Preparation method of high-reliability ceramic component for ignition device

Abstract

The invention discloses a preparation method of a high-reliability ceramic component for an ignition device, the ceramic component comprises a shell, ceramic, a contact pin, a solder, first sealing glass and second sealing glass, and the preparation process relates to two processes, namely a brazing process and a glass sealing process. According to the brazing process, ceramic and a contact pin are bonded through welding flux, and a ceramic electrode plug is obtained; according to the glass sealing process, the ceramic electrode plug and the shell are sealed through the first sealing glass and the second sealing glass, the ceramic assembly is obtained, a chip containing area and a medicine containing area are designed in the ceramic assembly, and the ceramic assembly has the advantages of being high in safety, high in structural strength, high in integration and the like. By adopting the sealing glass with different melting points, the problems of cavities and gaps in the glass filling area due to the fact that gas is difficult to discharge due to the structure problem are solved, and the insulation resistance performance and the pressure resistance performance of the ceramic assembly are improved.

Description

Technical Field

[0001] The present invention relates to the technical field of ceramic components, and particularly to a preparation method of a highly reliable ceramic component for an ignition device. Background Art

[0002] Highly reliable ceramic components are connected by soldering and glass sealing technologies to obtain a metal-ceramic composite component. This technology can combine the advantages of both, giving full play to the excellent properties of ceramic materials and expanding their application fields. Among them, electrode plugs are widely used in the actual production and applications in industries such as aviation, aerospace, shipbuilding, nuclear power, and civilian products due to their excellent comprehensive properties such as airtightness, sealing performance, and mechanical strength. In recent years, the research and large-scale production of new ceramic materials have also promoted the rapid development and wide application of metal-ceramic soldering technology. Metal-ceramic sealed components have excellent comprehensive characteristics such as high reliability, high pressure resistance, oxidation resistance, corrosion resistance, high insulation, and high airtightness. Therefore, studying metal-ceramic sealing materials, their sealing technologies, and sealing processes has a positive effect and practical significance on improving the performance of various functional devices and expanding their application space.

[0003] For example, in the invention application with the application number CN202011582464.X, a pressure sensor base and its manufacturing method. The pressure sensor base includes a housing, a sealing glass blank, and leads. The housing is axially provided with a glass sealing hole. The sealing glass blank is placed in the glass sealing hole. The sealing glass blank is provided with several through holes. The leads pass through the through holes from bottom to top. The glass sealing hole is in a stepped shape. A first step is provided above the sealing glass hole, and a second step is provided above the first step. In this solution, the addition of the integral glass increases the amount of glass used, thus greatly improving the electrical performance of the product. However, it cannot solve the problem of the decrease in the insulation resistance performance and voltage resistance performance of the ceramic component caused by the acid cleaning solution entering the glass filling gap. Summary of the Invention

[0004] Aiming at the deficiencies of the prior art, the purpose of the present invention is to provide a preparation method of a highly reliable ceramic component for an ignition device, which solves the problem of the internal cavity in the glass filling area caused by the difficulty of gas discharge due to the structural problem in the prior art, and improves the insulation resistance performance and voltage resistance performance of the ceramic component.

[0005] The technical solution adopted by the present invention to solve the technical problem is: a preparation method of a highly reliable ceramic component for an ignition device. The ceramic component includes a housing, a ceramic, a pin, solder, a first sealing glass, and a second sealing glass. A jack is provided inside the ceramic. One end of the pin penetrates into the jack and is fixed by solder to obtain a ceramic electrode plug. The ceramic electrode plug is sealed in the housing through the first sealing glass and the second sealing glass to obtain a ceramic component.

[0006] The preparation method of the ceramic component comprises the following steps:

[0007] 1) Brazing: Position the ceramic and the pin through a mold, place solder in the socket of the ceramic, put it into a chain furnace for sintering, the sealing temperature is above 1000 °C, the heat preservation time is above 10 min, and the cooling rate is adjusted to 6 - 8 °C / min in the temperature range of 680 - 700 °C;

[0008] 2) Sealing: Thread the first sealing glass and the second sealing glass into the pins of the ceramic electrode plug in sequence, and place them into the mating hole positions of the housing, position them through the corresponding mold, sinter in a chain furnace, the sealing temperature is 930 - 980 °C, the heat preservation time is 15 - 20 min, and the cooling rate is adjusted to 3 - 5 °C / min in the temperature range of 530 - 680 °C; Slowly demold the sintered ceramic component;

[0009] 3) Pickling: Fix the ceramic component through a tooling fixture, completely immerse the tooling fixture into the pickling solution, perform ultrasonic treatment, take out the tooling fixture, rinse it in flowing water, then perform ultrasonic treatment in alcohol, and dry the tooling fixture after taking it out.

