CN103319209B - Metalized deposition method of nickel coating on ceramic surface - Google Patents
Metalized deposition method of nickel coating on ceramic surface Download PDFInfo
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- CN103319209B CN103319209B CN201310214709.7A CN201310214709A CN103319209B CN 103319209 B CN103319209 B CN 103319209B CN 201310214709 A CN201310214709 A CN 201310214709A CN 103319209 B CN103319209 B CN 103319209B
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Abstract
The invention discloses a metalized deposition method of a nickel coating on the ceramic surface. The method provided by the invention comprises the following steps: roughening ceramic and putting the roughened ceramic into a quartz tube, putting NiCl2 into a material vessel, and putting the material boat into the quartz tube; Putting the quartz tube into a program control box-type furnace, vacuumizing the program control box-type furnace and letting inert gas pass in, letting hydrogen pass in when the temperature in the program control box-type furnace rises to 700-800 DEG C under the condition of continuously letting inert gas pass in, continuously heating to 1000-1250 DEG C under the condition of continuously letting inert gas and hydrogen pass in, and insulating. The compact and smooth nickel coating which has advantages of good binding force with a matrix, high purity and uniform surface is prepared by the method. Reaction tail gas will not cause pollution to the nickel coating. According to the invention, the ceramic surface requires no sensitization treatment; the method is simple to operate and requires low cost; the nickel coating has less toxicity than nickel carbonyl; wetability between ceramic and metal is improved; and the method can be widely applied in preparation of a ceramic metal-matrix composite material.
Description
Technical field
The invention belongs to stupalith field, relate to the thin film metallized method of stupalith, be specifically related to a kind of method in ceramic surface metallization nickel deposited coating.
Background technology
Al
2o
3pottery, as common stupalith, has the features such as high temperature resistant, wear-resistant, corrosion-resistant, high rigidity, and wide material sources, low price.But its toughness is very poor, performance and the practical application of its premium properties have been restricted.Metallic substance has the characteristics such as good toughness, heat conduction, conduction, but density is large, and hardness is low, anti-corrosion and wear resistance is relatively poor.Single pottery and metal cannot meet people's demand, and ceramic-metal composites becomes people and studies new focus.Ceramic-metal composites is all widely used in aerospace, electronic industry, measurement instrument industry and Tool Industry.
But pottery has very large difference with the various performance perameters of metal, is mainly manifested in: both have different chemical bonds, be difficult to realize good metallurgy and connect; Pottery is different from the thermal expansivity of metal, during connection, easily produce larger unrelieved stress, so pottery is bad with the wettability of metal, therefore in ceramic-metal composites, often need surface modification in advance to improve the problems such as combination wettability between pottery and metal is poor.
Changing at present the poor more conventional method for surface metallation of ceramic metal wettability has dectroless plating, coating by vaporization metallization, ion sputtering method and chemical Vapor deposition process etc. to realize ceramic metallization.As the patent 201010520736.3 of the people such as Qu Xuanhui application in 2010, adopt the method for nickel salt liquid impregnation electroless plating, on the substrate aluminium nitride ceramics surface of difficulty plating, obtain dense smooth nickel coating, changed ceramic wettability.But the coating obtaining contains phosphorus, some high-end metallized ceramic base plates (as DBC substrate) are very high to the requirement of its weldability and solder joint, and the nickel coating of rich phosphorus can cause welding spot reliability to decline, and chemical nickel plating is to meet its needs conventionally; And chemical plating solution poor stability, safeguards, adjusts and regenerate cumbersomely, and cost is higher.Comparatively speaking, chemical Vapor deposition process has a lot of advantages: technique is simple, cost is low,, density and the coating purity that can control coating good around plating property.Can plated film on the matrix of complicated shape and on particulate material.Be applicable to apply the workpiece of various complicated shapes, good around plating performance due to chemical vapour deposition, so can apply the workpiece with trough, hole or even blind hole.
The Liu Shiliang of the Central China University of Science and Technology, the people such as Zhao Lifeng adopt the method for chemical vapour deposition, using nickle carbonoxide as presoma, obtained nickel film, its shortcoming is that nickle carbonoxide and reaction product CO thereof have higher toxicity and nickel film to be subject to there will be the pollution of carbon to nickel film in the pollution deposit process of degradation production.
