CN105174990A - High-temperature-application-based composite active middle layer diffusion bonding method for implementing interstitial carbide or nitride ceramic seamless connection - Google Patents
High-temperature-application-based composite active middle layer diffusion bonding method for implementing interstitial carbide or nitride ceramic seamless connection Download PDFInfo
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Abstract
The invention relates to a high-temperature-application-based composite active middle layer diffusion bonding method for implementing interstitial carbide or nitride ceramic seamless connection, which aims to solve the problem that a single-layer active metal middle layer can not form a homogeneous miscible connector. The method comprises the following steps: 1. surface cleaning; 2. active metal layer presetting; and 3. vacuum diffusion bonding. When the Ti/Zr/Ti composite active metal is used as a middle layer to connect the ZrC ceramic, the connector structure only contains ZrC and TiC solid solutions under the connection conditions of 1400 DEG C/1 hour/20 MPa, and the shear strength of the connector is 240 MPa; and compared with the connector obtained from the single-layer active metal middle layer, the strength of the connector obtained by the method provided by the invention is enhanced by 26%. Compared with the traditional method, the strength of the connector is enhanced by nearly 2.5 times. The method is applicable to the field of braze welding.
Description
Technical field
The present invention relates to a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application.
Background technology
Transition metal carbides or nitride ceramics MCx or MNx (TiC, ZrC, with HfC etc. or TiN, Zr3N4 etc.) there is fusing point high (almost all more than 3000 DEG C), hardness is large, thermal expansivity is low and wear-resisting and corrosion resistance and good etc. is excellent performance, be considered to the stupalith that (as supersonic vehicle, rocket engine of future generation and air cooling rapid reaction heap etc.) most is promising under ultra-high temperature condition.But these superhigh temperature ceramics parts need self to couple together with metal or they in actual applications usually, so connecting is requisite link in these superhigh temperature ceramics component processing manufacturing processedes.At welding field, concerning general pottery, basic requirement obtains the joint with good mechanical properties.But for superhigh temperature ceramics component, except this basic demand, due to the Working environment of their harshness, the resistance toheat of also butt junction has higher requirement.So, how to obtain there is good mechanical properties and the joint of resistance to elevated temperatures be superhigh temperature ceramics connect Focal point and difficult point.But, for ultrahigh-temperature interstitial carbon compound or nitride ceramics, existing method of attachment, as soldering, diffusion welding, liquid diffusion bonding etc., the temperature resistance problem that all can not solve joint well and the residual stress problems caused because of the existence of heterogeneous phase.In order to solve this two problems, in the patent (application number CN201310227145.0) that applicant has delivered, put forward a kind of based on the interstitial carbon compound of high temperature application or the active diffusion connection method of nitride ceramics, with monolayer active metal for middle layer, be devoted to formation and remain and the uniform jointing close with matrix constituent without metallographic phase.But the method is for the less ultrahigh-temperature interstitial carbon compound of vacant content or nitride ceramics (as ZrC), during with monolayer active metal Ti for middle layer, in actual connection procedure, be difficult to form homogeneous diffusion joint, the full ceramic joint of two-phase coexistent can only be formed in interface.This caused because newborn carbide can not be solid-solution in mother metal completely under condition of contact (connecting temperature lower than 1400 DEG C), this is main relevant with the miscibility gap between two-phase, makes the time required for formation homogeneous joint, temperature and pressure very harsh.
Summary of the invention
The present invention will solve the problem that monolayer active metal intermediate layer cannot form the homogeneous joint that dissolves each other, and provides a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application.
A kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application of the present invention, carries out according to the following steps:
One, removing surface: adopt the diamond disk of two kinds in 500# ~ 1500# or wherein two or more model to polish step by step to two ceramic mother metals to be connected, refine step by step with the silicon carbide paper of two in 1500# ~ 2000# kind or wherein two or more model again, after finally polishing being carried out to the ceramic mother metal that two after fine grinding are to be connected, be placed in acetone, ultrasonic cleaning 15min ~ 30min, then dehydrated alcohol is placed in, ultrasonic cleaning 10min ~ 15min, finally be placed in loft drier and dry, namely obtain the ceramic mother metal after two removing surfaces; Wherein said ceramic mother metal is MCx one-component ceramic, MNx one-component ceramic, MNx/MNx complex phase ceramic, MCx/MCx complex phase ceramic or MNx/MCx complex phase ceramic;
Two, preset reactive metal layer: the ceramic mother metal surface pre-set thickness after two removing surfaces adopting the mode of magnetron sputtering technique or electronics evaporation to obtain in step one is the reactive metal layer A of 2 ~ 10 μm, obtain the ceramic mother metal that two have reactive metal layer, then in the reactive metal layer of two ceramic mother metals, secondary magnetron sputtering or electronics evaporation is carried out, pre-set thickness is the reactive metal layer B of 5 ~ 20 μm, obtain the ceramic mother metal that two have double-layer active metal level, to obtain two, there is the ceramic mother metal cleaning coating surface 5min ~ 10min of double-layer active metal level with acetone and dehydrated alcohol successively, two samples to be connected are obtained after drying up, active metal in wherein said reactive metal layer A and B is Ti, Zr, Hf, V, Nb or Ta, and the active metal in reactive metal layer A and B is two kinds of metals,
Three, diffusion in vacuum connects: the interface to be connected with reactive metal layer of two samples to be connected step 2 obtained stacks up, and is placed in diffusion in vacuum stove, Bonding pressure be 15MPa ~ 25MPa, vacuum tightness is 0.8 × 10
-3pa ~ 1.3 × 10
-4under the condition of Pa, with the heating rate of 5 ~ 10 DEG C/min to 700 DEG C, then 10 ~ 180min is incubated, then be warming up to the speed of 5 ~ 10 DEG C/min and connect temperature 1300 ~ 1400 DEG C, after insulation 10 ~ 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.
The present invention realizes the formation of homogeneous solid solution joint at identical connection temperature, solves the problem of limited solid solution between carbide in the joint of individual layer middle layer or nitride well.For interstitial carbon compound or nitride ceramics, especially for containing vacant less interstitial carbon compound or nitride ceramics, by reacting in introducing compound transition active metal middle layer, ceramic joining interface and mother metal, in the applied at elevated temperature of ceramic joint, because the active reaction of composite interlayer in connection procedure forms high-melting-point carbide or nitride, remain without metallographic phase, therefore can realize the object improving joint use temperature; In the unrelieved stress of jointing, by reducing and the carbide of the limited solid solution of mother metal or the formation volume of nitride, increase and the carbide of the complete solid solution of mother metal or the formation volume of nitride, make newborn carbide or can phase mutual diffusion and complete solid solution between nitride with mother metal matrix, realize real seamless link, compare with individual layer transition metal layer, xenogenesis joint thermal stresses can be alleviated further and improve the intensity of joint; In addition, the present invention adopts composite reactive metal as middle layer, because the diffusion between metal and metal will faster than metal to the diffusion between pottery, so, the rapid diffusion between composite reactive metal intermediate layer, and the monolayer active metallographic phase ratio of same thickness, add the diffusibility of surface reaction, make to connect temperature and significantly reduce 500-800 DEG C, improve efficiency, save the energy.In sum, compared with traditional ceramics method of attachment, the invention solves the problems such as ceramic joining center tap unrelieved stress is large, intensity is low, resistance toheat is not enough, connection temperature is high, can under lower temperature conditions, realize containing vacant less interstitial carbon compound or the low-stress of nitride ceramics, high temperature resistant, highly reliable, high efficiency connection; Compared with being the active diffusion connection method in middle layer with employing monolayer active metal, the present invention is while its all advantages of succession, achieve the seamless link containing vacant less interstitial carbon compound or nitride ceramics, fully alleviate joint unrelieved stress further, improve strength of joint.
When the present invention adopts Ti/Zr/Ti composite reactive metal to be middle layer to connect ZrC pottery, under identical condition of contact 1400 DEG C/1h/20MPa, joint microstructure only has the sosoloid (Zr of ZrC and TiC, Ti) Cx, obtains homogeneous solid solution joint, and the seamless activity diffusion achieving the less ZrC pottery of the vacant content of carbon connects, under this condition, shearing strength of joint is 240MPa, and strength of parent (237MPa) is suitable, and fracture occurs on mother metal.The joint obtained with monolayer active metal intermediate layer is compared, and strength of joint improves 26%; Compared with traditional ceramics method of attachment, strength of joint improves nearly 2.5 times.
Accompanying drawing explanation
Fig. 1 is the tissue topography of the ZrC joint of comparative example in embodiment one;
Fig. 2 is the tissue topography of the ZrC joint of embodiment one.