[0010] Further, the first sealing glass is a silicate-based glass, the sealing temperature is between 930 - 980 °C, and the cooling rate is adjusted to 3 - 5 °C / min in the temperature range of 650 - 680 °C. The second sealing glass is a lead silicate glass, the sealing temperature is 800 - 850 °C, and the cooling rate is adjusted to 3 - 5 °C / min in the temperature range of 530 - 560 °C; The melting point of the first sealing glass is higher than that of the second sealing glass.

[0011] Further, the material of the housing is stainless steel, and the ceramic is alumina or zirconia ceramic.

[0012] Further, the filling amount of the glass inside the ceramic component must reach more than 98% of the theoretical value; The insulation resistance of the ceramic component reaches more than 10 GΩ, the voltage withstand capacity is greater than 40 MPa, it can withstand the instantaneous pressure of 80 MPa for gunpowder ignition, and the component structure can withstand a torque of 1000 N without deformation.

[0013] Further, the composition of the pickling solution is by volume ratio, hydrogen peroxide: hydrochloric acid: hydrofluoric acid: water = 1:1:0.5:10; Among them, the mass fraction of the hydrogen peroxide is 30 - 35%, the mass fraction of the hydrochloric acid is 40 - 45%, and the mass fraction of the hydrofluoric acid is 10 - 15%.

[0014] Further, a chip placement area and a charge loading area are provided above the ceramic component.

[0015] After high-temperature sintering of the ceramic component, an oxide film will form on the surface of the housing, affecting the appearance and welding performance. The current common treatment method is pickling. However, due to the gap between the ceramic and the housing, the pickling solution is likely to enter this gap, resulting in conductive ions adhering to the glass, which can easily cause poor insulation resistance after moisture absorption. An effective solution is to fill the gap between the ceramic and the housing with glass to prevent the pickling solution from contaminating the glass. The present invention applies a combination of two glasses with different melting points. The first sealing glass is a high-melting-point glass, and the second sealing glass is a low-melting-point glass. After heating, when the temperature is higher than the softening temperature of the second sealing glass, the second sealing glass will continuously be in a molten state. As the temperature continues to rise to the softening temperature of the first sealing glass, the first sealing glass begins to be in a molten state. During the cooling process, the first sealing glass preferentially starts to solidify after being below the strain point temperature, while the second sealing glass is still above the softening temperature. This is conducive to the discharge of the gas at the lower end until the second sealing glass is also below the strain point temperature, and both glasses are in a stable state; the internal gas existing during the vitrification and degumming processes of the glass and the gas in the clearance between the glass and the mold are discharged to the greatest extent, thereby ensuring that there is no gap between the ceramic and the housing and avoiding the pickling solution from contaminating the glass.

[0016] The beneficial effects of the present invention are as follows: Compared with the prior art, the preparation method of a highly reliable ceramic component for an ignition device provided by the present invention solves the problems of internal cavities and gaps in the glass filling area caused by difficult gas discharge due to structural problems by adopting sealing glasses with different melting points and combining the brazing process and the glass sealing process, and improves the insulation resistance performance and voltage resistance performance of the ceramic component. Brief Description of the Drawings

[0017] Figure 1 It is a schematic structural diagram of the ceramic component in the present invention.

[0018] Figure 2 It is a schematic structural diagram of the ceramic electrode plug in the present invention.

[0019] Wherein, 1 - ceramic; 2 - housing; 3 - pin; 4 - second sealing glass; 5 - first sealing glass; 6 - solder; 7 - charge area; 8 - chip placement area. Detailed Embodiments

[0020] The present invention will be further described below through specific embodiments. However, these examples are only used to illustrate the present invention and not to limit the scope of the present invention.

[0021] Such as Figure 1 and 2As shown in the figure, a preparation method of a highly reliable ceramic component for an ignition device, the ceramic component includes a housing 2, a ceramic 1, a pin 3, a solder 6, a first sealing glass 5 and a second sealing glass 4; a jack is provided in the ceramic 1, and one end of the pin 3 penetrates into the jack and is fixed by the solder 6 to obtain a ceramic electrode plug; the ceramic electrode plug is sealed in the housing 2 through the first sealing glass 5 and the second sealing glass 4 to obtain a ceramic component; a chip placement area 8 and a charge area 7 are provided above the ceramic component. The material of the housing 2 is stainless steel, and the ceramic 1 is alumina or zirconia ceramic.

