CN103288494B - Method for preparing titanium metal coating on ceramic surface - Google Patents
Method for preparing titanium metal coating on ceramic surface Download PDFInfo
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- CN103288494B CN103288494B CN201310182744.5A CN201310182744A CN103288494B CN 103288494 B CN103288494 B CN 103288494B CN 201310182744 A CN201310182744 A CN 201310182744A CN 103288494 B CN103288494 B CN 103288494B
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Abstract
The invention discloses a method for preparing a titanium metal coating on a ceramic surface. The method for preparing the titanium metal coating on the ceramic surface comprises the following steps of: firstly, placing ceramic the surface of which is treated into a quartz tube; then placing a mixture of titanium powder and iodine powder into a container, and placing the container into the quartz tube; then placing the quartz tube into a program control furnace, vacuumizing the program control furnace repeatedly, and introducing an inert gas, warming the program control furnace at the warming speed of 15-20 DEG C/min to 1030-1200 DEG C and carrying out heat preservation, and cooling, thereby obtaining the ceramic the surface of which is coated with the metal coating. The coating provided by the invention is high in purity, and has strong bonding force with base body ceramic, is uniform in distribution on the whole ceramic plane, can form a smooth deposition surface easily; and the device is simple, low in cost and simple to operate.
Description
Technical field
The present invention belongs to pottery and processes and make its surface metalation technical field, relates to a kind of method that makes its surface metalation that pottery is processed, and is specifically related to a kind of method of preparing titanium metal coating at ceramic surface.
Background technology
Along with scientific and technical develop rapidly, more and more higher to the requirement of material over-all properties, the superior material of single performance cannot meet the demand of practical application.Therefore the matrix material that, has structured material, functional materials or a structure-function integration of excellent comprehensive performance more and more comes into one's own.
Metal composite is owing to having high specific strength, specific modulus, wear resistance, high-temperature behavior that thermal expansivity is little, good, and many advantages such as good heat conduction, electroconductibility etc., add its low price, aboundresources, make it be subject to attention both domestic and external, in decades, make great progress in the past.Metal current matrix material has the metal-base composites of 3 types with the formal classification of reinforcement: particle strengthens, whisker strengthens and continuous fiber strengthens, and the reinforced effects of these 3 kinds of enhancement methods strengthens successively.But it is larger respectively to otherness to find that with people's research traditional metal-base composites exists in performance.
Therefore to metal composite, adopt recently porous ceramics or foamed ceramics as reinforcement, then metal is immersed in reinforcement, form so-called three-dimensional ceramic and strengthen metal composite.Three-dimensional ceramic strengthens metal composite and has advantages of manyly, as ceramic phase in structure and metallographic phase intersect mutually, mutually runs through and permeates, and is evenly distributed; In performance, have that higher bearing capacity and anti-impact force, high temperature dimensional performance are stable, high-wearing feature.Compared with traditional metal composite, there is more unique mechanical property, wear Characteristics, damping property and thermomechanical property, and possess performance isotropy.Thereby there is very wide application prospect.
Greatest difficulty prepared by three-dimensional ceramic enhancing metal composite is that therefore the wettability between metal and pottery is poor because stupalith is different from the bonding mechanism of metallic substance.Wettability how to improve metal pair pottery is key factor prepared by present material.Improving at present pottery is at ceramic surface metallization with intermetallic wettability the best way.As the Yang Shaofeng of South China Science & Engineering University etc. adopts the method for nickel salt liquid impregnation at the coating of the coated one deck nickel of ceramic surface, research shows that the wetting angle of aluminium liquid on ceramic plate is about 57 °, and Ni coating has effectively improved the wettability between aluminium and pottery.The Zhao Qing of Aviation Engineering Institutes Of Nanchang etc. adopt the method for chemical nickel plating to form one deck nickel coating on Alumina Foam Ceramics surface, result of study shows that nickel coating has improved the interface binding power of pottery with aluminum substrate, and the wear resistance of aluminium base foamed ceramics matrix material significantly improves.But to Al
2o
3pottery, the activation of Ni coating belongs to non-reactive wetting and can not form reactant, the motivating force of wet processes is only diffusive force and Van der Waals force, and a little less than the combination too of interface, the fusing point of nickel is lower simultaneously, the pottery of coated nickel is with fusing point higher metal during as Fe Long contact time, nickel layer will melt and be diffused in metal, causes nickel layer to destroy, and pottery/nickel layer/metal three-decker is destroyed, become molten metal directly with ceramic layer Surface Contact, nickel layer inefficacy.By contrast, titanium can better improve the wettability between metal and pottery as reactive wetting active metal than non-reactive wetting metals such as nickel.