Embodiment
Embodiment one: a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application of present embodiment, carry out according to the following steps:
One, removing surface: adopt the diamond disk of two kinds in 500# ~ 1500# or wherein two or more model to polish step by step to two ceramic mother metals to be connected, refine step by step with the silicon carbide paper of two in 1500# ~ 2000# kind or wherein two or more model again, after finally polishing being carried out to the ceramic mother metal that two after fine grinding are to be connected, be placed in acetone, ultrasonic cleaning 15min ~ 30min, then dehydrated alcohol is placed in, ultrasonic cleaning 10min ~ 15min, finally be placed in loft drier and dry, namely obtain the ceramic mother metal after two removing surfaces; Wherein said ceramic mother metal is MCx one-component ceramic, MNx one-component ceramic, MNx/MNx complex phase ceramic, MCx/MCx complex phase ceramic or MNx/MCx complex phase ceramic;
Two, preset reactive metal layer: the ceramic mother metal surface pre-set thickness after two removing surfaces adopting the mode of magnetron sputtering technique or electronics evaporation to obtain in step one is the reactive metal layer A of 2 ~ 10 μm, obtain the ceramic mother metal that two have reactive metal layer, then in the reactive metal layer of two ceramic mother metals, secondary magnetron sputtering or electronics evaporation is carried out, pre-set thickness is the reactive metal layer B of 5 ~ 20 μm, obtain the ceramic mother metal that two have double-layer active metal level, to obtain two, there is the ceramic mother metal cleaning coating surface 5min ~ 10min of double-layer active metal level with acetone and dehydrated alcohol successively, two samples to be connected are obtained after drying up, active metal in wherein said reactive metal layer A and B is Ti, Zr, Hf, V, Nb or Ta, and the active metal in reactive metal layer A and B is two kinds of metals,
Three, diffusion in vacuum connects: the interface to be connected with reactive metal layer of two samples to be connected step 2 obtained stacks up, and is placed in diffusion in vacuum stove, Bonding pressure be 15MPa ~ 25MPa, vacuum tightness is 0.8 × 10
-3pa ~ 1.3 × 10
-4under the condition of Pa, with the heating rate of 5 ~ 10 DEG C/min to 700 DEG C, then 10 ~ 180min is incubated, then be warming up to the speed of 5 ~ 10 DEG C/min and connect temperature 1300 ~ 1400 DEG C, after insulation 10 ~ 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.
Present embodiment is for interstitial carbon compound or nitride ceramics, especially for containing vacant less interstitial carbon compound or nitride ceramics, by reacting in introducing compound transition active metal middle layer, ceramic joining interface and mother metal, in the applied at elevated temperature of ceramic joint, because the active reaction of composite interlayer in connection procedure forms high-melting-point carbide or nitride, remain without metallographic phase, therefore can realize the object improving joint use temperature; In the unrelieved stress of jointing, by reducing and the carbide of the limited solid solution of mother metal or the formation volume of nitride, increase and the carbide of the complete solid solution of mother metal or the formation volume of nitride, make newborn carbide or can phase mutual diffusion and complete solid solution between nitride with mother metal matrix, realize real seamless link, compare with individual layer transition metal layer, xenogenesis joint thermal stresses can be alleviated further and improve the intensity of joint; In addition, the present invention adopts composite reactive metal as middle layer, because the diffusion between metal and metal will faster than metal to the diffusion between pottery, so, the rapid diffusion between composite reactive metal intermediate layer, and the monolayer active metallographic phase ratio of same thickness, add the diffusibility of surface reaction, make to connect temperature and significantly reduce 500-800 DEG C, improve efficiency, save the energy.In sum, compared with traditional ceramics method of attachment, the invention solves the problems such as ceramic joining center tap unrelieved stress is large, intensity is low, resistance toheat is not enough, connection temperature is high, can under lower temperature conditions, realize containing vacant less interstitial carbon compound or the low-stress of nitride ceramics, high temperature resistant, highly reliable, high efficiency connection; Compared with being the active diffusion connection method in middle layer with employing monolayer active metal, the present invention is while its all advantages of succession, achieve the seamless link containing vacant less interstitial carbon compound or nitride ceramics, fully alleviate joint unrelieved stress further, improve strength of joint.
