Method of sintering glass to tantalum material

Abstract

This invention provides a method for sintering glass and tantalum, comprising the following steps: S1, pretreatment: obtaining a pretreated glass embryo and a pretreated tantalum material; S2, preheating and degassing: assembling the glass embryo and the pretreated tantalum material into a mold, placing the mold in a sintering furnace, and raising the furnace temperature to a first preset temperature value at a rate of 2-4℃ / min; S3, dynamic vacuum sintering: raising the furnace temperature to a second preset temperature value at a rate of 2-4℃ / min; S4, heat preservation and stress relief: lowering the furnace temperature to a third preset temperature value at a rate of 1-3℃ / min; S5, cooling: lowering the furnace temperature to room temperature at a rate of 4-6℃ / min. Therefore, the glass-tantalum sintering method of this application can prevent cracking caused by thermal stress concentration at the interface between the glass embryo and the tantalum material, and the formation of honeycomb-like pores in the glass during vacuum sintering.

Description

Technical Field

[0001] This invention relates to the field of tantalum insulator manufacturing technology, specifically to a method for sintering glass and tantalum material. Background Technology

[0002] Tantalum insulators, as core components of high-end electronic devices, must meet the performance requirements of "high insulation, high corrosion resistance, and high reliability." The key to their manufacturing lies in the encapsulation and sintering process of glass and tantalum material. In existing technologies, the sintering of glass and tantalum material mainly employs "constant-temperature vacuum sintering" or "simple gradient temperature sintering," but this method suffers from the following unresolved technical drawbacks: 1. Interface cracking problem: The thermal expansion coefficients of tantalum and glass differ significantly (tantalum: 6.5×10). -6 / ℃, Glass: 4.5×10 -6 (℃), in traditional processes, the temperature rises too quickly in simple gradient heating sintering, generally using 5-8℃ / min for gradient heating, or constant temperature vacuum sintering, which leads to concentration of thermal stress at the interface, cracking rate ≥15%, seriously affecting product reliability. 2. Honeycomb-like defects in glass: Under vacuum conditions, adsorbed water, crystal water, and low-boiling-point impurities (such as B2O3) in glass powder rapidly escape at high temperatures, forming a honeycomb structure with a porosity ≥3%, leading to a decrease in airtightness (only 10). -7 Pa m³ / s). Summary of the Invention

[0003] The technical problem to be solved by the present invention is to provide a method for sintering glass and tantalum materials to solve the problems of cracking caused by thermal stress concentration at the glass-tantalum interface and the formation of honeycomb-like pores in the glass during vacuum sintering.

[0004] The technical problem to be solved by this invention, and the technical solution adopted, are as follows: A method for sintering glass and tantalum material includes the following steps: S1, pretreatment: sieving glass powder, adding binder and stirring, drying, cold pressing, and sintering to obtain a glass embryo; surface treating and cleaning the tantalum material with an acidic solution to obtain pretreated tantalum material; S2, preheating and degassing: assembling the glass embryo and pretreated tantalum material into a mold, placing the mold in a sintering furnace, evacuating the sintering furnace to a preset vacuum value, and holding at this temperature for a first preset time value; then maintaining a first pressure value inside the sintering furnace and continuously introducing protective gas, and then raising the temperature of the sintering furnace to a first preset temperature value at a rate of 2-4℃ / min, and holding at this temperature for a second preset time value; S3, dynamic vacuum sintering: raising the temperature of the sintering furnace to a second preset temperature value at a rate of 2-4℃ / min, while maintaining a second pressure value inside the sintering furnace and continuously introducing protective gas. S4, Insulation and Stress Relief: The sintering furnace temperature is reduced to the third preset temperature value at a rate of 1-3℃ / min, while maintaining the third pressure value inside the sintering furnace and continuously introducing protective gas, and the temperature is maintained for a fourth preset time value, where the third preset temperature value is greater than the first preset temperature value; the third pressure value is greater than or equal to the second pressure value; S5, Cooling: The sintering furnace temperature is reduced to the fourth preset temperature value at a rate of 4-6℃ / min, while continuously introducing protective gas, and the pressure value inside the sintering furnace is depressurized to atmospheric pressure. When the temperature inside the sintering furnace drops to the fourth preset temperature value, the introduction of protective gas is stopped, allowing the sintering furnace to continue cooling to room temperature. In one embodiment, the first pressure value is ≥1×10²Pa.