Summary of the invention
Object of the present invention, in order to overcome prior art problem, provides a kind of method in ceramic surface metallization nickel deposited coating, and operation is simple for it, with low cost, and the tail gas of reaction can not pollute nickel coating, and toxicity is little.
For achieving the above object, the present invention adopts following technical scheme:
A method in ceramic surface metallization nickel deposited coating, comprises the following steps,
First, pottery is carried out putting into silica tube after roughening treatment, then by NiCl
2put into material boat, then material boat is put into silica tube; Then silica tube is put into program control box-type furnace, after being vacuumized, program control box-type furnace passes into rare gas element, continuing to pass under the condition of rare gas element, when being warming up to 700-800 ℃, program control box-type furnace passes into hydrogen, then continue to be warming up to 1000-1250 ℃ continuing to pass under the condition of rare gas element and hydrogen, at 1000-1250 ℃, be incubated, obtain the pottery of surface deposition nickel coating.
The method that the roughening treatment of described pottery adopts is: after with 300 orders, 400 orders, 500 order waterproof abrasive papers, pottery being polished successively, by washed with de-ionized water; Again pottery is put into spirituous solution, ultrasonic cleaning 10-15min, then use washed with de-ionized water.
Described NiCl
2by NiCl
26H
2o carries out that processed obtains, and the method for processed is: by NiCl
26H
2o is incubated 2-3 hour at 135-200 ℃, then grinds, then be incubated 1-2 hour at 250-300 ℃.
The time of described insulation is 30-60min.
The speed of described intensification is 20 ℃/min.
After described vacuumizing, passing into rare gas element is specially: when being evacuated to vacuum tightness and being 0.1MPa, stop vacuumizing, pass into rare gas element, repeat to vacuumize the operation 3 times of rear logical rare gas element.
Described rare gas element intake is 200-300mL/min, and the intake of hydrogen is 100-200mL/min.
Described rare gas element is argon gas.
With respect to prior art, the beneficial effect that the present invention has: the present invention is by cheap NiCl
2as presoma, method with halogenide reduction, by chemical vapour deposition at ceramic surface, obtain fine and close smooth, good with basal body binding force, purity is high, the nickel coating of surface uniform, the tail gas of reaction can not pollute nickel coating, the present invention is without ceramic surface is carried out to sensitization processing, simple to operate, with low cost, toxicity is much smaller compared with nickle carbonoxide, pottery through nickel plating has strengthened the combination of pottery with metal, has improved the wettability between ceramic metal, can be widely used in the preparation of ceramic metal based composites; In addition, the present invention is not only applicable to flaky pottery, and the plating nickel on surface of the device of the arbitrary shape that is applicable to be made by pottery is processed.
Accompanying drawing explanation
Fig. 1 is the metal Ni coating XRD diffractogram that the present invention makes;
Fig. 2 is the micro-structure diagram of the ceramic Ni metal layer prepared of the present invention.
Embodiment
Below in conjunction with accompanying drawing, by specific examples, the invention will be further described.
Following examples are all to take the Al that radius is 3mm as 10mm, thickness
2o
3ceramic plate is that example describes, but should not be considered as limitation of the invention.
Embodiment 1
(1) use successively 300 orders, 400 orders, 500 order liquid honing Al
2o
3ceramic plate, and by washed with de-ionized water, then ceramic plate is put into spirituous solution, ultrasonic cleaning 15min, then use washed with de-ionized water 3 times, seasoning, obtains cleaning and has the Al of uneven surface
2o
3ceramic plate, passes through the ceramic plate of roughening treatment;
(2) with electronic balance, take the NiCl of 15g
26H
2o puts into crucible, then crucible is put into thermostatic drying chamber, at 135 ℃, is incubated 3 hours, then takes out with mortar, to pulverize lastly, then puts into thermostatic drying chamber, at 250 ℃, is incubated 2 hours, obtains luteotestaceous NiCl
2powder, and by NiCl
2powder is put into material boat;
(3) first by crossing, through the ceramic plate of roughening treatment, put into silica tube, then will fill NiCl
2the material boat of powder is put into silica tube, finally silica tube is put into program control box-type furnace, is evacuated to 0.1MPa and stops vacuumizing, and passes into argon gas, repeats to vacuumize the operation 3 times of logical argon gas; Vacuumize in order to remove airborne O
2, avoid O
2with reactant gases H
2the danger that reaction is blasted;
(4) continuing to pass under the condition of argon gas, with the temperature rise rate of 20 ℃/min, when being warming up to 800 ℃, program control box-type furnace passes into H
2, when then continuing at the same time to pass into the temperature rise rate continuing under the condition of argon gas and hydrogen with 20 ℃/min and being heated to 1150 ℃, after stopping heating and be incubated 60min at 1150 ℃, cool to room temperature with the furnace; Wherein, argon gas intake is 300mL/min, H
2intake is 200mL/min;
(5) take out ceramic plate and its surface is cleaned repeatedly, then drying, obtaining the surperficial ceramic plate with nickel deposited coating; The nickel coating depositing on ceramic plate is even, and nickel coating thickness is about 40 μ m.
