CN103864467B - A kind of ceramic surface metallization method - Google Patents
A kind of ceramic surface metallization method Download PDFInfo
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- CN103864467B CN103864467B CN201410121881.2A CN201410121881A CN103864467B CN 103864467 B CN103864467 B CN 103864467B CN 201410121881 A CN201410121881 A CN 201410121881A CN 103864467 B CN103864467 B CN 103864467B
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Abstract
The invention discloses a kind of ceramic surface metallization method, it is characterized in that step is as follows: step one, design and manufacture titanium alloy crucible, step 2, nonactive solder is placed in titanium alloy crucible, under vacuum or inert atmosphere protection condition, 700 DEG C ~ 1000 DEG C are heated to the temperature rise rate of 5 ~ 20 DEG C/min, obtain the nonactive solder of melting, titanium now in titanium alloy spreads in nonactive solder, obtain the active solder containing active element titanium of melting, step 3, the ceramic substrate end face of surface metalation will put into the titanium alloy crucible that molten solder is housed, time 5 ~ 30min, step 4, take out ceramic substrate, namely tiling cooling obtains uniform metal layer on ceramic substrate end face, the present invention not only makes metallization process be simplified, reduce production cost, and the solder of melting can reuse, improve the utilization ratio of metallization alloy, liquid metal alloy is compared powdery and is had better mobility this is beneficial to it and sprawls, and the thickness of rete is more even, good operability, batch micro operations can be realized.
Description
Technical field
The present invention relates to a kind of novel material, specifically a kind of ceramic surface metallization method.
Background technology
Pottery has high temperature resistant, many excellent performances such as high strength, high rigidity, high-wearing feature, improved corrosion, but pottery poor toughness at normal temperatures, is difficult to the part preparing complicated shape.Only have and the obdurability of metal is combined with ceramic wear resistance, erosion resistance, high thermal resistance, just can become desirable structured material.General needs could link together with metal at ceramic surface metallization.
At present, it is that molybdenum powder and oxidation manganese powder are hybridly prepared into slurry that the method for ceramic surface pre-metallization mainly contains method, is coated in ceramic surface, then at 1500 DEG C of sintering, forms metal molybdenum layer at ceramic surface.The method belongs to high temperature conjunction, and it will inevitably bring following problem: (1) equipment requirements is strict; (2) large size and baroque joint easily produce large internal stress; (3) connect temperature and exceed multiple Mo-Mn method, electroless plating and vapour deposition etc.Its strengthening or malleableize effect seriously can be reduced when wherein Mo-Mn closes the allowable temperature of strengthening phase or malleableize phase in pottery; Two is electroless plating methods, and its technical process is: and oil removing → flowing water washes → neutralizes → flowing water washes → and alligatoring → flowing water washes → sensitization → distillation washing → activation → distillation washing → reduction → electroless plating.The method complex steps, and the discharge of chemical plating fluid can to environment, three is vapour deposition processes, it is divided into chemical vapour deposition and physical vapor deposition, chemical vapor deposition (CVD) is the Technology by space gas-phase chemical reaction depositing solid films on matrix surface, and physical vapor deposition (PVD) adopts the method for heating or high energy beam bombardment that material to be plated or target are flashed to gaseous state in a vacuum chamber and makes it to be deposited in the technology that workpiece surface forms coating.The method is high to equipment requirements, manufacturing cost is high.
Summary of the invention
Object of the present invention is exactly to overcome the deficiencies in the prior art, provides that a kind of technique is simple, the uniform ceramic surface metallization method of layer of metallized film.
The present invention is reached by following measure:
A kind of ceramic surface metallization method, is characterized in that step is as follows:
Step one, design and manufacture titanium alloy crucible,
Step 2, nonactive solder is placed in titanium alloy crucible; under vacuum or inert atmosphere protection condition; 700 DEG C ~ 1000 DEG C are heated to the temperature rise rate of 5 ~ 20 DEG C/min; obtain the nonactive solder of melting; titanium now in titanium alloy spreads in nonactive solder; obtain the active solder containing active element titanium of melting
Step 3, the ceramic substrate end face of surface metalation will put into the titanium alloy crucible that molten solder is housed, time 5 ~ 30min,
Step 4, taking-up ceramic substrate, namely tiling cooling obtains uniform metal layer on ceramic substrate end face.