[0005] In one embodiment, the preheating and degassing step is pre-set with a vacuum value ≤ 1 × 10⁻⁶. -2 Pa; the first preset time value is 10-15 min; the first preset temperature value is 200-400℃; the second preset time value is 0.3-0.5 h.

[0006] In one embodiment, in the dynamic vacuum sintering step, the second preset temperature value is 720-850℃; and the third preset time value is 2-3h.

[0007] In one embodiment, in the heat preservation and stress relief step, the third preset temperature value is 600-620℃; and the fourth preset time value is 1-2h.

[0008] In one embodiment, the fourth preset temperature value is 120°C.

[0009] In one embodiment, the glass powder pretreatment specifically involves: sieving the glass powder through a 120-mesh sieve, adding a binder to the sieved glass powder to form granulated powder, drying the granulated powder at 100-120℃ for 2 hours to achieve a moisture content of ≤0.1%, then cold-pressing the dried granulated powder at 100-180MPa into a preform, and finally air-sintering it in a 650℃ sintering furnace to obtain a glass preform.

[0010] In one embodiment, the granulated powder is dried at 120°C for 2 hours to reduce the moisture content of the granulated powder to ≤0.1%, and then the dried granulated powder is cold-pressed into embryos at 180MPa.

[0011] In one embodiment, the tantalum material includes a tantalum wire and a tantalum cap, the tantalum cap having a receiving cavity, the glass embryo being located within the receiving cavity, and the tantalum wire being inserted into the glass embryo.

[0012] In one embodiment, the tantalum material is surface-treated with an acidic solution to remove oxides and impurities from its surface, and then pre-treated by magnetic polishing and plasma cleaning for 10-20 minutes.

[0013] Compared with the prior art, the beneficial effects of the present invention are as follows: This invention prevents cracking caused by thermal stress concentration at the interface between the glass embryo and the tantalum material, and avoids the formation of honeycomb-like pores in the glass during vacuum sintering by preheating and degassing the glass and the pretreated tantalum material, dynamic vacuum sintering, heat preservation and stress relief, and cooling steps. In the preheating and degassing step, the moisture in the pretreated glass embryo and the pretreated tantalum material can be fully removed by vacuuming; the slow heating can prevent the moisture in the pretreated glass embryo and the pretreated tantalum material from boiling over and rapidly escaping to form bubbles; and the control of pressure and protective gas can suppress the volatilization of impurities in the pretreated glass embryo and the pretreated tantalum material. In the dynamic vacuum sintering process, medium-speed heating can simultaneously address both venting and melting. This means that thorough venting and impurity removal are performed at the softening points of the pretreated glass embryo and the pretreated tantalum material. By maintaining constant pressure and a constant flow rate of protective gas, venting and volatilization are simultaneously achieved, allowing the obstructing gases between the glass embryo and the tantalum material to be quickly expelled, resulting in better adhesion between them. This also allows the glass embryo to better penetrate the tantalum material, resulting in a stronger bond and ensuring that the pretreated glass embryo and the pretreated tantalum material are fully filled, free of pores and unfused areas. In the heat preservation and stress relief step, slow cooling ensures full stress release, i.e., the thermal stress at the glass-tantalum interface is gradually released; constant pressure and constant flow rate of protective gas promote the flow of the glass liquid phase, closure of shrinkage cavities, and densification of the structure, eliminating honeycomb defects at the source; ensuring that the final product is stress-free, crack-free, highly dense, and highly airtight. During the cooling process, rapid cooling can lock in the dense structure, that is, quickly pass through the crystallization-sensitive region, and avoid secondary crystallization of the glass, which would lead to a decrease in strength. Attached Figure Description

[0014] Figure 1 This is a schematic diagram of the process of the present invention; Figure 2 This is a schematic diagram of the tantalum cap structure of the present invention; Figure 3 This is a schematic diagram of the structure of the glass and tantalum material after sintering according to the present invention; Figure 4 For the present invention Figure 3 A schematic diagram of the cross-sectional structure; Figure 5 This is a strength test diagram of a glass embryo after sintering glass and tantalum material using existing technology. Figure 6 This is a strength test diagram of the glass embryo after sintering the glass and tantalum material according to the present invention.

