Ceramic material co-fired high-strength high-hermetic connector and preparation method thereof

Abstract

The application belongs to the technical field of sealed connectors and specifically relates to a ceramic material co-fired high-strength high-airtightness connector and a preparation method thereof. The high-strength high-airtightness connector is co-fired by ceramic material, silver paste and a contact, and the ceramic material comprises the following components in parts by weight: 10-70 parts of alumina, 20-90 parts of CaZrBSiO glass powder, 1-5 parts of bauxite, and 1-5 parts of magnesium oxide. The obtained electric connector has the characteristics of good stability, high strength, excellent high and low temperature impact resistance, high airtightness, excellent corrosion resistance, moisture resistance and excellent thermal shock resistance, greatly improves the service life of the electric connector, effectively prevents the air leakage phenomenon caused by high and low temperature impact, and improves the reliability of the electric connector.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of sealed connectors, and particularly relates to a co-fired high-strength high-airtightness connector made of ceramic material and a preparation method thereof. BACKGROUND

[0002] Sealed interconnection technology is widely used in important fields such as infrared detection and imaging systems, T / R components, spaceflight and underwater cabin equipment. With the development of science and technology and the upgrading of weapon types, connectors with high sealing, miniaturization, high strength and non-hygroscopicity have become a development trend. Therefore, it is necessary to study the preparation technology of high-strength and moisture-proof ceramic materials and the high-density high-strength ceramic metallization / encapsulation technology to meet the development needs of future ultra-high sealing interconnection technology.

[0003] Sealed interconnection technology generally includes glue filling sealing, glass sintering sealing and ceramic sealing. Glue filling sealing has poor sealing performance and is usually used in application scenarios with low sealing performance requirements. Although the glass sintering sealing technology can meet most sealing performance requirements, it has the disadvantages of poor compression resistance and unstable glass sintering quality, and often has failure cases such as voids and cracks. The ceramic sealing has high sealing performance and high strength, but has high processing difficulty and high cost.

[0004] In the future, domestic and foreign sealed interconnection products will continue to develop towards high strength, non-hygroscopicity, miniaturization and high airtightness. Special alumina composite ceramic material has excellent properties such as high temperature resistance, wear resistance, corrosion resistance, low density, non-hygroscopicity and good insulation, and has broad application prospects in important military fields such as aerospace, aviation, weapons and ships. With the development of science and technology, the air tightness, strength and insulation of interconnection devices are required to be higher in major projects, and almost all high-end interconnection devices in service use ceramic sealing technology. The connection methods of ceramic and metal mainly include mechanical connection, adhesion and welding, among which the welding method has the characteristics of high bonding strength and high temperature resistance, can significantly improve the air tightness of the interconnection device, and has low requirements for the geometric shape and size of the connector, and can realize special-shaped processing. In the preparation of traditional ceramic connectors, domestic research institutions mainly use traditional 95 or 99 alumina ceramic and add low-temperature sintering agent to metalize the ceramic, and finally weld the contact piece to prepare an electric connector with high air tightness. However, the method has complex production process, and for high-density multi-core electric connectors, the overflow in the welding process is uncontrollable, the welding consistency is poor, and other problems are prominent, so it is difficult to realize mass production. SUMMARY

[0005] The application solves the problems of low strength of glass insulator, easy cracking, and difficult to reduce the leakage rate to less than 10 -12 Pa·m 3 / s, and the problem of poor thermal shock resistance, a ceramic material co-fired high-strength high-airtight connector and a preparation method thereof are provided.

[0006] The technical scheme is specifically implemented as follows:

[0007] The ceramic material co-fired high-strength high-airtight connector is sintered from a ceramic material, silver paste and a contact, and the ceramic material comprises the following components in parts by weight: 10-70 parts of alumina, 20-90 parts of CaZrBSiO glass powder, 1-5 parts of bismuth oxide and 1-5 parts of magnesium oxide.

[0008] The ceramic material and the Kovar alloy have matched thermal expansion coefficients, and the difference between the thermal expansion coefficients of the two is not more than 10%.

[0009] The technical scheme is specifically implemented as follows:

[0010] (1) Preparing ceramic raw materials; taking 10-70 parts of alumina, 20-90 parts of CaZrBSiO glass powder, 1-5 parts of bismuth oxide and 1-5 parts of magnesium oxide, and mixing the four materials to form a composite ceramic powder;

[0011] (2) Ball-milling and mixing the composite ceramic powder with deionized water for 6-24 hours, aging, and then spray drying to obtain the ceramic material;

[0012] (3) Forming and degassing the obtained ceramic material, then coating silver paste in the ceramic hole, inserting the contact into the hole coated with silver paste, positioning with a mold, and then sintering in a vacuum furnace, stopping sintering after the ceramic is formed, and naturally cooling to obtain the high-strength high-airtight connector.

[0013] The amount of deionized water is 4-8% of the total mass of the composite ceramic powder.

[0014] In step (2), the aging time is 12-48 hours.

[0015] In step (3), the sintering temperature is 820-950°C, and the time is 0.5-3 hours.