The present invention to implement the 1 surface deposition nickel coating making carrying out XRD diffraction and scanning electron microscope measure; As shown in Figure 1, can find out that embodiment 1 has obtained the higher nickel coating of purity on ceramic plate surface, overcome the phosphorous and problem that causes welding spot reliability to decline of nickel coating in existing electroless plating technology.As shown in Figure 2, can find out the smooth densification of nickel coating, uniform and delicate, there is no crackle and pore, the combination of ceramic plate and coating is good, matrix and coating junction do not exist flaw, and the thickness of coating is about 40 μ m.
Embodiment 2
(1) use successively 300 orders, 400 orders, 500 order liquid honing Al
2o
3ceramic plate, and by washed with de-ionized water, then ceramic plate is put into spirituous solution, ultrasonic cleaning 10min, then use washed with de-ionized water 3 times, seasoning, obtains cleaning and has the Al of uneven surface
2o
3ceramic plate, passes through the ceramic plate of roughening treatment;
(2) with electronic balance, take the NiCl of 15g
26H
2o puts into crucible, then crucible is put into thermostatic drying chamber, at 200 ℃, is incubated 2.5 hours, then takes out with mortar, to pulverize lastly, then puts into thermostatic drying chamber, at 300 ℃, is incubated 1.5 hours, obtains luteotestaceous NiCl
2powder, and by NiCl
2powder is put into material boat;
(3) first by crossing, through the ceramic plate of roughening treatment, put into silica tube, then will fill NiCl
2the material boat of powder is put into silica tube, finally silica tube is put into program control box-type furnace, is evacuated to 0.1MPa and stops vacuumizing, and passes into rare gas element Ar, repeats to vacuumize the operation 3 times of logical argon gas; Vacuumize in order to remove airborne O
2, avoid O
2with reactant gases H
2the danger that reaction is blasted;
(4) continuing to pass under the condition of argon gas, with the temperature rise rate of 20 ℃/min, when being warming up to 700 ℃, program control box-type furnace passes into H
2, when then continuing at the same time to pass into the temperature rise rate continuing under the condition of argon gas and hydrogen with 20 ℃/min and being heated to 1200 ℃, after stopping heating and be incubated 30min at 1200 ℃, cool to room temperature with the furnace; Wherein, argon gas intake is 250mL/min; H
2intake is 150mL/min;
(5) take out ceramic plate and its surface is cleaned repeatedly, then drying, obtaining the surperficial ceramic plate with nickel deposited coating; The nickel coating depositing on ceramic plate is even.
Embodiment 3
(1) use successively 300 orders, 400 orders, 500 order liquid honing Al
2o
3ceramic plate, and by washed with de-ionized water, then ceramic plate is put into spirituous solution, ultrasonic cleaning 12min, then use washed with de-ionized water 3 times, seasoning, obtains cleaning and has the Al of uneven surface
2o
3ceramic plate, passes through the ceramic plate of roughening treatment;
(2) with electronic balance, take the NiC1 of 15g
26H
2o puts into crucible, then crucible is put into thermostatic drying chamber, at 170 ℃, is incubated 2 hours, then takes out with mortar, to pulverize lastly, then puts into thermostatic drying chamber, at 280 ℃, is incubated 1 hour, obtains luteotestaceous NiCl
2powder, and by NiCl
2powder is put into material boat;
(3) first by crossing, through the ceramic plate of roughening treatment, put into silica tube, then will fill NiCl
2the material boat of powder is put into silica tube, finally silica tube is put into program control box-type furnace, is evacuated to 0.1MPa and stops vacuumizing, and passes into rare gas element Ar, repeats to vacuumize the operation 3 times of logical argon gas; Vacuumize in order to remove airborne O
2, avoid O
2with reactant gases H
2the danger that reaction is blasted;
(4) continuing to pass under the condition of argon gas, with the temperature rise rate of 20 ℃/min, when being warming up to 750 ℃, program control box-type furnace passes into H
2, when then continuing at the same time to pass into the temperature rise rate continuing under the condition of argon gas and hydrogen with 20 ℃/min and being heated to 1250 ℃, after stopping heating and be incubated 45min at 1250 ℃, cool to room temperature with the furnace; Wherein, argon gas intake is 200mL/min, H
2intake is 100mL/min;
(5) take out ceramic plate and its surface is cleaned repeatedly, then drying, obtaining the surperficial ceramic plate with nickel deposited coating; The nickel coating depositing on ceramic plate is even.