[0015] In the diagram, 10 is the tantalum cap; 20 is the glass embryo; 30 is the tantalum wire; and 40 is the receiving cavity. Detailed Implementation

[0016] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0017] Example 1 like Figure 1 As shown, this embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; in this embodiment, the glass powder formula is: SiO2, -B2O3, -ZnO; tantalum material includes tantalum caps and tantalum wires. In this embodiment, the glass powder pretreatment specifically involves: sieving the glass powder through a 120-mesh sieve, adding binder to the sieved glass powder, then passing it through a ball mill and high-speed stirring to form granulated powder. The granulated powder is then dried at 120°C for 2 hours to achieve a moisture content ≤0.05%. After drying, the granulated powder is cold-pressed at 180MPa to form an embryo, and finally placed in a 650°C sintering furnace for air pre-sintering to obtain a glass embryo.

[0018] Tantalum cap: After being stamped, the tantalum cap is surface treated with an acidic solution to remove oxides and impurities from its surface. It is then subjected to magnetic polishing and plasma cleaning for 10 minutes before drying to obtain the pre-treated tantalum cap.

[0019] Tantalum wire: After wire cutting, the oxide layer of tantalum wire is removed with an acidic solution, and then it is dried after being cleaned with a magnetic polisher and plasma for 20 minutes; the pretreated tantalum wire is obtained.

[0020] like Figure 2 As shown, the tantalum cap 10 is annular and has a receiving cavity 40. The glass embryo 20 is located in the receiving cavity 40, and the tantalum wire 30 is inserted into the glass embryo 20. That is, the glass embryo 20 is placed in the receiving cavity 40, and then the tantalum wire 30 is inserted into the glass embryo 20. In this embodiment, the tantalum wire 30 passes through the glass embryo 20. The tantalum wire 30 is used to make an electrical connection between the glass embryo 20 and the tantalum cap 10 after sintering.

[0021] S2, Preheating and Degassing: Assemble the glass embryo and the pretreated tantalum material into the mold, place the mold into the sintering furnace, evacuate the sintering furnace to the preset vacuum value, and hold it for the first preset time value; then maintain the first pressure value in the sintering furnace and continuously introduce protective gas, and then raise the temperature of the sintering furnace to the first preset temperature value at a rate of 2-4℃ / min, and hold it for the second preset time value. In this embodiment, the preset vacuum value is ≤1×10 -2 Pa; First preset time value is 10-15 min; First pressure value is ≥1×10² Pa; First preset temperature value is 200-400℃; Second preset time value is 0.3-0.5 h; Protective gas is argon; In this embodiment, the glass embryo and the pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 The pressure inside the sintering furnace is maintained at 1×10²Pa for 10 minutes, then argon gas is introduced at a rate of 20 L / min to maintain the pressure inside the furnace at 1×10²Pa (it should be noted that the introduction of argon gas and the maintenance of the pressure inside the sintering furnace will inevitably result in exhaust). The temperature of the sintering furnace is then increased to 300℃ at a rate of 2℃ / min (i.e., slow heating, which can prevent the moisture in the glass embryo and pretreated tantalum material from boiling over), and held at this temperature for 0.5 hours. Thus, by evacuating, the moisture in the pretreated glass embryo and pretreated tantalum material can be fully removed; by heating slowly (at a rate of 2℃ / min), the boiling over and rapid escape of the moisture in the pretreated glass embryo and pretreated tantalum material can be prevented from forming bubbles; and by controlling the pressure and protective gas, the volatilization of impurities in the pretreated glass embryo and pretreated tantalum material can be suppressed. S3, Dynamic Vacuum Sintering: The temperature of the sintering furnace is raised to the second preset temperature value at a rate of 2-4℃ / min, while maintaining the second pressure value inside the sintering furnace and continuously introducing protective gas, and holding for a third preset time value; in this embodiment, the second preset temperature value is 720-850℃; the third preset time value is 2-3h; the second preset temperature value is greater than the first preset temperature value; the second pressure value is greater than or equal to the first pressure value; In this embodiment, the sintering furnace temperature is raised to 800°C at a rate of 3°C / min, while maintaining the pressure inside the sintering furnace at 1×10²Pa, and argon gas is introduced at a rate of 30L / min for 2 hours. Thus, by raising the temperature at a medium rate (3°C / min), both venting and melting can be achieved, that is, sufficient venting and impurity removal are performed at the softening point of the pretreated glass embryo and the pretreated tantalum material. By maintaining constant pressure and constant flow rate of protective gas, venting and volatilization are simultaneously achieved, while allowing the obstructing gas between the glass embryo and the tantalum material to be quickly discharged, allowing the glass embryo and the tantalum material to adhere better. This allows the glass embryo to penetrate the tantalum material better, resulting in a stronger bond, ensuring that the pretreated glass embryo and the pretreated tantalum material are fully filled, without pores or unfused areas. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to the third preset temperature value at a rate of 1-3℃ / min, while maintaining the third pressure value inside the sintering furnace and continuously introducing protective gas, and the heat preservation is carried out for a fourth preset time value; in this embodiment, the third preset temperature value is 600-620℃; the fourth preset time value is 1-2h; the third preset temperature value is greater than the first preset temperature value; the third pressure value is greater than or equal to the second pressure value; In this embodiment, the sintering furnace temperature is reduced to 620°C at a rate of 1°C / min, while maintaining the pressure inside the sintering furnace at 2×10²Pa (to better suppress bubbles and reduce thermal stress), and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1 hour. Slow cooling (at a rate of 1°C / min) ensures sufficient stress release, i.e., the thermal stress at the glass-tantalum interface is gradually released. Constant pressure and a constant flow rate of protective gas promote glass liquid phase flow, pore closure, and structural densification, eliminating honeycomb defects at their source. This ensures that the final product is stress-free, crack-free, highly dense, and highly airtight. S5, Cooling: The temperature of the sintering furnace is reduced to the fourth preset temperature value at a rate of 4-6℃ / min, while protective gas is continuously introduced and the pressure inside the sintering furnace is released to atmospheric pressure. When the temperature inside the sintering furnace drops to the fourth preset temperature value, the protective gas is stopped, and the sintering furnace continues to cool to room temperature. In this embodiment, the fourth preset temperature value is 120℃. In this embodiment, the sintering furnace temperature is reduced to 120°C at a rate of 4°C / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120°C, the argon gas supply is stopped, and cooling continues to room temperature (i.e., rapidly passing through the crystallization-sensitive zone to avoid secondary crystallization of the glass leading to a decrease in strength; maintaining argon gas protection before 120°C to prevent high-temperature oxidation of the tantalum material; stopping gas supply in the low-temperature section to save gas and avoid uneven cooling). Figures 3-6As shown, the glass-tantalum material sintered using this method, after testing, exhibits a glass porosity of 0.8%, an interface cracking rate of 0.3%, an interface bond strength of 340 kgf (compared to 240 kgf in the prior art), and an airtightness of 3.2 × 10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00018, yield 98.5%.

