismuth oxide, boron oxide, and silicon oxide, and the mass ratio of bismuth oxide, boron oxide, and silicon oxide is 5:4:(1-2).

[0006] To achieve the above objectives, this application also provides a method for preparing the above-mentioned glass powder, comprising: ball milling and mixing bismuth oxide powder, boron oxide powder and silicon oxide powder in a mass ratio of 5:4:(1-2) to obtain a mixture; heating the mixture to obtain a molten glass liquid; pouring the glass liquid into cold water to obtain glass particles; and ball milling the glass particles to obtain glass powder.

[0007] Optionally, the ball milling is carried out in a ball mill with a rotation speed of 600-800 rpm and a milling time of 5-6 hours.

[0008] Optionally, during the heating process, the temperature is increased to 1000℃ at a rate of 5-10℃ / min and held for 1-2 hours.

[0009] To achieve the above objectives, this application also provides an application of the aforementioned glass powder in brazing sapphire.

[0010] To achieve the above objectives, this application also provides a novel glass brazing process for sapphire, comprising: mixing the aforementioned glass powder and butyl acetate to obtain glass solder paste; applying the glass solder paste to the surface of sapphire to form a sapphire-glass solder paste-sapphire sandwich structure; heating the sandwich structure to 300°C, holding it at that temperature for 10 minutes, and continuing to heat it to the brazing temperature to obtain the brazed sapphire.

[0011] The mass ratio of glass powder to binder is 5:0.3-0.6.

[0012] The binder is terpineol.

[0013] The heating rate during the heating process is 5℃ / min, and the brazing temperature is 550℃-650℃.

[0014] Compared with the prior art, the beneficial effects of this application are as follows:

[0015] The present invention employs a novel glass brazing process for sapphire, using the aforementioned glass powder to prepare a solder paste as a brazing filler metal. This process reduces thermal stress caused by the anisotropic thermal expansion coefficient of the sapphire base material, resulting in welds with excellent mechanical properties and long-term service stability. The welds are narrow and have high strength. The glass powder obtained in this application effectively wets the ceramic interface, reducing joint stress and ensuring high-quality joint connections with improved mechanical properties. The process is relatively simple, requires low equipment investment, and is suitable for large-scale production. Attached Figure Description

[0016] Figure 1 This is an electron microscope image of a sample obtained in Example 1 of a novel glass brazing process for sapphire according to this application.

[0017] Figure 2 This is a sample with precipitated whiskers obtained in Example 1 of a novel glass brazing process for sapphire according to this application.

[0018] The realization of the purpose, functional features and advantages of this application will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation

[0019] To make the objectives, technical solutions, and advantages of this application clearer, the technical solutions of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0020] The first embodiment of the present invention provides a glass powder, the raw materials of which include bismuth oxide, boron oxide and silicon oxide, and the mass ratio of bismuth oxide, boron oxide and silicon oxide is 5:4:(1-2).

[0021] The glass powder of this invention uses bismuth oxide, boron oxide, and silicon oxide as raw materials, and Bi₂O₃ as a flux. This reduces the melting temperature and viscosity of the glass powder, promotes its melting and flow, allows the brazing filler metal to better fill the weld seam, and improves its chemical stability. Increased chemical stability reduces the possibility of chemical reactions with sapphire and the surrounding environment during brazing, helping to ensure the stability and reliability of the weld joint. Simultaneously, it helps reduce the coefficient of thermal expansion of the glass powder, making it more compatible with the coefficient of thermal expansion of sapphire, reducing thermal stress caused by differences in thermal expansion coefficients during welding, and preventing defects such as cracks in the weld joint. SiO2 possesses high chemical and thermal stability, which can improve the overall stability of glass powder, making it less prone to decomposition and deterioration during high-temperature brazing and ensuring the smooth progress of the brazing process. It can also adjust the viscosity of glass powder, giving the brazing filler metal appropriate fluidity and viscosity after melting, which is beneficial for filling the weld seam and prevents excessive flow of the brazing filler metal, thereby obtaining good weld shape and dimensional accuracy. During the brazing process, SiO2 can undergo a certain chemical reaction with the sapphire surface to form chemical bonds, enhancing the interfacial bonding force between the brazing filler metal and sapphire, and improving the strength and reliability of the weld joint.