[0016] In step (3), the amount of silver paste is 3-6% of the total mass of the composite ceramic powder.

[0017] The thermal expansion coefficient of the CaZrBSiO glass powder is between 5 and 7, and the bending strength is greater than 200 MPa; the thermal expansion coefficient of the alumina ceramic is between 6.5 and 7.5, and the bending strength is greater than 400 MPa. Mixing bismuth oxide, magnesium oxide and the two materials can obtain a composite ceramic with high strength, low-temperature co-firing with silver paste, high bonding force and no diffusion.

[0018] The key of the present application is as follows:

[0019] 1、The present application takes into account that the thermal expansion coefficient of CaZrBSiO glass is low and the glass transition temperature is low, and the thermal expansion coefficient of aluminum oxide is high and the sintering temperature is high, so aluminum oxide, magnesium oxide and erbium oxide are added to the CaZrBSiO glass formula to obtain a composite material with adjustable temperature and thermal expansion coefficient, so as to match the thermal expansion coefficient of metal materials and prevent cracking and gas leakage caused by stress at high temperature.

[0020] 2、The addition of aluminum oxide, magnesium oxide and erbium oxide in the CaZrBSiO glass formula can ensure that the ceramic material does not chemically react with silver paste during co-sintering at high temperature, and does not diffuse, while improving the bonding force between silver paste and the interface of the composite ceramic, thereby greatly improving its insulation performance and high and low temperature impact resistance.

[0021] 3、The addition of aluminum oxide, magnesium oxide and erbium oxide in the CaZrBSiO glass formula can improve the strength of the ceramic material, so that when subjected to high and low temperature impact, it can resist the internal stress generated from the inside of the ceramic.

[0022] Advantages:

[0023] The present application provides a method for low-temperature co-sintering of a low-leakage-rate electrical connector. The obtained electrical connector has good stability, high strength, excellent high and low temperature impact resistance, high airtightness, excellent corrosion resistance, moisture resistance, and excellent thermal shock resistance. The service life of the electrical connector is greatly improved, the gas leakage phenomenon caused by high and low temperature impact is effectively prevented, the reliability of the electrical connector is improved, and it is especially suitable for connection fields with large high and low temperature differences.

[0024] The present application has the advantages of simple operation, easy control of process parameters, low cost, high production efficiency and good production consistency. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 is the co-sintering micro-morphology of the material prepared in Example 2.

[0026] Figure 2 is the co-sintering micro-morphology of the material prepared in Example 4.

[0027] Figure 3 is the design drawing of the co-sintering connector of Example 5. DETAILED DESCRIPTION

[0028] The specific embodiments of the present application will be further described in detail below, but the present application is not limited to these embodiments, and any improvement or replacement within the basic spirit of the present application still belongs to the scope of protection claimed by the present application.

[0029] Example 1

[0030] A method for preparing a ceramic material co-fired high-strength high-hermetic connector, comprising the following steps:

[0031] Step 1: Take 20 parts of alumina, 78 parts of CaZrBSiO glass powder, 1 part of bismuth oxide, and 1 part of magnesium oxide, mix the four materials to form a composite ceramic powder;

[0032] Step 2: Mix and ball mill the composite ceramic powder of step 1 with deionized water, the amount of deionized water is 6% of the total mass of the raw materials, after uniform mixing and stirring, stand for 24 hours, then spray drying to obtain a ceramic material;

[0033] Step 3: Form and degas the ceramic material obtained in step 2, pre-burn at 600°C for 3 hours, then apply silver paste inside the ceramic hole, then insert the contact into the coated hole, and position it with the mold;

[0034] Step 4: Put the assembled and positioned ceramic and contact composition obtained in step 3 into a vacuum furnace for heating and co-firing, sinter at 860°C for 1 hour, stop heating after the ceramic is formed, and naturally cool to obtain a high-strength high-hermetic connector.

[0035] Example 2:

[0036] Step 1: Take 25 parts of alumina, 73 parts of CaZrBSiO glass powder, 1 part of bismuth oxide, and 1 part of magnesium oxide, mix the four materials to form a composite ceramic powder;

[0037] Step 2: Mix and ball mill the composite ceramic powder of step 1 with deionized water, the amount of deionized water is 6% of the total mass of the raw materials, after uniform mixing and stirring, stand for 24 hours, then spray drying to obtain a ceramic material;

[0038] Step 3: Form and degas the ceramic material obtained in step 2, pre-burn at 600°C for 3 hours, then apply silver paste inside the ceramic hole, then insert the contact into the coated hole, and position it with the mold;

[0039] Step 4: Put the assembled and positioned ceramic and contact composition obtained in step 3 into a vacuum furnace for heating and co-firing, sinter at 860°C for 1 hour, stop heating after the ceramic is formed, and naturally cool to obtain a high-strength high-hermetic connector.

[0040] Example 3:

[0041] Step 1: Take 30 parts of alumina, 68 parts of CaZrBSiO glass powder, 1 part of bismuth oxide, and 1 part of magnesium oxide, mix the four materials to form a composite ceramic powder;

[0042] Step 2: The composite ceramic powder of step 1 is mixed with deionized water, the amount of which is 6% of the total mass of the raw materials. After uniform mixing and stirring, the mixture is aged for 24 hours, and then spray dried to obtain a ceramic material.

