CN105254321A - Ceramic/metal connecting method based on Ni-B/Ti instant liquid phase in-situ reaction - Google Patents
Ceramic/metal connecting method based on Ni-B/Ti instant liquid phase in-situ reaction Download PDFInfo
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- CN105254321A CN105254321A CN201510656797.5A CN201510656797A CN105254321A CN 105254321 A CN105254321 A CN 105254321A CN 201510656797 A CN201510656797 A CN 201510656797A CN 105254321 A CN105254321 A CN 105254321A
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Abstract
The invention provides a ceramic/metal connecting method based on Ni-B/Ti instant liquid phase in-situ reaction and relates to a brazed connection method. The method solves the problems that an existing ceramic/metal connector is low in strength and poor in stability. The ceramic/metal connecting method comprises the following steps that an electroplating or chemical plating method is used for depositing a Ni-B amorphous alloy on the surface of Ni foil to prepare (Ni/Ni-B) composite foil, the (Ni/Ni-B) composite foil and Ti foil with a certain thickness proportion are arranged between metal to be welded and ceramic to form a part to be welded, the part to be welded is placed into a vacuum pressure sintering furnace to be welded, and ceramic/metal connection is finished. According to the method, TiB whisker reinforcement is generated in ceramic/metal weld joints in an in-situ mode, connector stress is effectively relieved, and connector strength is improved; the shearing strength of an obtained connector can reach 92-136 MPa, and the strength of the connector is improved by 43-72%. The method can be used in the field of ceramic/metal brazed connection.
Description
Technical field
The present invention relates to the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ.
Background technology
Pottery has many excellent properties such as density is low, intensity is high, wear-resisting, high temperature resistant, corrosion-resistant, is the very promising structured materials of industrial circle such as military equipment, nuclear power, chemical industry and automobile.But because pottery does not have the dislocation system of slip, its hardness is high, fragility greatly, not easily machine-shaping.In order to address this problem, often pottery is connected with metal in industry, the two is prepared into composite component, to play ceramic and that metal is excellent separately performance.Welding connects ceramic and that metal is the most frequently used method, and it makes materials to be welded form interatomic diffusion and combination by the mode heated or pressurize.Ceramic/metal welding process conventional at present comprises soldering, diffusion welding, self-propagating reaction connection, Transient liquid phase (TLP) diffusion connection, laser/electrons leaves welding etc.But no matter which kind of mode of connection, all needs to consider because of the residual stress problems that the difference of pottery, physics of metals character is brought.In the last few years, investigator improved the performance of joint mainly through the Composition Design and process optimization welding middle layer, and wherein most is representational is exactly composite soldering method.The method for matrix, is mixed into a certain proportion of ceramic particle, refractory metal particulate or staple fibre etc. as second-phase reinforcement with active A g-Cu-Ti solder.Utilize the physical properties in middle layer such as characteristic butt welded seam such as reinforcement self high-modulus, low thermal coefficient of expansion etc. to regulate, reduce the difference of thermal expansion coefficient of weld seam and ceramic interface, and then alleviate the unrelieved stress of heterogenous material joint.Composite soldering method is a kind of simple and practical method, but it also exists some problems in actual applications: first, and the mechanically mixing mode of active solder and wild phase can cause wild phase at the inner skewness of weld seam, easily reunites; Secondly, wild phase and active solder generation complex chemical reaction, easily generate brittle intermetallic thing, butt junction performance is unfavorable; Again, the mobility adding membership reduction active solder of wild phase and wettability, easily produce the defect such as hole, non-seam in weld seam inside.
Summary of the invention
For the weak point that above-mentioned background technology exists, the open ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ of the present invention.
The inventive method adopts two-layer Ti middle layer paillon foil and layer of Ni/Ni-B composite foil to be welding middle layer, 1. two kinds of Ti middle layer foil thickness are respectively titanium foil: 10 μm ~ 50 μm and titanium foil 2.: 50 ~ 150 μm, the thickness of initial Ni middle layer paillon foil is 50 ~ 100 μm, and welding process is carried out according to the following steps:
One, 800#, 1000#, 1200#, 1500# sand papering surface is adopted to metallic matrix, then immerse acetone soln ultrasonic cleaning 5min, dry for subsequent use; 1200# and 1500# diamond disk polishing surface is adopted to ceramic matrix, immerses acetone soln ultrasonic cleaning 5min, dry for subsequent use;
Two, get Ti, Ni middle layer paillon foil, first immersed ultrasonic cleaning 5min in acetone soln, put into oxide film dissolving solution soaking 10 ~ 15min afterwards and carry out oxide film dissolving process, then take out Ti, Ni middle layer paillon foil clear water and rinse well, dry for subsequent use; Described oxide film dissolving solution is the HF, the mass percentage that are 2% ~ 5% by mass percentage is the HNO of 20% ~ 45%
3form with the water of surplus;
Three, get the Ni middle layer paillon foil that thickness is 50 μm ~ 100 μm of step 2 process, immerse ultrasonic cleaning 5min in acetone soln, deposit 1 μm ~ 5 μm thick Ni-B amorphous alloy layer afterwards in paillon foil side, Ni middle layer, obtain Ni/Ni-B composite foil; Then clean water is adopted to Ni/Ni-B composite foil, dry for subsequent use; Wherein, the B content of described Ni-B amorphous alloy layer is 3wt.% ~ 6wt.%;
Four, get Ni/Ni-B composite foil that pottery that step one processes, metal, Ti middle layer paillon foil after step 2 process and step 3 obtain to be assembled into treat weldment to stack mode, assembling sequence is: metal/Ti middle layer paillon foil/Ni/Ni-B composite foil/Ti middle layer paillon foil/pottery; To treat that weldment is placed in Vacuum diffusion bonding furnace, and apply 5 ~ 10MPa pressure, and be evacuated to 5 × 10
-4~ 1 × 10
-3pa, then Vacuum diffusion bonding furnace is warming up to 900 DEG C with the speed of 30 DEG C/min, insulation 5min, 950 ~ 1000 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 5 ~ 30min, be cooled to 300 DEG C with the speed of 5 DEG C/min again, last weldment cools to room temperature with the furnace, completes the described ceramic/metal based on Ni-B/Ti Transient liquid phase reaction in－situ and connects; Wherein, the Ni-B amorphous alloy layer of Ni/Ni-B composite foil is near ceramic side, and the total thickness of two-layer Ti middle layer paillon foil is 1:(1.0 ~ 2.5 with the thickness proportion of the Ni middle layer foil thickness not comprising Ni-B amorphous alloy layer).