[0022] The synergistic effect of Bi₂O₃, B₂O₃, and SiO₂ significantly reduces the melting point and viscosity of the glass powder, allowing it to form a liquid brazing filler metal with good fluidity at lower temperatures. This facilitates easy spreading and wetting of the sapphire surface, providing a prerequisite for high-quality brazing. The addition of B₂O₃ and SiO₂ helps to adjust the thermal expansion coefficient of the glass powder, making it closer to that of sapphire, thus reducing thermal stress. Simultaneously, the low melting point of Bi₂O₃ helps to reduce the temperature gradient during brazing, further alleviating thermal stress and improving the stability and reliability of the weld joint. Bi₂O₃ and B₂O₃ improve the wettability of the brazing filler metal, enabling SiO₂ to better contact and react chemically with the sapphire surface, forming a strong chemical bond. The synergistic effect of these three components greatly enhances the interfacial bonding force between the brazing filler metal and sapphire, improving the strength and quality of the weld joint. Furthermore, it effectively wets the sapphire interface, reducing joint stress.

[0023] A second embodiment of the present invention provides a method for preparing the above-mentioned glass powder, specifically including the following steps:

[0024] Step S1: Bismuth oxide powder, boron oxide powder, and silicon oxide powder are placed in a planetary ball mill and mixed in a mass ratio of 5:4:(1-2) for 5-6 hours at a speed of 600-800 rpm to obtain a mixture.

[0025] Step S2: Pour the mixture into a platinum crucible, heat it to 1000℃ at a rate of 5-10℃ / min, and hold it at that temperature for 1-2 hours to obtain molten glass.

[0026] Step S3: Pour the molten glass into cold water to obtain glass particles, and then ball mill the glass particles to obtain glass powder.

[0027] The third embodiment of the present invention provides a novel glass brazing process for sapphire, specifically including the following steps:

[0028] Step S4: Mix glass powder and terpineol at a mass ratio of 5:0.3-0.6 to obtain glass solder paste;

[0029] Step S5: Apply glass solder paste to the surface of sapphire to form a sandwich structure of sapphire-glass solder paste-sapphire.

[0030] Step S6: The sandwich structure is heated to 300°C at a rate of 5°C / min and held at this temperature for 10 minutes to burn off the organic components. This is done to ensure that the brazing filler metal melts and flows evenly, better filling the weld seam; and to ensure that the temperature of each part of the weldment is uniform, reducing thermal stress and avoiding defects such as cracks, thereby improving the welding quality. The temperature is then increased to 550°C-650°C at a rate of 5°C / min. The sample is then cooled to room temperature with the furnace to obtain the welded sapphire.

[0031] In this embodiment, the above-mentioned glass powder is used to prepare solder paste as brazing filler metal. The solder paste achieves excellent wetting and flow between the sapphire crystals, completely filling the gaps between the sapphire crystals. Therefore, the joint formed is very uniform, and no defects such as inclusions or pores can be observed with the naked eye. This ensures a good connection effect, improves the strength and sealing of the joint, and guarantees the mechanical properties of the sapphire crystals.

[0032] Example 1

[0033] Step S1: Bi2O3, B2O3 and SiO2 are placed in a planetary ball mill and mixed in a mass ratio of 5:4:1 for 5 hours at a speed of 600 rpm to obtain a mixture.

[0034] Step S2: Pour the mixture into a platinum crucible, heat it to 1000°C at a rate of 5°C / min, and hold it at that temperature for 1 hour to obtain molten glass.

[0035] Step S3: Pour the molten glass into cold water to obtain 3mm glass particles. Ball mill the glass particles (size) to obtain glass powder.

[0036] Step S4: Mix glass powder and terpineol at a mass ratio of 5:0.3 to obtain glass solder paste;

[0037] Step S5: Apply glass solder paste to the surface of sapphire to form a sandwich structure of sapphire-glass solder paste-sapphire.

