Glass solder for YAG transparent ceramic welding and preparation method thereof

Abstract

The invention discloses a glass solder for YAG transparent ceramic welding and a preparation method thereof, and belongs to the technical field of welding. The glass solder is composed of the following components in percentage by weight: 18%-24% of Ta2O5, 12%-16% of B2O3, 54%-60% of SiO2, 1%-4% of BaO and 3%-6% of R2O. The preparation method of the solder comprises the following steps: weighing the oxide powder by using a balance; ball-milling the weighed powder for 2-3 hours by taking absolute ethyl alcohol as a medium; the ball-milled powder is heated to 1500-1600 DEG C in a muffle furnace, heat preservation is conducted for 30-60 min, then the powder is taken out of the furnace and poured into a casting mold, and the casting mold is rapidly put into the muffle furnace at the temperature of 500-600 DEG C to be subjected to heat preservation for 6-8 h; and taking out the annealed glass block and cutting the glass block in a corresponding size. The refraction coefficient and the thermal expansion coefficient of the prepared glass solder are matched with those of YAG transparent ceramic.

Description

Technical Field

[0001] The invention relates to the technical field of welding, and in particular to a glass solder for YAG transparent ceramic welding and a preparation method thereof. Background Art

[0002] YAG transparent ceramics have the advantages of high transparency, high melting point, excellent mechanical and chemical properties, etc. It is currently the most widely used solid laser gain medium and is widely used in fields such as material processing and laser weapons. YAG transparent ceramics are mainly prepared by hot isostatic pressing, hot pressing and spark plasma sintering. Limited by the preparation method of ceramic materials, large-size components are still difficult to prepare. Connection technology is an important method to solve this problem.

[0003] Among the many methods of connecting ceramic materials, glass solder has good chemical compatibility with ceramic materials. In addition, glass solder has a controllable thermal expansion coefficient, so it is more suitable for connecting ceramics themselves. Glass solder has been used to connect transparent ceramic materials such as transparent sapphire ceramics and transparent aluminum nitride ceramics, and has obtained good optical and mechanical properties.

[0004] However, in order to obtain a joint with good light transmittance, the refractive index of the glass solder must match that of the ceramic base material. At the same time, in order to ensure a good joint connection and high strength, the thermal expansion coefficient of the glass solder needs to match that of the ceramic base material. Summary of the invention

[0005] The object of the present invention is to provide a glass solder for YAG transparent ceramic welding and a preparation method thereof, wherein the refractive index and thermal expansion coefficient of the glass solder match those of the YAG transparent ceramic.

[0006] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0007] A glass solder for YAG transparent ceramic welding, wherein the glass solder has the following composition by weight percentage:

[0008] Ta2O5: 18-24%, B2O3: 12-16%, SiO2: 54-60%, BaO: 1-4%, R2O: 3-6%.

[0009] The R2O is one or more of Li2O, Na2O and K2O.

[0010] A method for preparing glass solder suitable for YAG transparent ceramic welding, the specific steps are as follows:

[0011] (1) Weighing: Weigh each raw material in mass percentage according to the composition of the glass solder, and pour the weighed powder into a polytetrafluoroethylene ball mill;

[0012] (2) Mixing: Use anhydrous ethanol as the medium, ball mill for 2-3 hours, and then evaporate the mixed liquid on a heating table;

[0013] (3) Melting: Pour the powder obtained after evaporation into an alumina crucible, heat it to 1500-1600°C in a muffle furnace at a certain heating rate, and keep it warm for 30-60 minutes;

[0014] (4) Casting: Pour the molten glass into a mold, and after rapid cooling and solidification into a glass block, quickly place it in a muffle furnace at 500-600°C;

[0015] (5) Annealing: Keep in a muffle furnace at 500-600°C for 6-8 hours, and then cool to room temperature;

[0016] (6) Cutting: Cut the cooled glass block into corresponding sizes.

[0017] In the step (1), the grinding balls in the polytetrafluoroethylene ball mill are made of zirconium oxide.