The present invention comprises following beneficial effect:
Method And Principle of the present invention: welding middle layer exists Ti/Ni and Ti/Ni-B two kinds of reaction interfaces, when temperature is higher than 942 DEG C, two interfaces produce eutectic Transient liquid phase by Ti-Ni contact reacts.For Ti/Ni-B reaction interface, B atom progressively enters liquid phase equably with the dissolving of Ni, occurs to react as follows with Ti:
Ti+B→TiBΔ
rG＝-163200+5.9TJ/mol
TiB is fine acicular ceramic whisker, has higher modulus and lower thermal expansivity.It effectively can regulate the thermal expansivity of weld seam entirety as reinforcement, reduces joint stress.Because the reaction generating TiB reinforcement produces at welding process situ, doing so avoids the problem of the uneven and easy reunion of reinforcement mixing occurred in composite soldering method, improve joint microstructure and mechanical property.In addition, in the present invention, TiB reaction in－situ only appears in weld seam Transient liquid phase district, because the dissolution rate of reaction in－situ speed and Ni-B layer and Ni-B layer B content are closely related, can be controlled by Joining Technology and Ni-B composition of layer controls fine adjustment TiB and grow.
Test shows, uses method of the present invention to connect GH99 alloy and Al
2o
3pottery, GH99/Ti/ (the Ni/Ni-B)/Ti/Al of preparation
2o
3joint bending stiffness can reach 92 ~ 136MPa, than the GH99/Ti/Ni/Ti/Al not adopting reaction in－situ
2o
3strength of joint improves 43% ~ 72%.
Existing patent (application number: 201010215105. publication numbers: CN101863677A) it is also proposed a kind of method that in-situ self-generated TiB whisker improves strength of ceramic soldered joint.The present invention is from the different of existing patent, and the method that present invention employs plating or electroless plating prepares Ni-B amorphous alloy layer, the boron source using Ni-B amorphous alloy layer as reaction in－situ.TiB can be made to generate position for method of the present invention and generation density is controlled, and then is conducive to improving joint performance.Compared with joint prepared by joint prepared by the present invention and documents, slip resistance improves about 20% ~ 40%.
Accompanying drawing explanation
Fig. 1 is that ceramic/metal of the present invention treats weldment assembling mode schematic diagram.
Embodiment
Embodiment one: the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ of present embodiment, it carries out according to following steps:
One, 800#, 1000#, 1200#, 1500# sand papering surface is adopted to metallic matrix, then immerse acetone soln ultrasonic cleaning 5min, dry for subsequent use; 1200# and 1500# diamond disk polishing surface is adopted to ceramic matrix, immerses acetone soln ultrasonic cleaning 5min, dry for subsequent use;
Two, get Ti, Ni middle layer paillon foil, first immersed ultrasonic cleaning 5min in acetone soln, put into oxide film dissolving solution soaking 10 ~ 15min afterwards and carry out oxide film dissolving process, then take out Ti, Ni middle layer paillon foil clear water and rinse well, dry for subsequent use; Described oxide film dissolving solution is the HF, the mass percentage that are 2% ~ 5% by mass percentage is the HNO of 20% ~ 45%
3form with the water of surplus;
Three, get the Ni middle layer paillon foil that thickness is 50 μm ~ 100 μm of step 2 process, immerse ultrasonic cleaning 5min in acetone soln, deposit 1 μm ~ 5 μm thick Ni-B amorphous alloy layer afterwards in paillon foil side, Ni middle layer, obtain Ni/Ni-B composite foil; Then clean water is adopted to Ni/Ni-B composite foil, dry for subsequent use; Wherein, the B content of described Ni-B amorphous alloy layer is 3wt.% ~ 6wt.%;
Four, get Ni/Ni-B composite foil that pottery that step one processes, metal, Ti middle layer paillon foil after step 2 process and step 3 obtain to be assembled into treat weldment to stack mode, assembling sequence is: metal/Ti middle layer paillon foil/Ni/Ni-B composite foil/Ti middle layer paillon foil/pottery; To treat that weldment is placed in Vacuum diffusion bonding furnace, and apply 5 ~ 10MPa pressure, and be evacuated to 5 × 10
-4~ 1 × 10
-3pa, then Vacuum diffusion bonding furnace is warming up to 900 DEG C with the speed of 30 DEG C/min, insulation 5min, 950 ~ 1000 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 5 ~ 30min, be cooled to 300 DEG C with the speed of 5 DEG C/min again, last weldment cools to room temperature with the furnace, completes the described ceramic/metal based on Ni-B/Ti Transient liquid phase reaction in－situ and connects; Wherein, the Ni-B amorphous alloy layer of Ni/Ni-B composite foil is near ceramic side, and the total thickness of two-layer Ti middle layer paillon foil is 1:(1.0 ~ 2.5 with the thickness proportion of the Ni middle layer foil thickness not comprising Ni-B amorphous alloy layer).