Nonactive solder described in step 2 of the present invention refers to the solder not containing active element (as Ti, Ge etc.).
Nonactive solder described in step 2 of the present invention is tin-based solder, aluminium base solder or silver-base solder.
Solder heat described in step 2 of the present invention adopts the mode of resistance or high-frequency induction to heat.
Active solder variation with temperature described in step 2 of the present invention, the mass percent respective change of titanium in molten solder.
Ceramic substrate described in step 3 of the present invention is oxide ceramics, nitride ceramics or carbide ceramics.
Want intermittent in step 3 of the present invention and rock ceramic substrate back and forth, promote sprawling of metal layer, namely obtain uniform metal layer.
The present invention not only makes metallization process be simplified, reduce production cost, and the tin-based solder of melting can reuse, improve the utilization ratio of metallization alloy, liquid metal alloy is compared powdery and is had better mobility this is beneficial to it and sprawls, and the thickness of rete is more even.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Nonactive solder is put into titanium alloy crucible by the present invention; in vacuum or protection of inert gas environment; obtain the nonactive solder of melting at a certain temperature; at this moment; titanium in titanium alloy is to transition in the nonactive solder of melting; just obtain the active solder containing active element titanium, react with pottery under certain temperature condition and form metal layer.
Embodiment 1: a kind of ceramic surface metallization method, step is as follows: (one) designs and manufactures titanium alloy crucible, be of a size of 15mm × 15mm × 5mm with ceramic substrate and manufacture titanium alloy crucible, (2) the nonactive solder of certain mass is taken, preparation mass fraction is 99%Sn, the tin-based solder 10g of 1%Ag, tin-based solder adopts Powdered, be made up of metal simple-substance, its quality purity is 99 ~ 99.95%, particle is not more than 100um, tin-based solder is placed in titanium alloy crucible, and together put into vacuum oven with alumina-ceramic, under vacuum or inert gas conditions, vacuum tightness is 10
-4under Pa condition, with the heating rate of 20 DEG C/min to 800 DEG C, obtain the active solder containing Quantitative titanium of melting, (3) metallize: alumina-ceramic put into the active solder of melting and intermittently rock ceramic substrate back and forth, leave standstill 10min, then take out, naturally cooling, obtain evenly, in conjunction with good metal layer.
Embodiment 2: a kind of ceramic surface metallization method, step is as follows: (one) designs and manufactures titanium alloy crucible, be of a size of 15mm × 15mm × 5mm with ceramic substrate and manufacture titanium alloy crucible, (2) taking massfraction is 99%Sn, the 10g tin-based solder of 1%Cu, being placed in titanium alloy crucible, and together putting into vacuum oven with alumina-ceramic, is 10 in vacuum tightness
-4under Pa condition, be heated to 700 DEG C with the speed of 5 DEG C/min, insulation 1min, (3) metallize: alumina-ceramic put into the tin-based solder of melting and intermittently rock ceramic substrate back and forth, leave standstill 20min, then take out, naturally cooling, obtains evenly, in conjunction with good metal layer.
Embodiment 3: a kind of ceramic surface metallization method, step is as follows: (one) designs and manufactures titanium alloy crucible, ceramic substrate is of a size of 15mm × 15mm × 5mm(bis-) take as 90%Sn, the tin-based solder 10g of 10%Ag, be placed in titanium alloy crucible, put into vacuum oven, under argon shield condition, with the heating rate of 15 DEG C/min to 950 DEG C, obtain the active solder containing a certain amount of titanium of melting, (3) metallize: alumina-ceramic put into the active solder of melting and intermittently rock ceramic substrate 5min back and forth, then take out, naturally cooling, obtain evenly, in conjunction with good metal layer.