[0022] The preparation method of the ceramic component includes the following steps:

[0023] 1) Brazing: Position the ceramic 1 and the pin 3 through a mold, place the solder 6 in the jack of the ceramic 1, put it into a chain furnace for sintering, the sealing temperature is above 1000 °C, the holding time is above 10 min, and the cooling rate is adjusted to 6 - 8 °C / min in the temperature range of 680 - 700 °C;

[0024] 2) Sealing: Thread the first sealing glass 5 and the second sealing glass 4 into the pin 3 of the ceramic electrode plug in sequence, and place it into the mating hole position of the housing 2, position it through the corresponding mold, sinter it in a chain furnace, the sealing temperature is 930 - 980 °C, the holding time is 15 - 20 min, and the cooling rate is adjusted to 3 - 5 °C / min in the temperature range of 530 - 680 °C; Slowly demold the sintered ceramic component;

[0025] 3) Pickling: Fix the ceramic component through a tooling, completely immerse the tooling in the pickling solution, perform ultrasonic treatment, take out the tooling, rinse it in flowing water, then perform ultrasonic treatment in alcohol, and dry the tooling after taking it out. The composition of the pickling solution is by volume ratio, hydrogen peroxide: hydrochloric acid: hydrofluoric acid: water = 1:1:0.5:10; wherein, the mass fraction of the hydrogen peroxide is 30 - 35%, the mass fraction of the hydrochloric acid is 40 - 45%, and the mass fraction of the hydrofluoric acid is 10 - 15%.

[0026] The first sealing glass 5 is a silicate-based glass, the sealing temperature is between 930 - 980 °C, and the cooling rate is adjusted to 3 - 5 °C / min in the temperature range of 650 - 680 °C, the second sealing glass 4 is a lead silicate glass, the sealing temperature is 800 - 850 °C, and the cooling rate is adjusted to 3 - 5 °C / min in the temperature range of 530 - 560 °C; The melting point of the first sealing glass 5 is higher than that of the second sealing glass 4.

[0027] The glass filling amount inside the ceramic component must reach more than 98% of the theoretical value; the insulation resistance of the ceramic component is more than 10GΩ, the pressure resistance is greater than 40MPa, and it can withstand the instantaneous pressure of 80MPa required by gunpowder ignition. The component structure can withstand a torque of 1000N without deformation.

[0028] Example 1

[0029] 1) Ceramic electrode plug brazing:

[0030] First, the ceramic and the pin are positioned by a mold, and solder is placed in the ceramic socket. The ceramic electrode plug is sintered in a chain furnace with a sealing temperature of 1010°C and a holding time of 10 minutes. The cooling rate is adjusted to 6°C / min in the temperature range of 680-700°C to obtain a ceramic electrode plug.

[0031] 2) Ceramic electrode plug and stainless steel shell glass seal:

[0032] The first and second sealing glasses were sequentially inserted into the pins of the ceramic electrode plug and then into the matching holes of the stainless steel housing. Positioned using the corresponding mold, the components were sintered in a chain furnace at a sealing temperature of 930°C for 15 minutes, with a cooling rate of 3°C / min within the 650-680°C range. The sintered ceramic assembly was slowly demolded.

[0033] 3) Pickling process:

[0034] Prepare the pickling solution: hydrogen peroxide (30% by mass): hydrochloric acid (40% by mass): hydrofluoric acid (10%): water in a volume ratio of 1:1:0.5:10. Measure the appropriate volume of distilled water and slowly add the corresponding volumes of hydrogen peroxide, hydrochloric acid, and hydrofluoric acid to the distilled water, stirring for 20-30 seconds.

[0035] Pickling: Secure the ceramic components with fixtures, placing 50 pieces per fixture to ensure the shells do not contact each other, causing bumps or scratches. Completely immerse the fixture in the pickling solution and ultrasonicate for 20 seconds. Remove the fixture and rinse it in running water for 2 minutes, then ultrasonicate it in alcohol for 3 minutes. Remove the fixture and place it in an oven to dry.