Embodiment two: present embodiment and embodiment one unlike: referring in the surface deposition Ni-B amorphous alloy layer of paillon foil side, Ni middle layer described in step 3 adopts chemical nickel boron alloy method or electronickelling boron alloy method to deposit.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one unlike: the condition of described chemical nickel boron alloy method is: chemical plating solution contains the NiCl6H that concentration is 5g/L
2o, concentration are the NaC of 7g/L
2h
3o
2, concentration is the C of 1g/L
2h
10bN and concentration are the PbCl of 10 ~ 50mg/L
2; Chemical plating solution pH is 4, and chemical plating solution temperature is 59 ~ 81 DEG C, and the electroless plating time is 5 ~ 30min.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one unlike: the condition of described chemical nickel boron alloy method is: chemical plating solution contains the NiCl6H that concentration is 5g/L
2o, concentration are the NaC of 7g/L
2h
3o
2, concentration is the C of 1g/L
2h
10bN and concentration are the PbCl of 10 ~ 50mg/L
2; Chemical plating solution pH is 4, and chemical plating solution temperature is 65 ~ 80 DEG C, and the electroless plating time is 5 ~ 20min.Other is identical with embodiment one.
Embodiment five: present embodiment and embodiment one unlike: the condition of described electronickelling boron alloy method is: electroplating solution contains the NiSO that concentration is 240g/L
46H
2o, concentration are the NiCl6H of 5g/L
2o, concentration are the H of 30g/L
3bO
3be the C of 3g/L with concentration
2h
10bN; Electroplating solution liquid pH is 3.5, and electroplating solution temperature is 44 ~ 46 DEG C, and current density is 0.5 ~ 1.5A/dm
2, electroplating time is 10 ~ 60min.Other is identical with embodiment one.
Embodiment six: present embodiment and embodiment one unlike: the condition of described electronickelling boron alloy method is: electroplating solution contains the NiSO that concentration is 240g/L
46H
2o, concentration are the NiCl6H of 5g/L
2o, concentration are the H of 30g/L
3bO
3be the C of 3g/L with concentration
2h
10bN; Electroplating solution liquid pH is 3.5, and electroplating solution temperature is 45 ~ 46 DEG C, and current density is 0.8 ~ 1.2A/dm
2, electroplating time is 10 ~ 50min.Other is identical with embodiment one.
Embodiment seven: present embodiment and embodiment one are be 2% ~ 4% by mass percentage HF, mass percentage are the HNO of 20% ~ 40% unlike: described oxide film dissolving solution
3form with the water of surplus.Other is identical with embodiment one.
Embodiment eight: present embodiment and embodiment one unlike: the B content of described Ni-B amorphous alloy layer is 3wt.% ~ 5wt.%.Other is identical with embodiment one.
Embodiment nine: present embodiment and embodiment one unlike: the B content of described Ni-B amorphous alloy layer is 4wt.%.Other is identical with embodiment one.
Embodiment ten: present embodiment and embodiment one unlike: will treat in step 4 that weldment is placed in Vacuum diffusion bonding furnace, and apply 5 ~ 10MPa pressure, and be evacuated to 5 × 10
-4~ 1 × 10
-3pa, is then warming up to 900 DEG C by Vacuum diffusion bonding furnace with the speed of 30 DEG C/min, insulation 5min, 980 ~ 1000 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 5 ~ 20min, then be cooled to 300 DEG C with the speed of 5 DEG C/min, last weldment cools to room temperature with the furnace.Other is identical with embodiment one.
Embodiment 11: present embodiment and embodiment one unlike: that assembles in step 4 treats that the Ti middle layer foil thickness near ceramic side in weldment is 50 ~ 150 μm; Ti middle layer foil thickness near metal side is 10 ~ 50 μm.Other is identical with embodiment one.
Embodiment 12: present embodiment and embodiment one unlike: that assembles in step 4 treats that the Ti middle layer foil thickness near ceramic side in weldment is 50 ~ 120 μm; Ti middle layer foil thickness near metal side is 20 ~ 50 μm.Other is identical with embodiment one.