Embodiment 4
(1) use successively 300 orders, 400 orders, 500 order liquid honing Al
2o
3ceramic plate, and by washed with de-ionized water, then ceramic plate is put into spirituous solution, ultrasonic cleaning 13min, then use washed with de-ionized water 3 times, seasoning, obtains cleaning and has the Al of uneven surface
2o
3ceramic plate, passes through the ceramic plate of roughening treatment;
(2) with electronic balance, take the NiCl of 15g
26H
2o puts into crucible, then crucible is put into thermostatic drying chamber, at 180 ℃, is incubated 2.4 hours, then takes out with mortar, to pulverize lastly, then puts into thermostatic drying chamber, at 265 ℃, is incubated 1 hour, obtains luteotestaceous NiCl
2powder, and by NiCl
2powder is put into material boat;
(3) first by crossing, through the ceramic plate of roughening treatment, put into silica tube, then will fill NiCl
2the material boat of powder is put into silica tube, finally silica tube is put into program control box-type furnace, is evacuated to 0.1MPa and stops vacuumizing, and passes into argon gas, repeats to vacuumize the operation 3 times of logical argon gas; Vacuumize in order to remove airborne O
2, avoid O
2with reactant gases H
2the danger that reaction is blasted;
(4) continuing to pass under the condition of argon gas, with the temperature rise rate of 20 ℃/min, when being warming up to 770 ℃, program control box-type furnace passes into H
2, when then continuing at the same time to pass into the temperature rise rate continuing under the condition of argon gas and hydrogen with 20 ℃/min and being heated to 1100 ℃, after stopping heating and be incubated 50min at 1100 ℃, cool to room temperature with the furnace; Wherein, argon gas intake is 270mL/min, H
2intake is 130mL/min;
(5) take out ceramic plate and its surface is cleaned repeatedly, then drying, obtaining the surperficial ceramic plate with nickel deposited coating; The nickel coating depositing on ceramic plate is even.
Embodiment 5
(1) use successively 300 orders, 400 orders, 500 order liquid honing Al
2o
3ceramic plate, and by washed with de-ionized water, then ceramic plate is put into spirituous solution, ultrasonic cleaning 10min, then use washed with de-ionized water 3 times, seasoning, obtains cleaning and has the Al of uneven surface
2o
3ceramic plate, passes through the ceramic plate of roughening treatment;
(2) with electronic balance, take the NiCl of 15g
26H
2o puts into crucible, then crucible is put into thermostatic drying chamber, at 200 ℃, is incubated 3 hours, then takes out with mortar, to pulverize lastly, then puts into thermostatic drying chamber, at 290 ℃, is incubated 1.8 hours, obtains luteotestaceous NiCl
2powder, and by NiCl
2powder is put into material boat;
(3) first by crossing, through the ceramic plate of roughening treatment, put into silica tube, then will fill NiCl
2the material boat of powder is put into silica tube, finally silica tube is put into program control box-type furnace, is evacuated to 0.1MPa and stops vacuumizing, and passes into argon gas, repeats to vacuumize the operation 3 times of logical argon gas; Vacuumize in order to remove airborne O
2, avoid O
2with reactant gases H
2the danger that reaction is blasted;
(4) continuing to pass under the condition of argon gas, with the temperature rise rate of 20 ℃/min, when being warming up to 720 ℃, program control box-type furnace passes into H
2, when then continuing at the same time to pass into the temperature rise rate continuing under the condition of argon gas and hydrogen with 20 ℃/min and being heated to 1000 ℃, after stopping heating and be incubated 40min at 1000 ℃, cool to room temperature with the furnace; Wherein, argon gas intake is 230mL/min, and hydrogen intake is 180mL/min;
(5) take out ceramic plate and its surface is cleaned repeatedly, then drying, obtaining the surperficial ceramic plate with nickel deposited coating; The nickel coating depositing on ceramic plate is even.