[0038] Step S6: The sandwich structure is heated to 300°C at a rate of 5°C / min, held at this temperature for 10 min, and then heated to 550°C at a rate of 5°C / min. The sample is cooled to room temperature with the furnace to obtain the brazed sapphire, i.e., the brazed sample.

[0039] The properties of the welded sapphire obtained in this embodiment were tested, and the results are as follows.

[0040] The coefficient of thermal expansion of the glass powder, as assessed using a dilatometer, is 9.3 × 10⁻⁶. -6 / °C.

[0041] The microstructure and fracture surface of the brazed samples were examined using a scanning electron microscope equipped with an Oxford energy-dispersive X-ray analysis system, such as... Figure 1 As shown, the glass powder (novel glass) obtained in this embodiment achieves excellent wetting and flow between the sapphire crystals, completely filling the gaps. The resulting joint is very uniform, and no defects such as inclusions or pores are visible to the naked eye.

[0042] Transmission electron microscopy with a super-XEDS system was used to further characterize and identify the precipitated whisker phase in the brazed joint. For example... Figure 2 As shown, whisker phases are generated at the joint during brazing. Under suitable conditions, these beneficial precipitates can enhance the joint performance.

[0043] In air, the dimensions are 6×6×3 mm. 3 A wetting experiment was conducted on the glass particles, and the wetting angle was 116.7°. 。

[0044] The relatively large wetting angle at this temperature indicates good wettability between the glass and sapphire.

[0045] Using a Helios Nanolab 600i with focused ion beam (FIB) technology at a heating rate of 10 °C / min, three identical 12*6 sapphire samples were prepared from the brazed sample at room temperature to 550 °C. The middle layer was covered with a novel glass powder composed of Bi₂O₃, B₂O₃, and SiO₂, and the top layer was a 6*6 sapphire sample, forming a TEM sample. The shear strength of the TEM sample joint was measured using a TMST universal testing machine at a constant speed of 0.5 mm / min. The average shear strength of the brazed joint was calculated to be 50 MPa.

[0046] After the shear test, the shear fracture surface was inspected using SEM. The surface was found to be relatively smooth and even, indicating that a good bond was achieved between the glass and sapphire during the brazing process. The stress distribution was relatively uniform, and there was no rough or uneven fracture caused by poor bonding or excessive internal stress concentration. This allowed the overall structure to maintain a relatively stable state until fracture when subjected to shear force, which reflects the reliable connection quality between the two.

[0047] Comparative Example 1

[0048] Using Bi2O3 and B2O3 as raw materials, brazed samples were obtained according to steps S1-S6. TEM samples were then prepared, and the average shear strength of the TEM sample joint was measured to be 47 MPa.

[0049] Example 2

[0050] Step S1: Bi2O3, B2O3, and SiO2 are placed in a planetary ball mill and mixed in a mass ratio of 5:4:1.2. The mixture is ball-milled at 650 rpm for 5 hours to obtain the mixture.

[0051] Step S2: Pour the mixture into a platinum crucible, heat it to 1000℃ at a rate of 6℃ / min, and hold it at that temperature for 1.2h to obtain molten glass.

[0052] Step S3: Pour the molten glass into cold water to obtain glass particles of 3mm size. Then, ball mill the glass particles (size) to obtain glass powder.

[0053] Step S4: Mix glass powder and terpineol at a mass ratio of 5:0.3 to obtain glass solder paste;

[0054] Step S5: Apply glass solder paste to the surface of sapphire to form a sandwich structure of sapphire-glass solder paste-sapphire.

[0055] Step S6: The sandwich structure is heated to 300°C at a rate of 5°C / min, held at this temperature for 10 min, and then heated to 575°C at a rate of 5°C / min. The sample is cooled to room temperature with the furnace to obtain the brazed sapphire, i.e., the brazed sample.

[0056] The properties of the welded sapphire obtained in this embodiment were tested, and the results are as follows.

[0057] The coefficient of thermal expansion of the glass powder was assessed using a dilatometer and found to be 8.4 × 10⁻⁶. -6 / °C.