Embodiment 13: present embodiment and embodiment one unlike: that assembles in step 4 treats that the Ti middle layer foil thickness near ceramic side in weldment is 50 ~ 100 μm; Ti middle layer foil thickness near metal side is 30 ~ 50 μm.Other is identical with embodiment one.
Embodiment 14: present embodiment and embodiment one unlike: get the Ni middle layer paillon foil that thickness is 60 μm ~ 100 μm of step 2 process in step 3, immerse ultrasonic cleaning 5min in acetone soln, deposit 1 μm ~ 4 μm thick Ni-B amorphous alloy layer afterwards in paillon foil side, Ni middle layer, obtain Ni/Ni-B composite foil.Other is identical with embodiment one.
Embodiment 15: present embodiment and embodiment one unlike: get the Ni middle layer paillon foil that thickness is 60 μm ~ 80 μm of step 2 process in step 3, immerse ultrasonic cleaning 5min in acetone soln, deposit 1 μm ~ 3 μm thick Ni-B amorphous alloy layer afterwards in paillon foil side, Ni middle layer, obtain Ni/Ni-B composite foil.Other is identical with embodiment one.
Embodiment 16: present embodiment and embodiment one unlike: get the Ni middle layer paillon foil that thickness is 70 μm of step 2 process in step 3, immerse ultrasonic cleaning 5min in acetone soln, deposit 2 μm of thick Ni-B amorphous alloy layer afterwards in paillon foil side, Ni middle layer, obtain Ni/Ni-B composite foil.Other is identical with embodiment one.
Content of the present invention is not limited only to the content of the respective embodiments described above, and the combination of one of them or several embodiment equally also can realize the object of inventing.
Beneficial effect of the present invention is verified by following examples:
Embodiment 1
The ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ of the present embodiment, it carries out according to following steps:
One, wlding material GH99 alloy, Al is treated
2o
3pottery and welding intermediate layer material 50 μm thick Ti paper tinsel, 50 μm of thick Ni paper tinsels carry out surface chemistry cleaning; 800#, 1000#, 1200#, 1500# sand papering surface is adopted to GH99 alloy, then immerses acetone soln ultrasonic cleaning 5min, dry for subsequent use; To Al
2o
3pottery adopts 1200# and 1500# diamond disk polishing surface, immerses acetone soln ultrasonic cleaning 5min, dries for subsequent use;
Two, Ti middle layer paillon foil and Ni middle layer paillon foil is got, first ultrasonic cleaning 5min in acetone soln is immersed, put into oxide film dissolving solution soaking 10 ~ 15min afterwards and carry out oxide film dissolving process, then taking-up Ti middle layer paillon foil and Ni middle layer paillon foil clear water are rinsed well, dry for subsequent use; Described oxide film dissolving solution is the HF, the mass percentage that are 2% ~ 5% by mass percentage is the HNO of 45%
3form with the water of surplus;
Three, the thickness after step 2 process is the Ni middle layer paillon foil of 50 μm, immerses ultrasonic cleaning 5min in acetone soln, deposits 2 μm of thick Ni-B amorphous alloy layer afterwards, obtain Ni/Ni-B composite foil in paillon foil side, Ni middle layer; Then clean water is adopted to Ni/Ni-B composite foil, dry for subsequent use; Wherein, the B content of described Ni-B amorphous alloy layer is 5wt.%;
Four, the Al that step one processes is got
2o
3the Ni/Ni-B composite foil that Ti middle layer paillon foil after pottery, GH99 alloy, step 2 process and step 3 obtain is assembled treat weldment to be stacked mode, and assembling sequence is: GH99/Ti (50 μm)/(Ni/Ni-B)/Ti (50 μm)/Al
2o
3; Wherein, the Ni-B amorphous alloy layer of Ni/Ni-B composite foil is near ceramic side, and the total thickness of two-layer Ti paillon foil and the thickness proportion of Ni middle layer paillon foil (not comprising the thickness of Ni-B amorphous alloy layer) are 1.0:2.0; To treat that weldment is placed in Vacuum diffusion bonding furnace, and apply 5MPa pressure, and be evacuated to 1 × 10
-3pa, then Vacuum diffusion bonding furnace is warming up to 900 DEG C with the speed of 30 DEG C/min, insulation 5min, 980 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 5min, be cooled to 300 DEG C with the speed of 5 DEG C/min again, last weldment cools to room temperature with the furnace, completes the described ceramic/metal based on Ni-B/Ti Transient liquid phase reaction in－situ and connects.
The electroless plating condition of the present embodiment is:
Chemical plating solution contains the NiCl6H that concentration is 5g/L
2o, concentration are the NaC of 7g/L
2h
3o
2, concentration is the C of 1g/L
2h
10bN and concentration are the PbCl of 10 ~ 50mg/L
2; Chemical plating solution pH is 4, and chemical plating solution temperature is 60 DEG C, and the electroless plating time is 10min.
The present embodiment method connects GH99 alloy and Al
2o
3pottery, GH99/Ti/ (the Ni/Ni-B)/Ti/Al of preparation
2o
3joint bending stiffness can reach 92 ~ 128MPa, than the GH99/Ti/Ni/Ti/Al not adopting reaction in－situ
2o
3strength of joint improves 43% ~ 57%.