[0043] Step 3: The ceramic material of step 2 is shaped and degassed, and then pre-fired at 600°C for 3 hours. Silver paste is then applied to the inside of the ceramic hole, and then the contact piece is inserted into the hole and positioned with a mold.

[0044] Step 4: The assembled and positioned ceramic and contact piece composition of step 3 is placed in a vacuum furnace for heating and co-firing, and fired at 900°C for 1 hour. After the ceramic is formed, heating is stopped, and the high-strength and high-airtightness connector is obtained after natural cooling.

[0045] Example 4:

[0046] Step 1: Take 25 parts of alumina, 70 parts of CaZrBSiO glass powder, 2.5 parts of bismuth oxide, and 2.5 parts of magnesium oxide, and mix the four materials to form a composite ceramic powder.

[0047] Step 2: The composite ceramic powder of step 1 is mixed with deionized water, the amount of which is 6% of the total mass of the raw materials. After uniform mixing and stirring, the mixture is aged for 24 hours, and then spray dried to obtain a ceramic material.

[0048] Step 3: The ceramic material of step 2 is shaped and degassed, and then pre-fired at 600°C for 3 hours. Silver paste is then applied to the inside of the ceramic hole, and then the contact piece is inserted into the hole and positioned with a mold.

[0049] Step 4: The assembled and positioned ceramic and contact piece composition of step 3 is placed in a vacuum furnace for heating and co-firing, and fired at 860°C for 1 hour. After the ceramic is formed, heating is stopped, and the high-strength and high-airtightness connector is obtained after natural cooling.

[0050] Example 5:

[0051] Step 1: Take 70 parts of alumina, 20 parts of CaZrBSiO glass powder, 5 parts of bismuth oxide, and 5 parts of magnesium oxide, and mix the four materials to form a composite ceramic powder.

[0052] Step 2: The composite ceramic powder of step 1 is mixed with deionized water, the amount of which is 6% of the total mass of the raw materials. After uniform mixing and stirring, the mixture is aged for 24 hours, and then spray dried to obtain a ceramic material.

[0053] Step 3: the ceramic material obtained in step 2 is shaped, degassed, pre-fired at 600℃ for 3 hours, then silver paste is coated inside the ceramic hole, then the contact is inserted into the coated hole and positioned by a mold;

[0054] Step 4: the assembled and positioned ceramic and contact composition obtained in step 3 is put into a vacuum furnace for heating and co-firing, fired at 950℃ for 1.5 hours, then heating is stopped after the ceramic is formed, and the high-strength and high-airtight connector is obtained after natural cooling.

[0055] The following table is the corrosion resistance test results of each embodiment:

[0056]

[0057] As can be seen from the data in the table, the leakage rate of the connector prepared by using the composition provided by the present application is significantly better than the leakage rate of the glass sintering in the industry. The ceramic co-firing connector of the present application has good high and low temperature impact resistance and insulation and moisture resistance during use, and there is no case of deterioration of the leakage rate after multiple high and low temperature impact experiments, significantly improving the quality and stability of the product, and the production raw materials are low, the preparation process is simple, compatible with traditional processes, and conducive to the improvement of enterprise production efficiency.

[0058] The embodiments of the present application are described in detail above in combination with the drawings, but the present application is not limited to the above specific embodiments, and the above specific embodiments are only illustrative and not limiting. Those skilled in the art can make many modifications without departing from the purpose of the present application and the scope of the claims, and these all belong to the protection of the present application.

Claims

1. A ceramic material co-fired high strength high hermetic connector characterized by, The high-strength and high-airtightness connector is sintered from a ceramic material, silver paste and a contact, wherein the ceramic material comprises the following components by weight: 10-70 parts of alumina, 20-90 parts of CaZrBSiO glass powder, 1-5 parts of bauxite and 1-5 parts of magnesia; The preparation method of the high-strength and high-airtightness connector comprises the following steps: (1) preparing ceramic raw materials; taking 10-70 parts of alumina, 20-90 parts of CaZrBSiO glass powder, 1-5 parts of bauxite and 1-5 parts of magnesia, and mixing the four materials to form composite ceramic powder; (2) ball-milling and mixing the composite ceramic powder with deionized water for 6-24 hours, aging, and then spray drying to obtain the ceramic material; (3) forming and degassing the obtained ceramic material, then coating silver paste in the ceramic hole, inserting the contact into the hole coated with silver paste, positioning with a mold, and then sintering in a vacuum furnace, stopping sintering after the ceramic is formed, and naturally cooling to obtain the high-strength and high-airtightness connector; In step (3), the sintering temperature is 820-950℃, and the time is 0.5-3 hours.

2. A co-fired ceramic material high strength high hermetic connector as defined in claim 1 wherein, The amount of deionized water is 4-8% of the total mass of the composite ceramic powder.

3. The co-fired ceramic material high strength high hermetic connector of claim 1, wherein, In step (2), the aging time is 12-48 hours.

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