[0058] In air, the dimensions are 6×6×3 mm. 3 A wetting experiment was conducted on the glass particles, and the wetting angle was 68.7°. 。

[0059] The relatively large wetting angle at this temperature indicates good wettability between the glass and sapphire.

[0060] Using a Helios Nanolab 600i with focused ion beam (FIB) technology at a heating rate of 10 °C / min, three identical 12*6 sapphire samples were prepared from the brazed sample at room temperature to 575 °C. The middle layer was covered with a novel glass powder composed of Bi₂O₃, B₂O₃, and SiO₂, and the top layer was a 6*6 sapphire sample, forming a TEM sample. The shear strength of the TEM sample joint was measured using a TMST universal testing machine at a constant speed of 0.5 mm / min. The average shear strength of the brazed joint was calculated to be 60 MPa.

[0061] After the shear test, the shear fracture surface was inspected using SEM. The surface was found to be relatively smooth and even, indicating that a good bond was achieved between the glass and sapphire during the brazing process. The stress distribution was relatively uniform, and there was no rough or uneven fracture caused by poor bonding or excessive internal stress concentration. This allowed the overall structure to maintain a relatively stable state until fracture when subjected to shear force, which reflects the reliable connection quality between the two.

[0062] Comparative Example 2

[0063] Using Bi2O3 and B2O3 as raw materials, brazed samples were obtained according to steps S1-S6. TEM samples were then prepared, and the average shear strength of the TEM sample joint was measured to be 54 MPa.

[0064] Example 3

[0065] Step S1: Bi2O3, B2O3 and SiO2 are placed in a planetary ball mill and mixed in a mass ratio of 5:4:1.4. The mixture is ball-milled at 700 rpm for 5.5 hours to obtain the mixture.

[0066] Step S2: Pour the mixture into a platinum crucible, heat it to 1000℃ at a rate of 5-10℃ / min, and hold it at that temperature for 2 hours to obtain molten glass.

[0067] Step S3: Pour the molten glass into cold water to obtain glass particles of 4mm size. Then, ball mill the glass particles (size) to obtain glass powder.

[0068] Step S4: Mix glass powder and terpineol at a mass ratio of 5:0.4 to obtain glass solder paste;

[0069] Step S5: Apply glass solder paste to the surface of sapphire to form a sandwich structure of sapphire-glass solder paste-sapphire.

[0070] Step S6: The sandwich structure is heated to 300°C at a rate of 5°C / min, held at this temperature for 10 min, and then heated to 600°C at a rate of 5°C / min. The sample is cooled to room temperature with the furnace to obtain the brazed sapphire, i.e., the brazed sample.

[0071] The properties of the welded sapphire obtained in this embodiment were tested, and the results are as follows.

[0072] The coefficient of thermal expansion of the glass powder was assessed using a dilatometer and found to be 7.8 × 10⁻⁶. -6 / °C.

[0073] In air, the dimensions are 6×6×3 mm. 3A wetting experiment was conducted on the glass particles, and the wetting angle was 43.2°. 。

[0074] The relatively large wetting angle at this temperature indicates good wettability between the glass and sapphire.

[0075] Using a Helios Nanolab 600i with focused ion beam (FIB) technology at a heating rate of 10 °C / min, three identical 12*6 sapphire samples were prepared from the brazed sample at room temperature to 600 °C. The middle layer was covered with a novel glass powder composed of Bi₂O₃, B₂O₃, and SiO₂, and the top layer was a 6*6 sapphire sample, forming a TEM sample. The shear strength of the TEM sample joint was measured using a TMST universal testing machine at a constant speed of 0.5 mm / min. The average shear strength of the brazed joint was calculated to be 75 MPa.

[0076] After the shear test, the shear fracture surface was inspected using SEM. The surface was found to be relatively smooth and even, indicating that a good bond was achieved between the glass and sapphire during the brazing process. The stress distribution was relatively uniform, and there was no rough or uneven fracture caused by poor bonding or excessive internal stress concentration. This allowed the overall structure to maintain a relatively stable state until fracture when subjected to shear force, which reflects the reliable connection quality between the two.