Embodiment 2
The ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ of the present embodiment, it carries out according to following steps:
One, wlding material GH99 alloy, Al is treated
2o
3pottery and welding intermediate layer material 50 μm thick Ti paper tinsel, 50 μm of thick Ni paper tinsels carry out surface chemistry cleaning; 800#, 1000#, 1200#, 1500# sand papering surface is adopted to GH99 alloy, then immerses acetone soln ultrasonic cleaning 5min, dry for subsequent use; To Al
2o
3pottery adopts 1200# and 1500# diamond disk polishing surface, immerses acetone soln ultrasonic cleaning 5min, dries for subsequent use;
Two, Ti middle layer paillon foil and Ni middle layer paillon foil is got, first ultrasonic cleaning 5min in acetone soln is immersed, put into oxide film dissolving solution soaking 10 ~ 15min afterwards and carry out oxide film dissolving process, then taking-up Ti middle layer paillon foil and Ni middle layer paillon foil clear water are rinsed well, dry for subsequent use; Described oxide film dissolving solution is the HF, the mass percentage that are 2% ~ 5% by mass percentage is the HNO of 45%
3form with the water of surplus;
Three, the thickness after step 2 process is the Ni middle layer paillon foil of 50 μm, immerses ultrasonic cleaning 5min in acetone soln, deposits 3 μm of thick Ni-B amorphous alloy layer afterwards, obtain Ni/Ni-B composite foil in paillon foil side, Ni middle layer; Then clean water is adopted to Ni/Ni-B composite foil, dry for subsequent use; Wherein, the B content of described Ni-B amorphous alloy layer is 5wt.%;
Four, the Al that step one processes is got
2o
3the Ni/Ni-B composite foil that Ti middle layer paillon foil after pottery, GH99 alloy, step 2 process and step 3 obtain is assembled treat weldment to be stacked mode, and assembling sequence is: GH99/Ti (50 μm)/(Ni/Ni-B)/Ti (50 μm)/Al
2o
3; Wherein, the Ni-B amorphous alloy layer of Ni/Ni-B composite foil is near ceramic side, and the total thickness of two-layer Ti paillon foil and the thickness proportion of Ni middle layer paillon foil (not comprising the thickness of Ni-B amorphous alloy layer) are 1.0:2.0; To treat that weldment is placed in Vacuum diffusion bonding furnace, and apply 5MPa pressure, and be evacuated to 1 × 10
- 3pa, then Vacuum diffusion bonding furnace is warming up to 900 DEG C with the speed of 30 DEG C/min, insulation 5min, 980 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 5min, be cooled to 300 DEG C with the speed of 5 DEG C/min again, last weldment cools to room temperature with the furnace, completes the described ceramic/metal based on Ni-B/Ti Transient liquid phase reaction in－situ and connects.
The electrodeposition condition of the present embodiment is: electroplating solution contains the NiSO that concentration is 240g/L
46H
2o, concentration are the NiCl6H of 5g/L
2o, concentration are the H of 30g/L
3bO
3be the C of 3g/L with concentration
2h
10bN; Electroplating solution pH is 3.5, and electroplating solution temperature is 45 DEG C, and current density is 1A/dm
2, electroplating time is 10min.
The present embodiment method connects GH99 alloy and Al
2o
3pottery, GH99/Ti/ (the Ni/Ni-B)/Ti/Al of preparation
2o
3joint bending stiffness can reach 93 ~ 120MPa, than the GH99/Ti/Ni/Ti/Al not adopting reaction in－situ
2o
3strength of joint improves 43% ~ 55%.
Embodiment 3
The ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ of the present embodiment, it carries out according to following steps:
One, wlding material GH99 alloy, Al is treated
2o
3pottery and welding intermediate layer material 20 μm thick Ti paper tinsel, 100 μm of thick Ti paper tinsels, 80 μm of thick Ni paper tinsels carry out surface chemistry cleaning; 800#, 1000#, 1200#, 1500# sand papering surface is adopted to GH99 alloy, then immerses acetone soln ultrasonic cleaning 5min, dry for subsequent use; To Al
2o
3pottery adopts 1200# and 1500# diamond disk polishing surface, immerses acetone soln ultrasonic cleaning 5min, dries for subsequent use;
Two, Ti middle layer paillon foil and Ni middle layer paillon foil is got, first ultrasonic cleaning 5min in acetone soln is immersed, put into oxide film dissolving solution soaking 10 ~ 15min afterwards and carry out oxide film dissolving process, then taking-up Ti middle layer paillon foil and Ni middle layer paillon foil clear water are rinsed well, dry for subsequent use; Described oxide film dissolving solution is the HF, the mass percentage that are 2% ~ 5% by mass percentage is the HNO of 45%
3form with the water of surplus;
Three, the thickness after step 2 process is the Ni middle layer paillon foil of 80 μm, immerses ultrasonic cleaning 5min in acetone soln, deposits 2 μm of thick Ni-B amorphous alloy layer afterwards, obtain Ni/Ni-B composite foil in paillon foil side, Ni middle layer; Then clean water is adopted to Ni/Ni-B composite foil, dry for subsequent use; Wherein, the B content of described Ni-B amorphous alloy layer is 5wt.%;
Four, the Al that step one processes is got
2o
3the Ni/Ni-B composite foil that Ti middle layer paillon foil after pottery, GH99 alloy, step 2 process and step 3 obtain is assembled treat weldment to be stacked mode, and assembling sequence is: GH99/Ti (20 μm)/(Ni/Ni-B)/Ti (100 μm)/Al
2o
3; Wherein, the Ni-B amorphous alloy layer of Ni/Ni-B composite foil is near ceramic side, and the total thickness of two-layer Ti middle layer paillon foil and the thickness proportion of Ni middle layer paillon foil (not comprising the thickness of Ni-B amorphous alloy layer) are 1.0:1.5; To treat that weldment is placed in Vacuum diffusion bonding furnace, and apply 5MPa pressure, and be evacuated to 1 × 10
-3pa, then Vacuum diffusion bonding furnace is warming up to 900 DEG C with the speed of 30 DEG C/min, insulation 5min, 980 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 5min, be cooled to 300 DEG C with the speed of 5 DEG C/min again, last weldment cools to room temperature with the furnace, completes the described ceramic/metal based on Ni-B/Ti Transient liquid phase reaction in－situ and connects.