[0022] Example 2 like Figure 1 As shown, this embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 250 °C at a rate of 2 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 800℃ at a rate of 3℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 620℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The resulting glass-tantalum material sintered using this method, after testing, exhibits a glass porosity of 0.6%, an interface cracking rate of 0.2%, an interface bond strength of 350 kgf (compared to 240 kgf in existing technology), and an airtightness of 2.8×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00018, yield 99.1%.

[0023] Example 3 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 250 °C at a rate of 2 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 850℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 600℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 5℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.7%, an interface cracking rate of 0.3%, an interface bond strength of 320 kgf, and an airtightness of 3.8×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00016, yield 98.9%.

[0024] Example 4 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 250 °C at a rate of 2 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 850℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 600℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 6℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.76%, an interface cracking rate of 0.28%, an interface bond strength of 310 kgf, and an airtightness of 4.1×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00018, yield 98.6%.

[0025] Comparative Example 1 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; In this embodiment, tantalum material includes tantalum cap and tantalum wire.

[0026] S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -1 Pa, maintain for 15 min, then introduce argon gas at 30 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 400 °C at a rate of 5 °C / min and hold for 0.3 h; S3, Dynamic Vacuum Sintering: The sintering furnace temperature is increased to 900℃ at a rate of 6℃ / min, while maintaining the pressure inside the sintering furnace at 10. 1 Pa, and argon gas is introduced at a rate of 30 L / min, and the temperature is maintained for 3 hours; S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 500℃ at a rate of 6℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 8℃ / min, while the pressure inside the sintering furnace is released to atmospheric pressure, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 6%, an interface cracking rate of 20%, an interface bond strength of 210 kgf, and an airtightness of 10 × 10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00038, yield 85.4%.

[0027] Example 5 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 300 °C at a rate of 3 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 610℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.81%, an interface cracking rate of 0.32%, an interface bond strength of 305 kgf, and an airtightness of 3.8×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00019, yield 92.6%.

[0028] Example 6 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 270 °C at a rate of 3 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 3℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 620℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.83%, an interface cracking rate of 0.36%, an interface bond strength of 300 kgf, and an airtightness of 3.4×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00019, yield 91.2%.