At present more conventional method for surface metallation has the methods such as ion implantation, plasma spraying, vacuum ionic evaporation, electroless plating.First three methods needs expensive equipment conventionally, complex process, and poor around plating property, cost is high, thereby is difficult to extensive realization; With regard to electroless plating, on pottery, to carry out electroless plating and need to carry out a series of sensitization reactivation process to ceramic surface, stability of solution is poor, safeguard, adjust and regenerate cumbersome, cost is higher, and not relevant research simultaneously shows to adopt the method for electroless plating, obtains single Ti coating.
Summary of the invention
The object of this invention is to provide a kind of technique simple, with low cost prepare the method for titanium metal coating at ceramic surface.
For achieving the above object, the present invention adopts following technical scheme:
First surface-treated pottery is put into silica tube, then the mixture of titanium and iodine powder is placed in container, container is put into silica tube; Again silica tube is put into program control stove, program control stove is vacuumized to logical rare gas element repeatedly, with 15～20 DEG C/min heat-up rate, program control stove is warming up to 1030～1200 DEG C of insulations, after cooling, obtain the pottery of surperficial coated titanium metallic coating, wherein, the mass ratio of titanium and iodine powder is: (1～3): (1～5).
The detailed process of ceramic surface processing is: with 600 order sand paper, pottery is polished repeatedly, obtain surface rubbing, roughness pottery uniformly, then after pottery is placed in to water and repeatedly cleans, carry out ultrasonic cleaning 10～15min with ethanol.
Described titanium is titanium valve or titanium sponge.
Described container is quartz material boat.
Described soaking time is 60min.
Described cooling after, take out and also ceramic surface cleaned repeatedly, then dry.
Described inert atmosphere is argon gas.
With respect to prior art, the beneficial effect that the present invention has is:
The present invention, under protection of inert gas effect, adopts titanium and iodine as precursors, carries out chemical vapour deposition titanium on ceramic matrix, completes deposition process.In deposition process of the present invention, active titanium is good around plating property, can on pottery, obtain the titanium coating that quality is consistent, thereby expanded the method for improving metal, ceramic wettability after deposition.
The present invention improves pottery and intermetallic wettability using titanium as active metal, Ti gets involved ceramic interface ceramic interface performance is changed, and forms TiO and the Ti with metallic character
3(Cu, Al)
3thereby O improves wetting.
The present invention adopts chemical Vapor deposition process to metallize to ceramic surface, adopts the advantage of chemical vapour deposition to be: 1, plated film is good around plating property, and to complex-shaped pottery, as porous ceramics, deep hole on pottery, pore can uniform coateds; 2, coatings purity is high, strong with the bonding force of matrix pottery; 3, nucleation rate is high, and nucleation density is large, in the whole plane of pottery, is evenly distributed, and easily forms level and smooth depositional plane; 4, equipment is simple, cost is lower, simple to operate, and environmental pollution is little, is easy to large-scale production.
Further, the present invention can effectively control the deposition of coating by controlling depositing time.
Brief description of the drawings
Fig. 1 is the ceramic surface Ti metallic coating XRD diffractogram that the present invention makes;
Fig. 2 is the micro-structure diagram of the ceramic surface Ti metallic coating that makes of the present invention.
Embodiment
By accompanying drawing, in conjunction with example, the present invention is described in detail below.
Embodiment 1
Pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, pottery being placed in to water cleans repeatedly again, carry out after ultrasonic cleaning 10min with ethanol again, surface-treated pottery is put into silica tube bottom, then the mixture of titanium valve and iodine powder is placed in quartz material boat, quartz is expected to boat puts into silica tube middle part; Again silica tube is put into program control stove, to the logical argon gas of program control stove evacuation, then repeated to vacuumize the operation of rear logical argon gas, with 15 DEG C/min heat-up rate, program control stove is warming up to 1030 DEG C of insulation 60min, furnace cooling; Take out pottery and repeatedly clean, then dry, obtain the pottery of surperficial coated titanium metallic coating, the coat-thickness obtaining is about 8.2um, and wherein, titanium valve is 3g, and the mass ratio of titanium valve and iodine powder is 1:3.
Embodiment 2
Pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, pottery being placed in to water cleans repeatedly again, carry out after ultrasonic cleaning 15min with ethanol again, surface-treated pottery is put into silica tube bottom, then the mixture of titanium valve and iodine powder is placed in quartz material boat, quartz is expected to boat puts into silica tube middle part; Again silica tube is put into program control stove, to program control stove evacuation logical rare gas element, then repeated to vacuumize the operation of rear logical argon gas, with 15 DEG C/min heat-up rate, program control stove is warming up to 1100 DEG C of insulation 60min, furnace cooling; Take out pottery and repeatedly clean, then dry, obtain the pottery of surperficial coated titanium metallic coating, the coat-thickness obtaining is about 28.9um, and wherein, titanium valve is 3g, and the mass ratio of titanium valve and iodine powder is 1:3.