The electroless plating condition of the present embodiment is:
Chemical plating solution contains the NiCl6H that concentration is 5g/L
2o, concentration are the NaC of 7g/L
2h
3o
2, concentration is the C of 1g/L
2h
10bN and concentration are the PbCl of 10 ~ 50mg/L
2; Chemical plating solution pH is 4, and chemical plating solution temperature is 60 DEG C, and the electroless plating time is 10min.
The present embodiment method connects GH99 alloy and Al
2o
3pottery, GH99/Ti/ (the Ni/Ni-B)/Ti/Al of preparation
2o
3joint bending stiffness can reach 95 ~ 136MPa, than the GH99/Ti/Ni/Ti/Al not adopting reaction in－situ
2o
3strength of joint improves 45% ~ 72%.
Embodiment 4
The ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ of the present embodiment, it carries out according to following steps:
One, wlding material GH99 alloy, Al is treated
2o
3pottery and welding intermediate layer material 20 μm thick Ti paper tinsel, 100 μm of thick Ti paper tinsels, 80 μm of thick Ni paper tinsels carry out surface chemistry cleaning; 800#, 1000#, 1200#, 1500# sand papering surface is adopted to GH99 alloy, then immerses acetone soln ultrasonic cleaning 5min, dry for subsequent use; To Al
2o
3pottery adopts 1200# and 1500# diamond disk polishing surface, immerses acetone soln ultrasonic cleaning 5min, dries for subsequent use;
Two, Ti middle layer paillon foil and Ni middle layer paillon foil is got, first ultrasonic cleaning 5min in acetone soln is immersed, put into oxide film dissolving solution soaking 10 ~ 15min afterwards and carry out oxide film dissolving process, then taking-up Ti middle layer paillon foil and Ni middle layer paillon foil clear water are rinsed well, dry for subsequent use; Described oxide film dissolving solution is the HF, the mass percentage that are 2% ~ 5% by mass percentage is the HNO of 45%
3form with the water of surplus;
Three, the thickness after step 2 process is the Ni middle layer paillon foil of 80 μm, immerses ultrasonic cleaning 5min in acetone soln, deposits 2 μm of thick Ni-B amorphous alloy layer afterwards, obtain Ni/Ni-B composite foil in paillon foil side, Ni middle layer; Then clean water is adopted to Ni/Ni-B composite foil, dry for subsequent use; Wherein, the B content of described Ni-B amorphous alloy layer is 5wt.%;
Four, the Al that step one processes is got
2o
3the Ni/Ni-B composite foil that Ti middle layer paillon foil after pottery, GH99 alloy, step 2 process and step 3 obtain is assembled treat weldment to be stacked mode, and assembling sequence is: GH99/Ti (20 μm)/(Ni/Ni-B)/Ti (100 μm)/Al
2o
3; Wherein, the Ni-B amorphous alloy layer of Ni/Ni-B composite foil is near ceramic side, and the total thickness of two-layer Ti paillon foil and the thickness proportion of Ni middle layer paillon foil (not comprising the thickness of Ni-B amorphous alloy layer) are 1.0:1.5; To treat that weldment is placed in Vacuum diffusion bonding furnace, and apply 5MPa pressure, and be evacuated to 1 × 10
-3pa, then Vacuum diffusion bonding furnace is warming up to 900 DEG C with the speed of 30 DEG C/min, insulation 5min, 1000 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 15min, be cooled to 300 DEG C with the speed of 5 DEG C/min again, last weldment cools to room temperature with the furnace, completes the described ceramic/metal based on Ni-B/Ti Transient liquid phase reaction in－situ and connects.
The electroless plating condition of the present embodiment is:
Chemical plating solution contains the NiCl6H that concentration is 5g/L
2o, concentration are the NaC of 7g/L
2h
3o
2, concentration is the C of 1g/L
2h
10bN and concentration are the PbCl of 10 ~ 50mg/L
2; Chemical plating solution pH is 4, and chemical plating solution temperature is 60 DEG C, and the electroless plating time is 10min.