[0077] Comparative Example 3

[0078] Using Bi2O3 and B2O3 as raw materials, brazed samples were obtained according to steps S1-S6. TEM samples were then prepared, and the average shear strength of the TEM sample joint was measured to be 68 MPa.

[0079] Example 4

[0080] Step S1: Bi2O3, B2O3 and SiO2 are placed in a planetary ball mill and mixed in a mass ratio of 5:4:1.6. The mixture is ball-milled at 800 rpm for 6 hours to obtain the mixture.

[0081] Step S2: Pour the mixture into a platinum crucible, heat it to 1000℃ at a rate of 10℃ / min, and hold it at that temperature for 2 hours to obtain molten glass.

[0082] Step S3: Pour the molten glass into cold water to obtain glass particles of 4mm size. Then, ball mill the glass particles (size) to obtain glass powder.

[0083] Step S4: Mix glass powder and terpineol at a mass ratio of 5:0.4 to obtain glass solder paste;

[0084] Step S5: Apply glass solder paste to the surface of sapphire to form a sandwich structure of sapphire-glass solder paste-sapphire.

[0085] Step S6: The sandwich structure is heated to 300°C at a rate of 5°C / min, held at this temperature for 10 min, and then heated to 625°C at a rate of 5°C / min. The sample is cooled to room temperature with the furnace to obtain the brazed sapphire, i.e., the brazed sample.

[0086] The properties of the welded sapphire obtained in this embodiment were tested, and the results are as follows.

[0087] The coefficient of thermal expansion of the glass powder was assessed using a dilatometer and found to be 6.8 × 10⁻⁶. -6 / °C.

[0088] In air, the dimensions are 6×6×3 mm. 3 Wetting experiments were conducted on the glass particles, with a wetting angle of 23.1°. 。

[0089] The relatively large wetting angle at this temperature indicates good wettability between the glass and sapphire.

[0090] Using a Helios Nanolab 600i with focused ion beam (FIB) technology at a heating rate of 10 °C / min, three identical 12*6 sapphire samples were prepared from brazed samples, heated from room temperature to 625 °C. The samples were then covered with a novel glass powder composed of Bi₂O₃, B₂O₃, and SiO₂, and topped with 6*6 sapphire samples to form a TEM sample for mechanical property testing. The shear strength of the joint was measured using a TMST universal testing machine at a constant speed of 0.5 mm / min, and the average shear strength of the brazed joint was calculated to be 70 MPa.

[0091] After the shear test, the shear fracture surface was inspected using SEM. The surface was found to be relatively smooth and even, indicating that a good bond was achieved between the glass and sapphire during the brazing process. The stress distribution was relatively uniform, and there was no rough or uneven fracture caused by poor bonding or excessive internal stress concentration. This allowed the overall structure to maintain a relatively stable state until fracture when subjected to shear force, which reflects the reliable connection quality between the two.

[0092] Comparative Example 4

[0093] Using Bi2O3 and B2O3 as raw materials, brazed samples were obtained according to steps S1-S6. TEM samples were then prepared, and the average shear strength of the TEM sample joint was measured to be 59 MPa.

[0094] Example 5

[0095] Step S1: Bi2O3, B2O3 and SiO2 are placed in a planetary ball mill and mixed in a mass ratio of 5:4:2. The mixture is ball-milled at 800 rpm for 6 hours to obtain the mixture.

[0096] Step S2: Pour the mixture into a platinum crucible, heat it to 1000℃ at a rate of 10℃ / min, and hold it at that temperature for 1-2 hours to obtain molten glass.

[0097] Step S3: Pour the molten glass into cold water to obtain glass particles of 4mm size. Then, ball mill the glass particles (size) to obtain glass powder.

[0098] Step S4: Mix glass powder and terpineol at a mass ratio of 5:0.4 to obtain glass solder paste;

[0099] Step S5: Apply glass solder paste to the surface of sapphire to form a sandwich structure of sapphire-glass solder paste-sapphire.

