CN103864467A - Ceramic surface metalizing method - Google Patents

Abstract

The invention discloses a ceramic surface metallization method, which is characterized in that the steps are as follows: step 1, designing and manufacturing a titanium alloy crucible, step 2, placing inactive brazing material in the titanium alloy crucible, and protecting it in vacuum or inert atmosphere , heated to 700°C~1000°C at a heating rate of 5~20°C/min to obtain molten inactive solder. At this time, titanium in the titanium alloy diffuses into the inactive solder to obtain molten titanium containing active element. Active solder, step 3, put the end face of the ceramic substrate to be surface metallized into a titanium alloy crucible with molten solder for 5-30 minutes, step 4, take out the ceramic substrate, flatten and cool it on the end face of the ceramic substrate Uniform metallization layer, the invention not only simplifies the metallization process, reduces the production cost, but also the molten solder can be reused, which improves the utilization rate of the metallization alloy, and the liquid metallization alloy has better properties than the powder The fluidity is good for its spreading, and the thickness of the film layer is more uniform, the operability is good, and batch production can be realized.

Description

A kind of ceramic surface metallization method

technical field

The invention relates to a new material, in particular to a ceramic surface metallization method.

Background technique

Ceramics have many excellent properties such as high temperature resistance, high strength, high hardness, high wear resistance, and high corrosion resistance. However, ceramics have poor toughness at room temperature and it is difficult to prepare parts with complex shapes. Only by combining the strength and toughness of metal with the wear resistance, corrosion resistance and high temperature resistance of ceramics can it become an ideal structural material. Generally, it is necessary to metallize the surface of the ceramic to connect with the metal.

At present, the main method for pre-metallizing the surface of ceramics is to mix molybdenum powder and manganese oxide powder to prepare a slurry, coat it on the surface of the ceramic, and then sinter at 1500°C to form a metal molybdenum layer on the surface of the ceramic. This method belongs to high-temperature connection, which will inevitably bring the following problems: (1) strict equipment requirements; (2) large-scale and complex-structured joints are prone to large internal stress; (3) the connection temperature exceeds the complex Mo-Mn method, Electroless plating and vapor deposition, etc. Among them, the allowable temperature of the strengthening phase or toughening phase in Mo-Mn alloy ceramics will seriously reduce its strengthening or toughening effect; the second is the electroless plating method, and its process flow is: degreasing → running water washing → neutralization → running water washing → Coarsening → washing with running water → sensitization → washing with distilled water → activation → washing with distilled water → reduction → electroless plating. The steps of this method are cumbersome, and the discharge of the chemical plating solution will pollute the environment. The third is the vapor deposition method, which is divided into chemical vapor deposition and physical vapor deposition. Chemical vapor deposition (CVD) is based on the space gas phase chemical reaction. The process technology of depositing solid-state thin films, physical vapor deposition (PVD) is a technology that uses heating or high-energy beam bombardment in a vacuum chamber to evaporate the material to be plated or the target into a gaseous state and deposit it on the surface of the workpiece to form a coating. This method requires high equipment and high manufacturing cost.

Contents of the invention

The object of the present invention is to overcome the deficiencies of the prior art and provide a method for metallizing ceramic surfaces with simple process and uniform metallized film layer.

The present invention reaches through following measures:

A ceramic surface metallization method is characterized in that the steps are as follows:

Step 1. Design and manufacture a titanium alloy crucible,

Step 2: Put the inactive solder in a titanium alloy crucible, and heat it to 700°C~1000°C at a heating rate of 5~20°C/min under vacuum or inert atmosphere protection conditions to obtain molten inactive solder. When the titanium in the titanium alloy diffuses into the inactive solder, the molten active solder containing the active element titanium is obtained.

Step 3. Put the end face of the ceramic substrate to be surface metallized into a titanium alloy crucible filled with molten solder for 5 to 30 minutes.

Step 4: Take out the ceramic substrate, flatten and cool to obtain a uniform metallization layer on the end surface of the ceramic substrate.

The inactive solder mentioned in the second step of the present invention refers to a solder that does not contain active elements (such as Ti, Ge, etc.).

The inactive solder described in step 2 of the present invention is tin-based solder, aluminum-based solder or silver-based solder.

The brazing filler metal described in the second step of the present invention is heated by means of resistance or high-frequency induction.

The mass percentage of titanium in the molten solder changes correspondingly with the change of temperature of the active solder described in the second step of the present invention.

The ceramic substrate described in step 3 of the present invention is oxide ceramics, nitride ceramics or carbide ceramics.

In the third step of the present invention, the ceramic substrate should be shaken back and forth intermittently to promote the spread of the metallized layer, that is, to obtain a uniform metallized layer.

The invention not only simplifies the metallization process and reduces the production cost, but also the molten tin-based solder can be reused, which improves the utilization rate of the metallization alloy, and the liquid metallization alloy has better fluidity than powder. It is conducive to its spreading, and the thickness of the film layer is more uniform.

Detailed ways

The present invention will be further described below in conjunction with embodiment:

The present invention puts inactive solder into a titanium alloy crucible, and obtains molten inactive solder at a certain temperature in a vacuum or inert gas protection environment. Transition in the brazing filler metal, the active brazing filler metal containing the active element titanium is obtained, which reacts with the ceramic under certain temperature conditions to form a metallized layer.