[0029] Example 7 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 300 °C at a rate of 3 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 610℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.78%, an interface cracking rate of 0.28%, an interface bond strength of 310 kgf, and an airtightness of 3.2×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00017, yield 95.6%.

[0030] Comparative Example 2 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; In this embodiment, tantalum material includes tantalum cap and tantalum wire.

[0031] S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -3 The pressure was maintained at 1 Pa for 15 minutes, then argon gas was introduced at a rate of 30 L / min to maintain the pressure inside the sintering furnace at 1 × 10⁻⁶. - ²Pa, then raise the temperature of the sintering furnace to 770℃ at a rate of 7℃ / min and hold for 0.3h; S3, Dynamic Vacuum Sintering: The sintering furnace temperature is increased to 880℃ at a rate of 6℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas is introduced at a rate of 30 L / min, and the temperature is maintained for 3 hours; S4, Thermal Insulation and Stress Relief: The sintering furnace temperature is reduced to 700℃ at a rate of 7℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas flow rate of 30L / min is introduced, and the temperature is maintained for 1h; S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 8℃ / min, while the pressure inside the sintering furnace is released to atmospheric pressure. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 8.8%, an interface cracking rate of 26.7%, an interface bond strength of 180 kgf, and an airtightness of 19 × 10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00066, yield 82.6%.

[0032] Example 8 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 300 °C at a rate of 4 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 610℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.88%, an interface cracking rate of 0.32%, an interface bond strength of 310 kgf, and an airtightness of 3.8×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00017, yield 91.6%.

[0033] Example 9 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 300 °C at a rate of 4 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 3℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 610℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.81%, an interface cracking rate of 0.37%, an interface bond strength of 310 kgf, and an airtightness of 3.2×10⁻⁶.-10 Pa m³ / s, dielectric loss tangent 0.00016, yield 90.8%.

[0034] Example 10 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 300 °C at a rate of 4 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 610℃ at a rate of 13℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.84%, an interface cracking rate of 0.36%, an interface bond strength of 310 kgf, and an airtightness of 3.4×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00018, yield 91.1%.

[0035] Comparative Example 3 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; In this embodiment, tantalum material includes tantalum cap and tantalum wire.

[0036] S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 2×10⁻⁶. -3The pressure was maintained at 1 Pa for 15 minutes, then argon gas was introduced at a rate of 30 L / min to maintain the pressure inside the sintering furnace at 1 × 10⁻⁶. - ²Pa, then raise the temperature of the sintering furnace to 790℃ at a rate of 8℃ / min and hold for 0.3h; S3, Dynamic Vacuum Sintering: The sintering furnace temperature is increased to 880℃ at a rate of 6℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas is introduced at a rate of 30 L / min, and the temperature is maintained for 3 hours; S4, Thermal Insulation and Stress Relief: The sintering furnace temperature is reduced to 600℃ at a rate of 8℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas flow rate of 30L / min is introduced, and the temperature is maintained for 1h; S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 7℃ / min, while the pressure inside the sintering furnace is released to atmospheric pressure. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 6.8%, an interface cracking rate of 28%, an interface bond strength of 180 kgf, and an airtightness of 19 × 10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00064, yield 82.3%.

[0037] Example 11 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 300 °C at a rate of 2 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 610℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.92%, an interface cracking rate of 0.41%, an interface bond strength of 300 kgf, and an airtightness of 3.6×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00017, yield 92.4%.

[0038] Example 12 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 300 °C at a rate of 3 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 610℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.88%, an interface cracking rate of 0.39%, an interface bond strength of 300 kgf, and an airtightness of 2.9×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00018, yield 95.4%.

[0039] Example 13 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 300 °C at a rate of 4 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 610℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.93%, an interface cracking rate of 0.45%, an interface bond strength of 300 kgf, and an airtightness of 3.9×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00017, yield 92.8%.

[0040] Comparative Example 4 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; In this embodiment, tantalum material includes tantalum cap and tantalum wire.