The present embodiment method connects GH99 alloy and Al
2o
3pottery, GH99/Ti/ (the Ni/Ni-B)/Ti/Al of preparation
2o
3joint bending stiffness can reach 98 ~ 132MPa, than the GH99/Ti/Ni/Ti/Al not adopting reaction in－situ
2o
3strength of joint improves 48% ~ 70%.
Embodiment 5
The ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ of the present embodiment, it carries out according to following steps:
One, treat weldering material metal Nb, SiC ceramic and the thick Ti paper tinsel of welding intermediate layer material 20 μm, 100 μm of thick Ti paper tinsels, 80 μm of thick Ni paper tinsels carry out surface chemistry cleaning; 800#, 1000#, 1200#, 1500# sand papering surface is adopted to metal Nb, then immerses acetone soln ultrasonic cleaning 5min, dry for subsequent use; 1200# and 1500# diamond disk polishing surface is adopted to SiC ceramic, immerses acetone soln ultrasonic cleaning 5min, dry for subsequent use;
Two, Ti middle layer paillon foil and Ni middle layer paillon foil is got, first ultrasonic cleaning 5min in acetone soln is immersed, put into oxide film dissolving solution soaking 10 ~ 15min afterwards and carry out oxide film dissolving process, then taking-up Ti middle layer paillon foil and Ni middle layer paillon foil clear water are rinsed well, dry for subsequent use; Described oxide film dissolving solution is the HF, the mass percentage that are 2% ~ 5% by mass percentage is the HNO of 45%
3form with the water of surplus;
Three, the thickness after step 2 process is the Ni middle layer paillon foil of 80 μm, immerses ultrasonic cleaning 5min in acetone soln, deposits 2 μm of thick Ni-B amorphous alloy layer afterwards, obtain Ni/Ni-B composite foil in paillon foil side, Ni middle layer; Then clean water is adopted to Ni/Ni-B composite foil, dry for subsequent use; Wherein, the B content of described Ni-B amorphous alloy layer is 5wt.%;
Four, get Ni/Ni-B composite foil that SiC ceramic that step one processes, metal Nb, Ti middle layer paillon foil after step 2 process and step 3 obtain to assemble treat weldment to stack mode, assembling sequence is: Nb/Ti (20 μm)/(Ni/Ni-B)/Ti (100 μm)/SiC; Wherein, the Ni-B amorphous alloy layer of Ni/Ni-B composite foil is near ceramic side, and the total thickness of two-layer Ti paillon foil and the thickness proportion of Ni middle layer paillon foil (not comprising the thickness of Ni-B amorphous alloy layer) are 1.0:1.5; To treat that weldment is placed in Vacuum diffusion bonding furnace, and apply 5MPa pressure, and be evacuated to 1 × 10
-3pa, then Vacuum diffusion bonding furnace is warming up to 900 DEG C with the speed of 30 DEG C/min, insulation 5min, 1000 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 15min, be cooled to 300 DEG C with the speed of 5 DEG C/min again, last weldment cools to room temperature with the furnace, completes the described ceramic/metal based on Ni-B/Ti Transient liquid phase reaction in－situ and connects.
The electroless plating condition of the present embodiment is:
Chemical plating solution contains the NiCl6H that concentration is 5g/L
2o, concentration are the NaC of 7g/L
2h
3o
2, concentration is the C of 1g/L
2h
10bN and concentration are the PbCl of 10 ~ 50mg/L
2; Chemical plating solution pH is 4, and chemical plating solution temperature is 60 DEG C, and the electroless plating time is 10min.
The present embodiment method connection metal Nb and SiC ceramic, Nb/Ti/ (the Ni/Ni-B)/Ti/SiC joint bending stiffness of preparation can reach 82 ~ 130MPa, improves 35% ~ 56% than not adopting the Nb/Ti/Ni/Ti/SiC strength of joint of reaction in－situ.