[0100] Step S6: The sandwich structure is heated to 300°C at a rate of 5°C / min, held at this temperature for 10 min, and then heated to 650°C at a rate of 5°C / min. The sample is cooled to room temperature with the furnace to obtain the brazed sapphire, i.e., the brazed sample.

[0101] The properties of the welded sapphire obtained in this embodiment were tested, and the results are as follows.

[0102] The coefficient of thermal expansion of the glass powder, as assessed using a dilatometer, is 5.9 × 10⁻⁶. -6 / °C.

[0103] In air, the dimensions are 6×6×3 mm. 3 A wetting experiment was conducted on the glass particles, and the wetting angle was 11.7°. 。

[0104] The relatively large wetting angle at this temperature indicates good wettability between the glass and sapphire.

[0105] Using a Helios Nanolab 600i with focused ion beam (FIB) technology at a heating rate of 10 °C / min, three identical 12*6 sapphire samples were prepared from the brazed sample at room temperature to 650 °C. The middle layer was covered with a novel glass powder composed of Bi₂O₃, B₂O₃, and SiO₂, and the top layer was a 6*6 sapphire sample, forming a TEM sample. The shear strength of the TEM sample joint was measured using a TMST universal testing machine at a constant speed of 0.5 mm / min. The average shear strength of the brazed joint was calculated to be 65 MPa.

[0106] After the shear test, the shear fracture surface was inspected using SEM. The surface was found to be relatively smooth and even, indicating that a good bond was achieved between the glass and sapphire during the brazing process. The stress distribution was relatively uniform, and there was no rough or uneven fracture caused by poor bonding or excessive internal stress concentration. This allowed the overall structure to maintain a relatively stable state until fracture when subjected to shear force, which reflects the reliable connection quality between the two.

[0107] Comparative Example 5

[0108] Using Bi2O3 and B2O3 as raw materials, brazed samples were obtained according to steps S1-S6. TEM samples were then prepared, and the average shear strength of the TEM sample joint was measured to be 47 MPa.

[0109] The above are merely preferred embodiments of this application and do not limit the patent scope of this application. Any equivalent structural or procedural transformations made using the content of this application's specification and drawings, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of this application.

Claims

1. A soldering process employing a novel glass soldering of sapphire, characterized in that, The application relates to a glass solder paste and a preparation method thereof. The raw materials of the glass powder include bismuth oxide, boron oxide and silicon oxide, and the mass ratio of the bismuth oxide, the boron oxide and the silicon oxide is 5:4:(1-2). The glass solder paste is coated on the surface of sapphire to form a sandwich structure of sapphire-glass solder paste-sapphire; The sandwich structure is heated to 300 DEG C and kept for 10 min, and then the temperature is continuously increased to a brazing temperature to obtain sapphire after welding; The heating rate is 5 DEG C / min, and the brazing temperature is 550 DEG C-650 DEG C. The preparation method of the glass powder comprises the following steps:

2. The soldering process employing novel glass brazing sapphire as claimed in claim 1, wherein, Bismuth oxide powder, boron oxide powder and silicon oxide powder are ball-mixed according to the mass ratio of 5:4:(1-2) to obtain a mixture; The mixture is heated to obtain a molten glass liquid; The glass liquid is poured into cold water to obtain glass particles; The glass particles are ball-milled to obtain the glass powder. The ball-mixing is carried out in a ball mill, the rotating speed of the ball mill is 600-800 rpm, and the ball-milling time is 5-6 h.

3. The soldering process employing novel glass brazing sapphire as claimed in claim 2, wherein, In the heating process, the temperature is increased to 1000 DEG C at a speed of 5-10 DEG C / min, and the temperature is kept for 1-2 h.

4. The soldering process employing novel glass brazing sapphire as claimed in claim 2, wherein, The mass ratio of the glass powder and the terpineol is 5:0.3-0.

6.

5. The soldering process employing novel glass brazing sapphire as claimed in claim 1, wherein, ​

Citation Information

Patent Citations

  • Low-temperature welding method for sapphires

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