[0041] S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 2×10⁻⁶. -3 The pressure was maintained at 1 Pa for 15 minutes, then argon gas was introduced at a rate of 30 L / min to maintain the pressure inside the sintering furnace at 1 × 10⁻⁶. - ²Pa, then raise the temperature of the sintering furnace to 770℃ at a rate of 7℃ / min and hold for 0.3h; S3, Dynamic Vacuum Sintering: The sintering furnace temperature is increased to 880℃ at a rate of 6℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas is introduced at a rate of 30 L / min, and the temperature is maintained for 3 hours; S4, Thermal Insulation and Stress Relief: The sintering furnace temperature is reduced to 700℃ at a rate of 8℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas flow rate of 30L / min is introduced, and the temperature is maintained for 1h; S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 7℃ / min, while the pressure inside the sintering furnace is released to atmospheric pressure. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 6.8%, an interface cracking rate of 26.4%, an interface bond strength of 185 kgf (compared to 240 kgf in existing technology), and an airtightness of 21 × 10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00061, yield 86.1%.

[0042] Example 14 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 2 × 10² Pa, and then raise the temperature of the sintering furnace to 270 °C at a rate of 2 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 800℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 620℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.86%, an interface cracking rate of 0.38%, an interface bond strength of 300 kgf, and an airtightness of 3.6×10⁻⁶.-10 Pa m³ / s, dielectric loss tangent 0.00016, yield 98.8%.

[0043] Example 15 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 2 × 10² Pa, and then raise the temperature of the sintering furnace to 270 °C at a rate of 3 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 800℃ at a rate of 3℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 620℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 5℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.89%, an interface cracking rate of 0.36%, an interface bond strength of 320 kgf, and an airtightness of 3.9×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00016, yield 97.9%.

[0044] Example 16 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 2 × 10² Pa, and then raise the temperature of the sintering furnace to 270 °C at a rate of 4 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 800℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 620℃ at a rate of 3℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 6℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.93%, an interface cracking rate of 0.42%, an interface bond strength of 330 kgf, and an airtightness of 3.9×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00016, yield 98.6%.

[0045] Comparative Example 5 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; In this embodiment, tantalum material includes tantalum cap and tantalum wire.

[0046] S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 2×10⁻⁶. -3 The pressure was maintained at 1 Pa for 15 minutes, then argon gas was introduced at a rate of 30 L / min to maintain the pressure inside the sintering furnace at 1 × 10⁻⁶. - ²Pa, then raise the temperature of the sintering furnace to 800℃ at a rate of 6℃ / min and hold for 0.3h; S3, Dynamic Vacuum Sintering: The sintering furnace temperature is increased to 980℃ at a rate of 6℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas is introduced at a rate of 30L / min, and the temperature is maintained for 3 hours; S4, Thermal Insulation and Stress Relief: The sintering furnace temperature is reduced to 600℃ at a rate of 6℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas flow rate of 30L / min is introduced, and the temperature is maintained for 1 hour; S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 8℃ / min, while the pressure inside the sintering furnace is released to atmospheric pressure. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 9.5%, an interface cracking rate of 34.7%, an interface bond strength of 180 kgf (current technology is 240 kgf), and an airtightness of 23 × 10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00046, yield 87.7%.

[0047] Example 17 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 270 °C at a rate of 2 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 800℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 620℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 1×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.81%, an interface cracking rate of 0.36%, an interface bond strength of 340 kgf, and an airtightness of 3.1×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00016, yield 96.9%.

[0048] Example 18 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 370 °C at a rate of 3 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 750℃ at a rate of 3℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 620℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 5℃ / min, while the pressure inside the sintering furnace is gradually released from 1×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.87%, an interface cracking rate of 0.38%, an interface bond strength of 330 kgf, and an airtightness of 3.6×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00016, yield 96.6%.

[0049] Example 19 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 370 °C at a rate of 4 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 810℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 600℃ at a rate of 3℃ / min, while the pressure inside the sintering furnace is maintained at 1×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 6℃ / min, while the pressure inside the sintering furnace is gradually released from 1×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.89%, an interface cracking rate of 0.36%, an interface bond strength of 330 kgf, and an airtightness of 3.9×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00018, yield 97.2%.

[0050] Comparative Example 6 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; In this embodiment, tantalum material includes tantalum cap and tantalum wire.