Present embodiment adopt Ti/Zr/Ti composite reactive metal be middle layer to connect ZrC pottery time, under identical condition of contact 1400 DEG C/1h/20MPa, joint microstructure only has the sosoloid (Zr of ZrC and TiC, Ti) Cx, obtains homogeneous solid solution joint, and the seamless activity diffusion achieving the less ZrC pottery of the vacant content of carbon connects, under this condition, shearing strength of joint is 240MPa, and strength of parent (237MPa) is suitable, and fracture occurs on mother metal.The joint obtained with monolayer active metal intermediate layer is compared, and strength of joint improves 26%; Compared with traditional ceramics method of attachment, strength of joint improves nearly 2.5 times.
Embodiment two: present embodiment and embodiment one unlike: the M in the MCx one-component ceramic described in step one is Ti, Zr, Hf, V, Nb or Ta, and x is: 0.55≤x≤1; M in MNx one-component ceramic described in step one is Ti, Zr, Hf, V, Nb or Ta, and x is: 0.55≤x≤1; M in MNx/MNx complex phase ceramic described in step one is Ti, Zr, Hf, V, Nb or Ta, and x is: 0.55≤x≤1; M in MCx/MCx complex phase ceramic described in step one is Ti, Zr, Hf, V, Nb or Ta, and x is 0.55≤x≤1; In MNx/MCx complex phase ceramic described in step one, the M in MNx is Ti, Zr, Hf, V, Nb or Ta, and x is: 0.55≤x≤1, and the M in MCx is Ti, Zr, Hf, V, Nb or Ta, and x is: 0.55≤x≤1.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: the silicon carbide paper described in step one is silicon carbide silicon carbide paper or aluminum oxide silicon carbide paper.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: the ultrasonic frequency described in step one is 88Hz.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: the oven dry described in step one refers to dry 10h at 60 DEG C.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: if the thickness of reactive metal layer A and reactive metal layer B is greater than 10 μm, the then operation of replacement step two or the operation according to step 2 in the steps below: to be the active metal paillon foil A of 10 ~ 30 μm and thickness by thickness the be active metal paillon foil B of 10 ~ 30 μm, with the hydrofluoric acid aqueous solution ultrasonic cleaning 1min that mass concentration is 5%, use washes of absolute alcohol 10min again, dry up rear stand-by; The size of wherein said active metal paillon foil A and active metal paillon foil B is greater than ceramic mother metal to be connected; Active metal in reactive metal layer A and B is Ti, Zr, Hf, V, Nb or Ta, and the active metal in reactive metal layer A and B is two kinds of metals.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: if the thickness of reactive metal layer A and reactive metal layer B is greater than 10 μm, the then operation of replacement step three or the operation according to step 3 in the steps below: in the middle of two samples to be connected that tinsel A and B step 2 obtained obtains in step one according to the laminated structure of A/B/A, the sample assembled is placed in diffusion in vacuum stove, Bonding pressure be 15MPa ~ 25MPa, vacuum tightness is 0.8 × 10
-3pa ~ 1.3 × 10
-4under the condition of Pa, with the heating rate of 5 ~ 10 DEG C/min to 700 DEG C, then 10 ~ 180min is incubated, then be warming up to the speed of 5 ~ 10 DEG C/min and connect temperature 1300 ~ 1400 DEG C, after insulation 10 ~ 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.Other is identical with one of embodiment one to six.If the operation of step 2 adopts active metal paillon foil, then present embodiment also adopts active metal paillon foil to connect.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: the magnetron sputtering technique specific operation process described in step 2 is as follows: put into by material to be sputtered in magnetron sputtering equipment vacuum oven, start to vacuumize, when vacuum tightness reaches 5.6E after aiming at sputtering source
-6during mbar, employing ion beam bombardment treats sputter material successively and equipment sputtering target cleans, and subsequently, under the condition of plasma body, start sputtering, sputter rate is 2nm/65s.Other is identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: the described electronics evaporation specific operation process described in step 2 is as follows: check the air-conditioning system of decontamination chamber and the humidity of instrument room, confirm normally, instrumentation master menu selects auto-programming, put deposition material into steaming and cross stove, after the ceramic mother metal had two after two removing surfaces that the ceramic mother metal of reactive metal layer or step one obtain puts into vacuum chamber, start to vacuumize, reach 1 × 10
-4after the vacuum tightness of Pa, unlocking electronic bundle high-voltage power supply, run the program write, until program end of run, plated film completes, and namely completes.Other is identical with one of embodiment one to eight.