The present invention adopts NiCl
2as presoma, by the method for halogenide reduction, with the method for chemical vapour deposition obtain fine and close smooth, and basal body binding force is good, purity is high, the nickel coating of surface uniform, the tail gas of its reaction can not pollute film, and NiCl
2cheap, toxicity is much smaller compared with nickle carbonoxide, and the nickel plating pottery making can be widely used in ceramic matric composite.
The present invention only be take aluminium sesquioxide ceramic plate and is carried out ceramic surface nickel deposited coating as example, the present invention is equally applicable to the ceramic surface nickel deposited coating of other materials, and the present invention is not only applicable to flaky pottery, and the plating nickel on surface of the device of the arbitrary shape that is applicable to be made by pottery is processed.
Claims (5)
1. in a method for ceramic surface metallization nickel deposited coating, it is characterized in that, first, pottery is carried out putting into silica tube after roughening treatment, then by NiCl
2put into material boat, then material boat is put into silica tube; Then silica tube is put into program control box-type furnace, after being vacuumized, program control box-type furnace passes into rare gas element, continuing to pass under the condition of rare gas element, when being warming up to 700-800 ℃, program control box-type furnace passes into hydrogen, then continue to be warming up to 1000-1250 ℃ continuing to pass under the condition of rare gas element and hydrogen, at 1000-1250 ℃, be incubated, obtain the pottery of surface deposition nickel coating;
The time of described insulation is 30-60min;
Described rare gas element intake is 200-300mL/min, and the intake of hydrogen is 100-200mL/min;
Described rare gas element is argon gas.
2. the method in ceramic surface metallization nickel deposited coating according to claim 1, is characterized in that, the method that the roughening treatment of described pottery adopts is: after with 300 orders, 400 orders, 500 order waterproof abrasive papers, pottery being polished successively, by washed with de-ionized water; Again pottery is put into spirituous solution, ultrasonic cleaning 10-15min, then use washed with de-ionized water.
3. the method in ceramic surface metallization nickel deposited coating according to claim 1, is characterized in that, described NiCl
2by NiC1
26H
2o carries out that processed obtains, and the method for processed is: by NiC1
26H
2o is incubated 2-3 hour at 135-200 ℃, then grinds, then be incubated 1-2 hour at 250-300 ℃.
4. the method in ceramic surface metallization nickel deposited coating according to claim 1, is characterized in that, the speed of described intensification is 20 ℃/min.
5. the method in ceramic surface metallization nickel deposited coating according to claim 1, it is characterized in that, described in pass into rare gas element after vacuumizing and be specially: when being evacuated to vacuum tightness and being 0.1MPa, stop vacuumizing, pass into rare gas element, repeat to vacuumize the operation 3 times of rear logical rare gas element.
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| CN201310214709.7A CN103319209B (en) | 2013-05-31 | 2013-05-31 | Metalized deposition method of nickel coating on ceramic surface |
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|---|---|---|---|
| CN201310214709.7A CN103319209B (en) | 2013-05-31 | 2013-05-31 | Metalized deposition method of nickel coating on ceramic surface |
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| CN104987134B (en) * | 2015-07-29 | 2017-04-12 | 长安大学 | Method for preparing nickel coating on ceramic surface by using in-situ reduction method |
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Non-Patent Citations (6)
| Title |
|---|
| 刘世良等.金属有机物化学气相沉积法沉积镍膜的影响因素.《材料保护》.2004,第37卷(第6期),4-6. |
| 张淑英 等.超细镍粉化学气相法制备过程中温度的影响.《湖南工业大学学报》.2010,第24卷(第4期),14-16. |
| 杨敏 等.陶瓷与金属连接的研究进展.《山东冶金》.2004,第26卷(第1期),37-40. |
| 超细镍粉化学气相法制备过程中温度的影响;张淑英 等;《湖南工业大学学报》;20100731;第24卷(第4期);14-16 * |
| 金属有机物化学气相沉积法沉积镍膜的影响因素;刘世良等;《材料保护》;20040630;第37卷(第6期);4-6 * |
| 陶瓷与金属连接的研究进展;杨敏 等;《山东冶金》;20040229;第26卷(第1期);37-40 * |
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