Embodiment 3
Pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, pottery being placed in to water cleans repeatedly again, carry out after ultrasonic cleaning 15min with ethanol again, surface-treated pottery is put into silica tube bottom, then the mixture of titanium valve and iodine powder is placed in quartz material boat, quartz is expected to boat puts into silica tube middle part; Again silica tube is put into program control stove, to the logical rare gas element of program control stove evacuation, then repeated to vacuumize the operation of rear logical argon gas, with 15 DEG C/min heat-up rate, program control stove is warming up to 1200 DEG C of insulation 60min, furnace cooling; Take out pottery and repeatedly clean, then dry, obtain the pottery of surperficial coated titanium metallic coating, the coat-thickness obtaining is about 29.5um, and wherein, titanium valve is 3g, and the mass ratio of titanium valve and iodine powder is 1:3.
As shown in Figure 1, the microtexture of coating as shown in Figure 2 for the contained essential substance of coating of the present embodiment.Can find out from Fig. 1 and Fig. 2, the ceramic plated film of surperficial coated titanium metallic coating is evenly distributed in whole plane, and purity is high.
Embodiment 4
Pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, pottery being placed in to water cleans repeatedly again, carry out after ultrasonic cleaning 12min with ethanol again, surface-treated pottery is put into silica tube bottom, then the mixture of titanium sponge and iodine powder is placed in quartz material boat, quartz is expected to boat puts into silica tube middle part; Again silica tube is put into program control stove, to the logical rare gas element of program control stove evacuation, then repeated to vacuumize the operation of rear logical argon gas, with 18 DEG C/min heat-up rate, program control stove is warming up to 1080 DEG C of insulation 60min, furnace cooling; Take out pottery and repeatedly clean, then dry, obtain the pottery of surperficial coated titanium metallic coating, wherein, the mass ratio of titanium sponge and iodine powder is 1:1.
Embodiment 5
Pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, pottery being placed in to water cleans repeatedly again, carry out after ultrasonic cleaning 13min with ethanol again, surface-treated pottery is put into silica tube bottom, then the mixture of titanium valve and iodine powder is placed in quartz material boat, quartz is expected to boat puts into silica tube middle part; Again silica tube is put into program control stove, to the logical rare gas element of program control stove evacuation, then repeatedly vacuumized the operation of rear logical argon gas, with 20 DEG C/min heat-up rate, program control stove is warming up to 1150 DEG C of insulation 60min, furnace cooling; Take out pottery and repeatedly clean, then dry, obtain the pottery of surperficial coated titanium metallic coating, wherein, the mass ratio of titanium valve and iodine powder is 1:5.
Embodiment 6
Pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, pottery being placed in to water cleans repeatedly again, carry out after ultrasonic cleaning 14min with ethanol again, surface-treated pottery is put into silica tube bottom, then the mixture of titanium sponge and iodine powder is placed in quartz material boat, quartz is expected to boat puts into silica tube middle part; Again silica tube is put into program control stove, to the logical rare gas element of program control stove evacuation, then repeated to vacuumize the operation of rear logical argon gas, with 16 DEG C/min heat-up rate, program control stove is warming up to 1170 DEG C of insulation 60min, furnace cooling; Take out pottery and repeatedly clean, then dry, obtain the pottery of surperficial coated titanium metallic coating, wherein, the mass ratio of titanium sponge and iodine powder is 3:1.
Embodiment 7
Pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, pottery being placed in to water cleans repeatedly again, carry out after ultrasonic cleaning 10min with ethanol again, surface-treated pottery is put into silica tube bottom, then the mixture of titanium valve and iodine powder is placed in quartz material boat, quartz is expected to boat puts into silica tube middle part; Again silica tube is put into program control stove, to the logical rare gas element of program control stove evacuation, then repeated to vacuumize the operation of rear logical argon gas, with 15 DEG C/min heat-up rate, program control stove is warming up to 1200 DEG C of insulation 60min, furnace cooling; Take out pottery and repeatedly clean, then dry, obtain the pottery of surperficial coated titanium metallic coating, wherein, the mass ratio of titanium valve and iodine powder is 3:5.
Embodiment 8
Pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, pottery being placed in to water cleans repeatedly again, carry out after ultrasonic cleaning 10min with ethanol again, surface-treated pottery is put into silica tube bottom, then the mixture of titanium valve and iodine powder is placed in quartz material boat, quartz is expected to boat puts into silica tube middle part; Again silica tube is put into program control stove, to the logical rare gas element of program control stove evacuation, then repeated to vacuumize the operation of rear logical argon gas, with 15 DEG C/min heat-up rate, program control stove is warming up to 1200 DEG C of insulation 60min, furnace cooling; Take out pottery and repeatedly clean, then dry, obtain the pottery of surperficial coated titanium metallic coating, wherein, the mass ratio of titanium valve and iodine powder is 3:4.