The following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1: a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application of the present embodiment, carry out according to the following steps:
One, removing surface: first adopt in 500#, 800#, 1000# and 1500# and two ZrC pottery mother metals to be connected are polished step by step, refine step by step with the silicon carbide paper of 1500# and 2000# again, after finally polishing being carried out to the ZrC pottery mother metal that two after fine grinding are to be connected, be placed in acetone, again through frequency be the ultrasonic cleaning 30min of 88Hz, then dehydrated alcohol is placed in, ultrasonic cleaning 10min, finally be placed in loft drier, dry 10h at 60 DEG C, namely obtains the pottery of the ZrC after two removing surfaces mother metal;
Two, preset reactive metal layer: the ZrC pottery mother metal surface pre-set thickness after two removing surfaces adopting magnetron sputtering technique to obtain in step one is the Ti layer of 5 μm, obtain the ZrC pottery mother metal that two have Ti layer, then on the Ti layer of two ZrC pottery mother metals, secondary magnetron sputtering is carried out, pre-set thickness is the Zr layer of 10 μm, obtain the ZrC pottery mother metal that two have double-deck Ti layer, to obtain two, there is the ZrC pottery mother metal cleaning coating surface 5min of double-layer active metal level with acetone and dehydrated alcohol successively, after drying up, obtain two samples to be connected;
Three, diffusion in vacuum connects: the interface to be connected with Ti/Zr layer of two samples to be connected step 2 obtained stacks up, and is placed in diffusion in vacuum stove, Bonding pressure be 20MPa, vacuum tightness is 1.3 × 10
-4the condition of Pa, with the heating rate of 10 DEG C/min to 700 DEG C, then 20min is incubated, then be warming up to the speed of 5 DEG C/min and connect temperature 1400 DEG C, after the insulation 60min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards.
The preparation method of comparative example is: one, removing surface: first adopt in 500#, 800#, 1000# and 1500# and polish step by step to two ZrC pottery mother metals to be connected, refine step by step with the silicon carbide paper of 1500# and 2000# again, after finally polishing being carried out to the ZrC pottery mother metal that two after fine grinding are to be connected, be placed in acetone, again through frequency be the ultrasonic cleaning 30min of 88Hz, then dehydrated alcohol is placed in, ultrasonic cleaning 10min, finally be placed in loft drier, dry 10h at 60 DEG C, namely obtains the pottery of the ZrC after two removing surfaces mother metal;
Two, preset reactive metal layer: the ZrC pottery mother metal surface pre-set thickness after two removing surfaces adopting magnetron sputtering technique to obtain in step one is the Ti layer of 5 μm, obtain the ZrC pottery mother metal that two have Ti layer, then to obtain two, there is the ZrC pottery mother metal cleaning coating surface 5min of Ti layer with acetone and dehydrated alcohol successively, after drying up, obtain two samples to be connected;
Three, diffusion in vacuum connects: the interface to be connected with reactive metal layer of two samples to be connected step 2 obtained stacks up, and is placed in diffusion in vacuum stove, Bonding pressure be 20MPa, vacuum tightness is 1.3 × 10
-4the condition of Pa, with the heating rate of 10 DEG C/min to 700 DEG C, then 20min is incubated, then be warming up to the speed of 5 DEG C/min and connect temperature 1400 DEG C, after the insulation 60min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards.
In the present embodiment and comparative example's step 2, magnetron sputtering technique specific operation process is as follows: put into by material to be sputtered in magnetron sputtering equipment vacuum oven, starts to vacuumize, when vacuum tightness reaches 5.6E after aiming at sputtering source
-6during mbar, employing ion beam bombardment treats sputter material successively and equipment sputtering target cleans, and subsequently, under the condition of plasma body, start sputtering, sputter rate is 2nm/65s, namely completes; Material to be sputtered is the ceramic mother metal after two removing surfaces obtaining of two ceramic mother metals with reactive metal layer or step one.
The method of the present embodiment and the method for comparative example are contrasted, when adopting monolayer active metal Ti to be middle layer to weld the vacant less ZrC pottery of carbon, under the condition of 1400 DEG C/1h/20MPa, the final tissue of joint is ZrC (Ti)+TiC, be difficult to form homogeneous solid solution joint, as shown in Figure 1, shearing strength of joint is 190MPa, and fracture occurs in TiC layer; And when adopt Ti/Zr/Ti composite reactive metal be middle layer to connect ZrC pottery time, under identical condition of contact 1400 DEG C/1h/20MPa, joint microstructure only has sosoloid (Zr, the Ti) Cx of ZrC and TiC, obtains homogeneous solid solution joint, as shown in Figure 2, the seamless activity diffusion achieving the less ZrC pottery of the vacant content of carbon connects, and under this condition, shearing strength of joint is 240MPa, suitable with strength of parent (237MPa), fracture occurs on mother metal.The joint obtained with monolayer active metal intermediate layer is compared, and strength of joint improves 26%; Compared with traditional ceramics method of attachment, strength of joint improves nearly 2.5 times.