Claims (10)
1., based on the ceramic/metal method of attachment of Ni-B/Ti Transient liquid phase reaction in－situ, it is characterized in that it carries out according to following steps:
One, 800#, 1000#, 1200#, 1500# sand papering surface is adopted to metallic matrix, then immerse acetone soln ultrasonic cleaning 5min, dry for subsequent use; 1200# and 1500# diamond disk polishing surface is adopted to ceramic matrix, immerses acetone soln ultrasonic cleaning 5min, dry for subsequent use;
Two, get Ti, Ni middle layer paillon foil, first immersed ultrasonic cleaning 5min in acetone soln, put into oxide film dissolving solution soaking 10 ~ 15min afterwards and carry out oxide film dissolving process, then take out Ti, Ni middle layer paillon foil clear water and rinse well, dry for subsequent use; Described oxide film dissolving solution is the HF, the mass percentage that are 2% ~ 5% by mass percentage is the HNO of 20% ~ 45%
3form with the water of surplus;
Three, get the Ni middle layer paillon foil that thickness is 50 μm ~ 100 μm of step 2 process, immerse ultrasonic cleaning 5min in acetone soln, deposit 1 μm ~ 5 μm thick Ni-B amorphous alloy layer afterwards in paillon foil side, Ni middle layer, obtain Ni/Ni-B composite foil; Then clean water is adopted to Ni/Ni-B composite foil, dry for subsequent use; Wherein, the B content of described Ni-B amorphous alloy layer is 3wt.% ~ 6wt.%;
Four, get Ni/Ni-B composite foil that pottery that step one processes, metal, Ti middle layer paillon foil after step 2 process and step 3 obtain to be assembled into treat weldment to stack mode, assembling sequence is: metal/Ti middle layer paillon foil/Ni/Ni-B composite foil/Ti middle layer paillon foil/pottery; To treat that weldment is placed in Vacuum diffusion bonding furnace, and apply 5 ~ 10MPa pressure, and be evacuated to 5 × 10
-4~ 1 × 10
-3pa, then Vacuum diffusion bonding furnace is warming up to 900 DEG C with the speed of 30 DEG C/min, insulation 5min, 950 ~ 1000 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 5 ~ 30min, be cooled to 300 DEG C with the speed of 5 DEG C/min again, last weldment cools to room temperature with the furnace, completes the described ceramic/metal based on Ni-B/Ti Transient liquid phase reaction in－situ and connects; Wherein, the Ni-B amorphous alloy layer of Ni/Ni-B composite foil is near ceramic side, and the total thickness of two-layer Ti middle layer paillon foil is 1:(1.0 ~ 2.5 with the thickness proportion of the Ni middle layer foil thickness not comprising Ni-B amorphous alloy layer).
2. the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ according to claim 1, is characterized in that referring in the surface deposition Ni-B amorphous alloy layer of paillon foil side, Ni middle layer described in step 3 adopts chemical nickel boron alloy method or electronickelling boron alloy method to deposit.
3. the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ according to claim 2, is characterized in that the mode of deposition of described chemical nickel boron alloy method is: chemical plating solution contains the NiCl6H that concentration is 5g/L
2o, concentration are the NaC of 7g/L
2h
3o
2, concentration is the C of 1g/L
2h
10bN and concentration are the PbCl of 10 ~ 50mg/L
2; Chemical plating solution pH is 4, and chemical plating solution temperature is 59 ~ 81 DEG C, and the electroless plating time is 5 ~ 30min.
4. the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ according to claim 3, is characterized in that the mode of deposition of described chemical nickel boron alloy method is: chemical plating solution contains the NiCl6H that concentration is 5g/L
2o, concentration are the NaC of 7g/L
2h
3o
2, concentration is the C of 1g/L
2h
10bN and concentration are the PbCl of 10 ~ 50mg/L
2; Chemical plating solution pH is 4, and chemical plating solution temperature is 65 ~ 80 DEG C, and the electroless plating time is 5 ~ 20min.
5. the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ according to claim 2, is characterized in that the mode of deposition of described electronickelling boron alloy method is: electroplating solution contains the NiSO that concentration is 240g/L
46H
2o, concentration are the NiCl6H of 5g/L
2o, concentration are the H of 30g/L
3bO
3be the C of 3g/L with concentration
2h
10bN; Electroplating solution pH is 3.5, and electroplating solution temperature is 44 ~ 46 DEG C, and current density is 0.5 ~ 1.5A/dm
2, electroplating time is 10 ~ 60min.
6. the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ according to claim 5, is characterized in that the mode of deposition of described electronickelling boron alloy method is: electroplating solution contains the NiSO that concentration is 240g/L
46H
2o, concentration are the NiCl6H of 5g/L
2o, concentration are the H of 30g/L
3bO
3be the C of 3g/L with concentration
2h
10bN; Electroplating solution pH is 3.5, and electroplating solution temperature is 45 ~ 46 DEG C, and current density is 0.8 ~ 1.2A/dm
2, electroplating time is 10 ~ 50min.
7. the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ according to claim 1, is characterized in that described oxide film dissolving solution is 2% ~ 4% by mass percentage HF, mass percentage are the HNO of 20% ~ 40%
3form with the water of surplus.
8. the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ according to claim 1, is characterized in that the B content of described Ni-B amorphous alloy layer is 3wt.% ~ 5wt.%.
9. the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ according to claim 1, is characterized in that treating that weldment is placed in Vacuum diffusion bonding furnace in step 4, applies 5 ~ 10MPa pressure, and is evacuated to 5 × 10
-4~ 1 × 10
-3pa, is then warming up to 900 DEG C by Vacuum diffusion bonding furnace with the speed of 30 DEG C/min, insulation 5min, 980 ~ 1000 DEG C are warming up to again with the speed of 10 DEG C/min, insulation 5 ~ 20min, then be cooled to 300 DEG C with the speed of 5 DEG C/min, last weldment cools to room temperature with the furnace.
10. the ceramic/metal method of attachment based on Ni-B/Ti Transient liquid phase reaction in－situ according to claim 1, is characterized in that the Ti middle layer foil thickness treating close ceramic side in weldment of assembling in step 4 is 50 ~ 150 μm; Ti middle layer foil thickness near metal side is 10 ~ 50 μm.
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