[0036] Example 2

[0037] 1) Ceramic electrode plug brazing:

[0038] First, the ceramic and the pin are positioned by a mold, and solder is placed in the ceramic socket. The ceramic electrode plug is sintered in a chain furnace with a sealing temperature of 1050°C and a holding time of 15 minutes. The cooling rate is adjusted to 7°C / min in the temperature range of 680-700°C to obtain a ceramic electrode plug.

[0039] 2) Ceramic electrode plug and stainless steel shell glass seal:

[0040] The first and second sealing glasses were sequentially inserted into the pins of the ceramic electrode plug and then into the matching holes of the stainless steel housing. Positioned using the corresponding mold, the components were sintered in a chain furnace at a sealing temperature of 950°C for 18 minutes, with a cooling rate of 4°C / min within the 650-680°C range. The sintered ceramic assembly was slowly demolded.

[0041] 3) Pickling process:

[0042] Prepare the pickling solution: hydrogen peroxide (35% by mass): hydrochloric acid (45% by mass): hydrofluoric acid (15% by mass): distilled water in a volume ratio of 1:1:0.5:10. Measure the appropriate volume of distilled water and slowly add the corresponding volumes of hydrogen peroxide, hydrochloric acid, and hydrofluoric acid to the distilled water, stirring for 30 seconds.

[0043] Pickling: Secure the ceramic components with fixtures, placing 50 pieces per fixture to ensure the shells do not contact each other, causing bumps or scratches. Completely immerse the fixture in the pickling solution and ultrasonicate for 45 seconds. Remove the fixture and rinse it in running water for 3 minutes, then ultrasonicate it in alcohol for 4 minutes. Remove the fixture and place it in an oven to dry.

[0044] Example 3

[0045] 1) Ceramic electrode plug brazing:

[0046] First, the ceramic and the pin are positioned by a mold, and solder is placed in the ceramic socket. The ceramic electrode plug is sintered in a chain furnace with a sealing temperature of 1100°C and a holding time of 20 minutes. The cooling rate is adjusted to 8°C / min in the temperature range of 680-700°C to obtain a ceramic electrode plug.

[0047] 2) Ceramic electrode plug and stainless steel shell glass seal:

[0048] The first and second sealing glasses are sequentially inserted into the pins of the ceramic electrode plug and then into the matching holes of the stainless steel housing. Positioned using the corresponding mold, the components are sintered in a chain furnace at a sealing temperature of 980°C for 20 minutes, with a cooling rate of 5°C / min within the 650-680°C range. The sintered ceramic assembly is then slowly demolded.

[0049] 3) Pickling process:

[0050] Prepare the pickling solution: hydrogen peroxide (35% by mass): hydrochloric acid (45% by mass): hydrofluoric acid (15%): water in a volume ratio of 1:1:0.5:10. Measure the appropriate volume of distilled water and slowly add the corresponding volumes of hydrogen peroxide, hydrochloric acid, and hydrofluoric acid to the distilled water, stirring for 30 seconds.

[0051] Pickling: Secure the ceramic components with fixtures, placing 50 pieces per fixture to ensure the shells do not contact each other and cause bumps or scratches. Completely immerse the fixture in the pickling solution and ultrasonicate for 50 seconds. Remove the fixture and rinse it in running water for 5 minutes, then ultrasonicate it in alcohol for 5 minutes. Remove the fixture and place it in an oven to dry.

[0052] Comparative Example

[0053] 1) Ceramic electrode plug brazing:

[0054] First, the ceramic and the pin are positioned by a mold, and solder is placed in the ceramic socket. The ceramic electrode plug is sintered in a chain furnace with a sealing temperature of 1010°C and a holding time of 10 minutes. The cooling rate is adjusted to 6°C / min in the temperature range of 680-700°C to obtain a ceramic electrode plug.

[0055] 2) Ceramic electrode plug and stainless steel shell glass seal:

[0056] The first and second sealing glasses (made of the same material) were sequentially inserted into the pins of the ceramic electrode plug and then into the matching holes of the stainless steel housing. Positioned using the corresponding molds, the components were sintered in a chain furnace at a sealing temperature of 930°C for 15 minutes, with a cooling rate of 3°C / min within the 650-680°C range. The sintered ceramic assembly was slowly demolded.

[0057] 3) Pickling process:

[0058] Prepare the pickling solution: hydrogen peroxide (30% by mass): hydrochloric acid (40% by mass): hydrofluoric acid (10%): water in a volume ratio of 1:1:0.5:10. Measure the appropriate volume of distilled water and slowly add the corresponding volumes of hydrogen peroxide, hydrochloric acid, and hydrofluoric acid to the distilled water, stirring for 20-30 seconds.