[0051] S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -3 The pressure was maintained at 1 Pa for 15 minutes, then argon gas was introduced at a rate of 30 L / min to maintain the pressure inside the sintering furnace at 1 × 10⁻⁶. - ²Pa, then raise the temperature of the sintering furnace to 500℃ at a rate of 8℃ / min and hold for 0.3h; S3, Dynamic Vacuum Sintering: The sintering furnace temperature is increased to 950℃ at a rate of 8℃ / min, while maintaining the pressure inside the sintering furnace at 1×10⁻⁶. - ²Pa, and argon gas is introduced at a rate of 30 L / min, and the temperature is maintained for 3 hours; S4, Thermal Insulation and Stress Relief: The sintering furnace temperature is reduced to 700℃ at a rate of 6℃ / min, while maintaining the pressure inside the sintering furnace at 1×10⁻⁶. - ²Pa, and argon gas flow rate of 30L / min is introduced, and the temperature is maintained for 1h; S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 8℃ / min, while the pressure inside the sintering furnace is released to atmospheric pressure. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 7%, an interface cracking rate of 25%, an interface bond strength of 190 kgf (current technology is 240 kgf), and an airtightness of 13 × 10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00041, yield 85.1%.

[0052] Example 20 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 380 °C at a rate of 2 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 830℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 610℃ at a rate of 1℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.81%, an interface cracking rate of 0.31%, an interface bond strength of 330 kgf, and an airtightness of 3.4×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00017, yield 95.2%.

[0053] Example 21 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 350 °C at a rate of 3 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 750℃ at a rate of 3℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 620℃ at a rate of 2℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 5℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.86%, an interface cracking rate of 0.38%, an interface bond strength of 330 kgf, and an airtightness of 3.8×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00018, yield 97.8%.

[0054] Example 22 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 1×10⁻⁶. -2 Pa, maintain for 10 min, then introduce argon gas at 20 L / min to maintain the pressure inside the sintering furnace at 1 × 10² Pa, and then raise the temperature of the sintering furnace to 290 °C at a rate of 4 °C / min and hold for 0.3 h; S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to 8400℃ at a rate of 4℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a rate of 30L / min and held at that temperature for 2h. S4, Heat preservation and stress relief: The temperature of the sintering furnace is reduced to 600℃ at a rate of 3℃ / min, while the pressure inside the sintering furnace is maintained at 2×10²Pa, and argon gas is introduced at a flow rate of 30L / min, and the temperature is maintained for 1h. S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 6℃ / min, while the pressure inside the sintering furnace is gradually released from 2×10²Pa to atmospheric pressure. Once the temperature inside the sintering furnace reaches 120℃, argon gas supply is stopped, and cooling continues to room temperature. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 0.84%, an interface cracking rate of 0.41%, an interface bond strength of 330 kgf, and an airtightness of 3.9×10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00018, yield 98.4%.

[0055] Comparative Example 7 This embodiment includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; In this embodiment, tantalum material includes tantalum cap and tantalum wire.

[0056] S2, Preheating and Degassing: The glass embryo and pretreated tantalum material are assembled into a graphite mold, and then the graphite mold is placed in a sintering furnace. The sintering furnace is first evacuated to a vacuum of 2×10⁻⁶. -3 The pressure was maintained at 1 Pa for 15 minutes, then argon gas was introduced at a rate of 30 L / min to maintain the pressure inside the sintering furnace at 1 × 10⁻⁶. - ²Pa, then raise the temperature of the sintering furnace to 770℃ at a rate of 6℃ / min and hold for 0.3h; S3, Dynamic Vacuum Sintering: The sintering furnace temperature is increased to 880℃ at a rate of 7℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas is introduced at a rate of 30 L / min, and the temperature is maintained for 3 hours; S4, Thermal Insulation and Stress Relief: The sintering furnace temperature is reduced to 700℃ at a rate of 7℃ / min, while maintaining the pressure inside the sintering furnace at 2×10⁻⁶. - ²Pa, and argon gas flow rate of 30L / min is introduced, and the temperature is maintained for 1h; S5, Cooling: The sintering furnace temperature is reduced to 120℃ at a rate of 7℃ / min, while the pressure inside the sintering furnace is released to atmospheric pressure. The glass-tantalum material sintered using this method, after testing, has a glass porosity of 7.8%, an interface cracking rate of 25%, an interface bond strength of 185 kgf (compared to 240 kgf in existing technology), and an airtightness of 22 × 10⁻⁶. -10 Pa m³ / s, dielectric loss tangent 0.00054, yield 86.1%.

[0057] Therefore, this application has the following effects; (1) The defect rate was significantly reduced: the glass porosity decreased from ≥3% to ≤1%, and the interface cracking rate decreased from ≥15% to ≤0.5%; (2) Product performance leap: the interfacial bonding strength has increased from ≤240kgf to ≥340kgf, and the airtightness has increased from 10 -7 Pa m³ / s increased to ≤5×10 -10 Pa m³ / s, stable dielectric properties (dielectric loss tangent ≤ 0.0002). (3) Improved production stability: Product yield increased from 82% to 98%, batch performance fluctuation ≤ ±2%, adapting to the needs of mass production; (4) Strong process compatibility: No need to change equipment, only adjust the temperature and pressure parameters to adapt to different glass formulations and tantalum material specifications, resulting in low industrialization costs.