Example 1: A ceramic surface metallization method, the steps are as follows: (1) Design and manufacture a titanium alloy crucible, and manufacture a titanium alloy crucible with a ceramic substrate size of 15 mm × 15 mm × 5 mm; Active solder, prepare 10g of tin-based solder with a mass fraction of 99% Sn and 1% Ag. The tin-based solder is in powder form and is composed of simple metals. Its mass purity is 99~99.95%, and the particles are not larger than 100um. Put tin-based solder in a titanium alloy crucible, and put it into a vacuum furnace together with alumina ceramics, under vacuum or inert gas conditions, with a vacuum degree of 10 ^-4 Pa, at a heating rate of 20°C/min Heating to 800°C to obtain molten active solder containing a certain amount of titanium. (3) Metallization: Put the alumina ceramics into the molten active solder and shake the ceramic substrate back and forth intermittently, let it stand for 10 minutes, and then take it out. Cool naturally to obtain a uniform and well-bonded metallization layer.

Example 2: A ceramic surface metallization method, the steps are as follows: (1) Design and manufacture a titanium alloy crucible, and manufacture a titanium alloy crucible with a ceramic substrate size of 15 mm × 15 mm × 5 mm; (2) weigh a mass fraction of 99 10g of tin-based solder with %Sn and 1%Cu ^is placed in a titanium alloy crucible and placed in a vacuum furnace together with alumina ceramics. Heating to 700°C, keeping it warm for 1min, (3) Metallization: Put the alumina ceramics into the molten tin-based solder and shake the ceramic substrate back and forth intermittently, let it stand for 20min, then take it out, and cool it naturally to get uniform and bonded Good metallization layer.

Embodiment 3: A kind of ceramic surface metallization method, steps are as follows: (one) design and manufacture titanium alloy crucible, the size of ceramic substrate is 15mm * 15mm * 5mm (two) take the tin that is 90%Sn, 10%Ag 10g of base brazing material is placed in a titanium alloy crucible, placed in a vacuum furnace, and heated to 950°C at a heating rate of 15°C/min under argon protection to obtain a molten active brazing filler metal containing a certain amount of titanium. (3) Metallization: Put the alumina ceramics into the molten active solder and shake the ceramic substrate back and forth intermittently for 5 minutes, then take it out and cool it naturally to obtain a uniform and well-bonded metallization layer.

Example 4: A ceramic surface metallization method, the steps are as follows: (1) Design and manufacture a titanium alloy crucible, the size of the ceramic substrate is 15 mm × 15 mm × 5 mm (2) Weigh 10 g of 90% Al, 10 %Cu aluminum-based brazing filler metal, aluminum-based brazing filler metal is composed of powdered metal, with a mass purity of 99~99.95%, and a particle size of 70um. Under the same conditions, heat to 950°C at a rate of 10°C/min to obtain a molten active solder containing a certain amount of titanium. (3) Metallization: put alumina ceramics into the molten active solder and intermittently reciprocate Shake the ceramic substrate for 5 minutes, then take it out, and let it cool naturally to obtain a uniform and well-bonded metallization layer.

Example 5: A ceramic surface metallization method, the steps are as follows: (1) Design and manufacture a titanium alloy crucible, the size of the ceramic substrate is 15mm × 15mm × 5mm (2) Weigh 95% Sn, 5% Ag, 5% Cu tin-based solder 10g, placed in a titanium alloy crucible, and placed in a vacuum furnace together with alumina ceramics, heated to 950°C at a rate of 10°C/min under the protection of argon, Obtain molten active solder containing a certain amount of titanium. (3) Metallization: Put the alumina ceramics into the molten active solder and shake the ceramic substrate back and forth intermittently for 10 minutes, then take it out and cool it naturally to obtain a uniform, bonded Good metallization layer.

Claims (6)

1. A ceramic surface metallization method, characterized in that the steps are as follows: Step 1. Design and manufacture a titanium alloy crucible, Step 2: Put the inactive solder in a titanium alloy crucible, and heat it to 700°C~1000°C at a heating rate of 5~20°C/min under vacuum or inert atmosphere protection conditions to obtain molten inactive solder. When the titanium in the titanium alloy diffuses into the inactive solder, the molten active solder containing the active element titanium is obtained. Step 3. Put the end face of the ceramic substrate to be surface metallized into a titanium alloy crucible filled with molten solder for 5 to 30 minutes. Step 4: Take out the ceramic substrate, flatten and cool to obtain a uniform metallization layer on the end surface of the ceramic substrate. 2. A method for metallizing ceramic surfaces according to claim 1, wherein the inactive solder in step 1 is tin-based solder, aluminum-based solder or silver-based solder. 3. A ceramic surface metallization method according to claim 1, characterized in that the brazing filler metal is heated in the second step by means of resistance or high-frequency induction. 4. A kind of ceramic surface metallization method according to claim 1, is characterized in that in the step 2, active brazing filler metal changes with temperature, and the mass percent of titanium in the molten brazing filler metal changes correspondingly. 5. A ceramic surface metallization method according to claim 1, characterized in that the ceramic substrate in step 3 is oxide ceramics, nitride ceramics or carbide ceramics. 6. A method for metallizing ceramic surfaces according to claim 1, characterized in that in step 3, the ceramic substrate is intermittently shaken back and forth to promote the spreading of the metallized layer.