[0059] Pickling: Secure the ceramic components with fixtures, placing 50 pieces per fixture to ensure the shells do not contact each other, causing bumps or scratches. Completely immerse the fixture in the pickling solution and ultrasonicate for 20 seconds. Remove the fixture and rinse it in running water for 2 minutes, then ultrasonicate it in alcohol for 3 minutes. Remove the fixture and place it in an oven to dry.

[0060] The ceramic components obtained in the above Examples 1 to 3 and Comparative Examples were subjected to performance tests. The insulation resistance and withstand voltage strength were tested under normal temperature and pressure respectively. The test results are shown in the following table:

[0061] Item Insulation Resistance (GΩ) Withstand Voltage Strength (KPa) Example 1 10.47 50 Example 2 10.25 48 Example 3 10.48 49 Comparative Example 0.5 10

[0062] The above embodiments are only used to illustrate the present invention and are not intended to limit the present invention. Those of ordinary skill in the relevant technical field can also make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention. The patent protection scope of the present invention shall be defined by the claims.

Claims

1. A preparation method of a highly reliable ceramic component for an ignition device, characterized in that: The ceramic component includes a housing, ceramics, pins, solder, a first sealing glass, and a second sealing glass; a jack is provided in the ceramics, and one end of the pin penetrates into the jack and is fixed by solder to obtain a ceramic electrode plug; the ceramic electrode plug is sealed in the housing through the first sealing glass and the second sealing glass to obtain a ceramic component; The preparation method of the ceramic component includes the following steps: 1) Brazing: Position the ceramics and the pins through a mold, place solder in the jacks of the ceramics, put them into a chain furnace for sintering, the sealing temperature is above 1000 °C, the heat preservation time is above 10 min, and the cooling rate is adjusted to 6 - 8 °C / min in the temperature range of 680 - 700 °C; 2) Sealing: Thread the first sealing glass and the second sealing glass into the pins of the ceramic electrode plug in sequence, and place them in the mating hole positions of the housing, position them through the corresponding mold, sinter them in a chain furnace, the sealing temperature is 930 - 980 °C, the heat preservation time is 15 - 20 min, and the cooling rate is adjusted to 3 - 5 °C / min in the temperature range of 530 - 680 °C; Slowly demold the sintered ceramic component; 3) Pickling: Fix the ceramic component through a tooling, completely immerse the tooling in the pickling solution, perform ultrasonic treatment, take out the tooling, rinse it in flowing water, then perform ultrasonic treatment in alcohol, and dry the tooling after taking it out.

2. The preparation method of a highly reliable ceramic component for an ignition device according to claim 1, characterized in that: The first sealing glass is a silicate - based glass, the sealing temperature is between 930 - 980 °C, and the cooling rate is adjusted to 3 - 5 °C / min in the temperature range of 650 - 680 °C. The second sealing glass is a lead silicate glass, the sealing temperature is 800 - 850 °C, and the cooling rate is adjusted to 3 - 5 °C / min in the temperature range of 530 - 560 °C; The melting point of the first sealing glass is higher than that of the second sealing glass.

3. The preparation method of a highly reliable ceramic component for an ignition device according to claim 1, wherein: The material of the housing is stainless steel, and the ceramics are alumina or zirconia ceramics.

4. The preparation method of a highly reliable ceramic component for an ignition device according to claim 1, characterized in that: The filling amount of the internal glass of the ceramic component must reach more than 98% of the theoretical value; the insulation resistance of the ceramic component reaches more than 10 GΩ, the withstand voltage capacity is greater than 40 MPa, it can withstand the instantaneous pressure of 80 MPa during gunpowder ignition, and the component structure can withstand a torque of 1000 N without deformation.

5. The preparation method of a highly reliable ceramic component for an ignition device according to claim 1, characterized in that: The composition of the pickling solution is by volume ratio, hydrogen peroxide: hydrochloric acid: hydrofluoric acid: water = 1:1:0.5:10; among them, the mass fraction of hydrogen peroxide is 30 - 35%, the mass fraction of hydrochloric acid is 40 - 45%, and the mass fraction of hydrofluoric acid is 10 - 15%.

6. The preparation method of a highly reliable ceramic component for an ignition device according to claim 1, characterized in that: A chip placement area and a charge loading area are provided above the ceramic component.

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