[0058] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the technical solutions of the present invention have been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or make equivalent substitutions for some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the various embodiments of the present invention.

Claims

1. A method for sintering glass and tantalum material, characterized in that, Includes the following steps: S1, Pretreatment: Glass powder is sieved, mixed with binder, dried, cold-pressed, and sintered to obtain a glass embryo; tantalum material is surface-treated and cleaned with an acidic solution to obtain pretreated tantalum material; S2, Preheating and Degassing: Assemble the glass embryo and the pretreated tantalum material into the mold, place the mold into the sintering furnace, evacuate the sintering furnace to the preset vacuum value, and hold it for the first preset time value; then maintain the first pressure value in the sintering furnace and continuously introduce protective gas, and then raise the temperature of the sintering furnace to the first preset temperature value at a rate of 2-4℃ / min, and hold it for the second preset time value. S3, Dynamic vacuum sintering: The temperature of the sintering furnace is raised to the second preset temperature value at a rate of 2-4℃ / min, while maintaining the second pressure value in the sintering furnace and continuously introducing protective gas, and holding for a third preset time value, wherein the second preset temperature value is greater than the first preset temperature value. The second pressure value is greater than or equal to the first pressure value; S4, Heat preservation and stress relief: Cool the sintering furnace temperature to the third preset temperature value at a rate of 1-3℃ / min, while maintaining the third pressure value in the sintering furnace and continuously introducing protective gas, and heat preservation for a fourth preset time value, wherein the third preset temperature value is greater than the first preset temperature value. The third pressure value is greater than or equal to the second pressure value; S5, Cooling: Cool the sintering furnace temperature to the fourth preset temperature value at a rate of 4-6℃ / min, while continuously introducing protective gas and depressurizing the pressure inside the sintering furnace to atmospheric pressure. When the temperature inside the sintering furnace drops to the fourth preset temperature value, stop introducing protective gas and allow the sintering furnace to continue cooling to room temperature.

2. The sintering method for glass and tantalum material according to claim 1, characterized in that, The first pressure value is ≥1×10²Pa.

3. The sintering method for glass and tantalum material according to claim 1, characterized in that, In the preheating and degassing step, the preset vacuum value is ≤1×10⁻⁶. -2 Pa; the first preset time value is 10-15 min; the first preset temperature value is 200-400℃; the second preset time value is 0.3-0.5 h.

4. The sintering method for glass and tantalum material according to claim 1, characterized in that, In the dynamic vacuum sintering step, the second preset temperature value is 720-850℃; the third preset time value is 2-3h.

5. The sintering method for glass and tantalum material according to claim 1, characterized in that, In the heat preservation and stress relief step, the third preset temperature value is 600-620℃; the fourth preset time value is 1-2h.

6. The sintering method for glass and tantalum material according to claim 1, characterized in that, The fourth preset temperature value is 120℃.

7. The sintering method for glass and tantalum material according to claim 1, characterized in that, The glass powder pretreatment specifically involves: sieving the glass powder through a 120-mesh sieve, adding a binder to the sieved glass powder to form granulated powder, drying the granulated powder at 100-120℃ for 2 hours to achieve a moisture content of ≤0.1%, then cold-pressing the granulated powder at 100-180MPa into a preform, and finally pre-sintering it in a 650℃ sintering furnace to obtain a glass preform.

8. The method for sintering glass and tantalum material according to claim 7, characterized in that, The granulated powder is dried at 120℃ for 2 hours to achieve a moisture content of ≤0.1%. After drying, the granulated powder is then cold-pressed at 180MPa to form an embryo.

9. The sintering method for glass and tantalum material according to claim 1, characterized in that, The tantalum material includes a tantalum wire (30) and a tantalum cap (10). The tantalum cap (10) has a receiving cavity (40). The glass embryo (20) is located in the receiving cavity (40), and the tantalum wire (30) is inserted into the glass embryo (20).

10. The glass-tantalum sintering method according to claim 9, characterized in that, The tantalum material is surface-treated with an acidic solution to remove oxides and impurities from its surface, and then pre-treated by magnetic polishing and plasma cleaning for 10-20 minutes.

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