Embodiment 4: a kind of ceramic surface metallization method, step is as follows: (one) designs and manufactures titanium alloy crucible, ceramic substrate is of a size of 15mm × 15mm × 5mm(bis-) to take 10g mass fraction be 90%Al, the aluminium base solder of 10%Cu, aluminium base solder adopts powder metal simple substance composition, quality purity is 99 ~ 99.95%, granular size is 70um, aluminium base solder and alumina-ceramic together put into vacuum oven, under argon shield condition, 950 DEG C are heated to the speed of 10 DEG C/min, obtain the active solder containing a certain amount of titanium of melting, (3) metallize: alumina-ceramic put into the active solder of melting and intermittently rock ceramic substrate 5min back and forth, then take out, naturally cooling, obtain evenly, in conjunction with good metal layer.
Embodiment 5: a kind of ceramic surface metallization method, step is as follows: (one) designs and manufactures titanium alloy crucible, ceramic substrate is of a size of 15mm × 15mm × 5mm(bis-) to take mass fraction be 95%Sn, 5%Ag, the tin-based solder 10g of 5%Cu, be placed in titanium alloy crucible, and together put into vacuum oven with alumina-ceramic, under argon shield condition, 950 DEG C are heated to the speed of 10 DEG C/min, obtain the active solder containing a certain amount of titanium of melting, (3) metallize: alumina-ceramic put into the active solder of melting and intermittently rock ceramic substrate 10min back and forth, then take out, naturally cooling, obtain evenly, in conjunction with good metal layer.
Claims (3)
1. a ceramic surface metallization method, is characterized in that step is as follows:
Step one, design and manufacture titanium alloy crucible,
Step 2, nonactive solder is placed in titanium alloy crucible, nonactive solder is tin-based solder, aluminium base solder or silver-base solder, is 10 in vacuum tightness
-4under the vacuum of Pa or inert atmosphere protection condition; the mode of resistance or high-frequency induction is adopted to heat; 700 DEG C ~ 1000 DEG C are heated to the temperature rise rate of 5 ~ 20 DEG C/min; obtain the nonactive solder of melting; titanium now in titanium alloy spreads in nonactive solder; obtain the active solder containing active element titanium of melting
Step 3, the ceramic substrate end face of surface metalation will put into the titanium alloy crucible that molten solder is housed, intermittently rock ceramic substrate back and forth, promote sprawling of metal layer, time 5 ~ 30min,
Step 4, taking-up ceramic substrate, namely tiling cooling obtains uniform metal layer on ceramic substrate end face.
2. a kind of ceramic surface metallization method according to claim 1, is characterized in that active solder variation with temperature in step 2, the mass percent respective change of titanium in molten solder.
3. a kind of ceramic surface metallization method according to claim 1, is characterized in that the ceramic substrate in step 3 is oxide ceramics, nitride ceramics or carbide ceramics.
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| CN105149717A (en) * | 2015-10-19 | 2015-12-16 | 哈尔滨工业大学 | Silicon-based ceramic surface metallization method |
| CN115302033B (en) * | 2022-08-22 | 2023-11-21 | 哈尔滨工业大学（威海） | Low-temperature indirect brazing method for zirconia ceramic and titanium alloy |
| CN116332629B (en) * | 2023-03-30 | 2024-02-06 | 中国科学院上海硅酸盐研究所 | Alumina ceramic-titanium alloy integrated composite structure and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467140A (en) * | 2013-09-03 | 2013-12-25 | 江苏大学 | Surface metalized layer of silicon carbide ceramic and metalizing method of silicon carbide ceramic |
| CN103464855A (en) * | 2013-09-26 | 2013-12-25 | 郑州机械研究所 | Stationary wave restrained large-area hard alloy soldering method and special equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467140A (en) * | 2013-09-03 | 2013-12-25 | 江苏大学 | Surface metalized layer of silicon carbide ceramic and metalizing method of silicon carbide ceramic |
| CN103464855A (en) * | 2013-09-26 | 2013-12-25 | 郑州机械研究所 | Stationary wave restrained large-area hard alloy soldering method and special equipment |
Non-Patent Citations (1)
| Title |
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| AlN陶瓷活性法金属化;张小勇等;《真空电子技术》;20071231(第4期);第53－55、73页 * |
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