[0018] In the step (3), the heating rate is no more than 15°C / min.

[0019] In the step (4), the casting mold is made of copper alloy and is cleaned with anhydrous ethanol before use.

[0020] The advantages and beneficial effects of the present invention are as follows:

[0021] 1. The glass solder prepared by the present invention has a refractive index higher than 1.75% and a thermal expansion coefficient higher than 7.5×10 -6 / ℃.

[0022] 2. The refractive index and thermal expansion coefficient of the glass solder of the present invention match those of YAG transparent ceramics. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 Thermal expansion curves of the glass solder prepared in Example 1 and YAG transparent ceramic.

[0024] Figure 2 This is a wetting photograph of the glass solder used in Example 1 on the YAG transparent ceramic surface (1300°C). DETAILED DESCRIPTION

[0025] The present invention is further described below in conjunction with the accompanying drawings and specific embodiments so that those skilled in the art can better understand the present invention and implement it, but the embodiments are not intended to limit the present invention.

[0026] Example 1

[0027] This embodiment includes the following steps:

[0028] (1) Material preparation: The size of YAG transparent ceramic is 10 mm × 10 mm × 20 mm. The surface of YAG transparent ceramic is polished with 800#, 1000#, and 1500# sandpapers in sequence, and then the surface of the ceramic is polished with diamond polishing liquid with particle sizes of 2.5 μm, 1.5 μm, and 0.5 μm in sequence. The polished YAG transparent ceramic is ultrasonically cleaned with acetone as the medium for 20 minutes, and then blown dry for use.

[0029] (2) Preparation of glass solder: The components and mass fractions of the glass solder used are: Ta2O5: 21%, B2O3: 13.4%, SiO2: 55.6%, BaO: 4%, Li2O: 6%. The oxide raw materials are weighed using an electronic balance according to the above proportions, where B2O3 is introduced by H3BO3 and Li2O is introduced by Li2CO3. The weighed raw materials are placed in a polytetrafluoroethylene ball mill and milled with anhydrous ethanol as the medium and zirconium oxide balls as the grinding balls. The ball milling speed is 450r / min and the ball milling time is 3h. The mixed powder is dried on a heating table for 4h. The dried raw materials are poured into an alumina crucible and heated to 1500℃ in a muffle furnace in an air atmosphere. After keeping the temperature for 60min, the glass melt is poured into a casting mold to obtain a glass block. The glass block is quickly placed in a muffle furnace at a temperature of 600℃, kept at the temperature for 6h, and then cooled to room temperature with the furnace.

[0030] (3) Cutting: Cut glass blocks with a size of 5 mm × 5 mm × 10 mm from the cooled glass block.

[0031] (4) Wetting test: Place the cut glass block on a polished YAG transparent ceramic, heat it to 1300°C at 10°C / min, keep it warm for 5 minutes, and then take it out of the furnace. Cut the sample in the middle and take a photo of the cross section. Use software to analyze the wetting angle in the photo.

[0032] (5) Refractive index test: Use a refractometer to test the refractive index of YAG transparent ceramic base material and glass solder.

[0033] (6) Thermal expansion coefficient test: The thermal expansion coefficient of YAG transparent ceramic base material and glass solder was tested using a thermal expansion tester at a heating rate of 10°C / min.

[0034] The refractive index of this glass solder is 1.7865. Figure 1 The thermal expansion curves of the glass solder YAG transparent ceramic used in Example 1 show that the thermal expansion behaviors of the two are basically the same, and the thermal expansion coefficients are 7.86×10 -6 / ℃. Figure 2When the temperature is 1300°C, the wetting angle of the glass solder used in Example 1 on the YAG transparent ceramic surface is less than 25°, and the wettability is good, which can meet the needs of welding applications.

[0035] Example 2

[0036] In step (2), the components and mass fractions of the glass solder used are: Ta2O5: 24%, B2O3: 13.4%, SiO2: 55.6%, BaO: 4%, Li2O: 3%. The other steps are the same as those in Example 1. The refractive index of the glass solder obtained in this example is 1.7798, and the thermal expansion coefficient is 7.82×10 -6 / ℃.