Embodiment 9
Pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, pottery being placed in to water cleans repeatedly again, carry out after ultrasonic cleaning 10min with ethanol again, surface-treated pottery is put into silica tube bottom, then the mixture of titanium valve and iodine powder is placed in quartz material boat, quartz is expected to boat puts into silica tube middle part; Again silica tube is put into program control stove, to the logical rare gas element of program control stove evacuation, then repeated to vacuumize the operation of rear logical argon gas, with 15 DEG C/min heat-up rate, program control stove is warming up to 1200 DEG C of insulation 60min, furnace cooling; Take out pottery and repeatedly clean, then dry, obtain the pottery of surperficial coated titanium metallic coating, wherein, the mass ratio of titanium valve and iodine powder is 2:3.
Claims (7)
1. a method of preparing titanium metal coating at ceramic surface, is characterized in that, first surface-treated pottery is put into silica tube, then the mixture of titanium and iodine powder is placed in container, and container is put into silica tube; Again silica tube is put into program control stove, to program control stove evacuation logical rare gas element, with 15～20 DEG C/min heat-up rate, program control stove is warming up to 1030～1200 DEG C of insulations, after cooling, obtain the pottery of surperficial coated titanium metallic coating, wherein, the mass ratio of titanium and iodine powder is: (1～3): (1～5).
2. a kind of method of preparing titanium metal coating at ceramic surface according to claim 1, it is characterized in that, the detailed process of ceramic surface processing is: pottery is polished repeatedly with 600 order sand paper, obtain surface rubbing, roughness pottery uniformly, after again pottery being placed in to water and repeatedly cleaning, carry out ultrasonic cleaning 10～15min with ethanol, obtain surface-treated pottery.
3. a kind of method of preparing titanium metal coating at ceramic surface according to claim 1, is characterized in that, described titanium is titanium valve or titanium sponge.
4. a kind of method of preparing titanium metal coating at ceramic surface according to claim 1, is characterized in that, described container is quartz material boat.
5. a kind of method of preparing titanium metal coating at ceramic surface according to claim 1, is characterized in that, described soaking time is 60min.
6. a kind of method of preparing titanium metal coating at ceramic surface according to claim 1, is characterized in that, described cooling after, take out and also ceramic surface cleaned repeatedly, then dry.
7. a kind of method of preparing titanium metal coating at ceramic surface according to claim 1, is characterized in that, described inert atmosphere is argon gas.
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| US10150184B2 (en) | 2015-10-21 | 2018-12-11 | Siemens Energy, Inc. | Method of forming a cladding layer having an integral channel |
| CN108516871B (en) * | 2018-04-23 | 2020-12-22 | 哈尔滨工业大学（威海） | Surface metallization method of porous silicon nitride ceramic |
| CN111943725B (en) * | 2020-07-29 | 2022-12-13 | 沈阳中钛装备制造有限公司 | Titanium modified ceramic and preparation method thereof, and ceramic-based metal composite and composite method thereof |
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|---|---|---|---|---|
| CN101353269A (en) * | 2008-07-17 | 2009-01-28 | 西北工业大学 | Preparation of carbon/silicon carbide composite material surface refractory coating |
| CN101602616A (en) * | 2009-07-16 | 2009-12-16 | 中国人民解放军国防科学技术大学 | Metallizing surface of ceramic base composite material member technology based on molten-salt growth method |
| CN102795894A (en) * | 2012-08-09 | 2012-11-28 | 浙江亚通金属陶瓷有限公司 | Surface metallization layer of high-purity alumina ceramics and compounding technology thereof |
| CN103102180A (en) * | 2013-02-22 | 2013-05-15 | 浙江亚通金属陶瓷有限公司 | Metallized surface of zirconia ceramic and preparation method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353269A (en) * | 2008-07-17 | 2009-01-28 | 西北工业大学 | Preparation of carbon/silicon carbide composite material surface refractory coating |
| CN101602616A (en) * | 2009-07-16 | 2009-12-16 | 中国人民解放军国防科学技术大学 | Metallizing surface of ceramic base composite material member technology based on molten-salt growth method |
| CN102795894A (en) * | 2012-08-09 | 2012-11-28 | 浙江亚通金属陶瓷有限公司 | Surface metallization layer of high-purity alumina ceramics and compounding technology thereof |
| CN103102180A (en) * | 2013-02-22 | 2013-05-15 | 浙江亚通金属陶瓷有限公司 | Metallized surface of zirconia ceramic and preparation method |
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