[0037] Example 3

[0038] In step (2), the components and mass fractions of the glass solder used are: Ta2O5: 21%, B2O3: 13.4%, SiO2: 55.6%, BaO: 4%, K2O: 6%. The other steps are the same as those in Example 1. The refractive index of the glass solder obtained in Example 3 is 1.7862, and the thermal expansion coefficient is 7.87×10 -6 / ℃.

[0039] Comparative Example 1

[0040] In step (2), the components and mass fractions of the glass solder used are: Ta2O5: 18%, B2O3: 23.4%, SiO2: 51.6%, BaO: 4%, Li2O: 3%. The other steps are the same as those in Example 1. The refractive index of the glass solder obtained in this example is 1.6521, and the thermal expansion coefficient is 7.32×10 -6 / ℃.

[0041] Comparative Example 2

[0042] In step (2), the components and mass fractions of the glass solder used are: Ta2O5: 17%, B2O3: 13.4%, SiO2: 59.6%, BaO: 4%, Na2O: 3%, K2O: 3%. The other steps are the same as those in Example 1. The refractive index of the glass solder obtained in Comparative Example 3 is 1.7152, and the thermal expansion coefficient is 8.17×10 -6 / ℃.

[0043] Table 1 Refractive index and thermal expansion coefficient data of the embodiments and comparative examples

[0044] Refractive index <![CDATA[Coefficient of thermal expansion (×10 -6 / °C)]]> YAG transparent ceramics 1.7985 7.9 Example 1 1.7865 7.86 Example 2 1.7798 7.82 Example 3 1.7862 7.87 Comparative Example 1 1.6521 7.32 Comparative Example 2 1.7152 8.17

Claims

1. A glass solder for YAG transparent ceramic welding, characterized in that: By weight percentage, the composition of the glass solder is as follows: Ta2O5: 18-24%, B2O3: 12-16%, SiO2: 54-60%, BaO: 1-4%, R2O: 3-6%.

2. The glass solder for YAG transparent ceramic welding according to claim 1, characterized in that: The R2O is one or more of Li2O, Na2O and K2O.

3. The glass solder for YAG transparent ceramic welding according to claim 1, characterized in that: B2O3 was introduced by H3BO3, BaO was introduced by BaCO3, Li2O, Na2O and K2O were introduced by Li2CO3, Na2CO3 and K2CO3 respectively.

4. The method for preparing glass solder for YAG transparent ceramic welding according to any one of claims 1 to 3, characterized in that: The preparation method specifically comprises the following steps: (1) Weighing: Weigh each raw material in mass percentage according to the composition of the glass solder, and pour the weighed powder into a polytetrafluoroethylene ball mill; (2) Mixing: Use anhydrous ethanol as the medium, ball mill for 2-3 hours, and then evaporate the mixed liquid on a heating table; (3) Melting: Pour the powder obtained after evaporation into an alumina crucible, heat it to 1500-1600°C in a muffle furnace at a certain heating rate, and keep it warm for 30-60 minutes; (4) Casting: Pour the molten glass into a mold, and after rapid cooling and solidification into a glass block, quickly place it in a muffle furnace at 500-600°C; (5) Annealing: Keep in a muffle furnace at 500-600°C for 6-8 hours, and then cool to room temperature; (6) Cutting: Cut the cooled glass block into corresponding sizes.

5. The method for preparing glass solder for YAG transparent ceramic welding according to claim 4, characterized in that: In step (1), the grinding balls in the polytetrafluoroethylene ball mill are made of zirconium oxide.

6. The method for preparing glass solder for YAG transparent ceramic welding according to claim 4, characterized in that: In step (3), the heating rate is no more than 15°C / min.

7. The method for preparing glass solder for YAG transparent ceramic welding according to claim 4, characterized in that: In step (4), the casting mold is made of copper alloy and is cleaned with anhydrous ethanol before use.

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