Embodiment 2: a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application of the present embodiment, carry out according to the following steps:
One, removing surface: first adopt ZrC to be connected to two in 500#, 800#, 1000# and 1500#
0.95pottery mother metal is polished step by step, then refines step by step with the silicon carbide paper of 1500# and 2000#, finally to the ZrC that two after fine grinding are to be connected
0.95after pottery mother metal carries out polishing, be placed in acetone, then be the ultrasonic cleaning 30min of 88Hz through frequency, be then placed in dehydrated alcohol, ultrasonic cleaning 10min, be finally placed in loft drier, dry 10h at 60 DEG C, namely obtains the ZrC after two removing surfaces
0.95pottery mother metal;
Two, preset reactive metal layer: the ZrC after two removing surfaces adopting magnetron sputtering technique to obtain in step one
0.95pottery mother metal surface pre-set thickness is the Ti layer of 5 μm, obtains the ZrC that two have Ti layer
0.95pottery mother metal, then at two ZrC
0.95the Ti layer of pottery mother metal carries out secondary magnetron sputtering, and pre-set thickness is the Zr layer of 5 μm, obtains the ZrC that two have double-layer active metal level
0.95pottery mother metal, has the ZrC of double-layer active metal level with acetone and dehydrated alcohol to obtain two successively
0.95pottery mother metal cleaning coating surface 5min, obtains two samples to be connected after drying up;
Three, diffusion in vacuum connects: the interface to be connected with Ti/Zr layer of two samples to be connected step 2 obtained stacks up, and is placed in diffusion in vacuum stove, Bonding pressure be 20MPa, vacuum tightness is 1.3 × 10
-4the condition of Pa, with the heating rate of 10 DEG C/min to 700 DEG C, then 20min is incubated, then be warming up to the speed of 5 DEG C/min and connect temperature 1300 DEG C, after the insulation 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.
In the present embodiment, magnetron sputtering technique specific operation process is as follows: put into by material to be sputtered in magnetron sputtering equipment vacuum oven, starts to vacuumize, when vacuum tightness reaches 5.6E after aiming at sputtering source
-6during mbar, employing ion beam bombardment treats sputter material successively and equipment sputtering target cleans, and subsequently, under the condition of plasma body, start sputtering, sputter rate is 2nm/65s; Material to be sputtered is the ceramic mother metal after two removing surfaces obtaining of two ceramic mother metals with reactive metal layer or step one.
The shearing resistance of the joint that the present embodiment connects is 244MPa.
Embodiment 3: a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application of the present embodiment, carry out according to the following steps:
One, removing surface: first adopt ZrC to be connected to two in 500#, 800#, 1000# and 1500#
0.85pottery mother metal is polished step by step, then refines step by step with the silicon carbide paper of 1500# and 2000#, finally to the ZrC that two after fine grinding are to be connected
0.85after pottery mother metal carries out polishing, be placed in acetone, then be the ultrasonic cleaning 30min of 88Hz through frequency, be then placed in dehydrated alcohol, ultrasonic cleaning 10min, be finally placed in loft drier, dry 10h at 60 DEG C, namely obtains the ZrC after two removing surfaces
0.85pottery mother metal;
Two, preset reactive metal layer: the ZrC after two removing surfaces adopting magnetron sputtering technique to obtain in step one
0.85pottery mother metal surface pre-set thickness is the Hf layer of 5 μm, obtains the ZrC that two have Hf layer
0.85pottery mother metal, then at two ZrC
0.85the Hf layer of pottery mother metal carries out secondary magnetron sputtering, and pre-set thickness is the Zr layer of 5 μm, obtains the ZrC that two have double-deck Hf/Zr reactive metal layer
0.85pottery mother metal, has the ZrC of double-deck Hf/Zr reactive metal layer with acetone and dehydrated alcohol to obtain two successively
0.85pottery mother metal cleaning coating surface 5min, obtains two samples to be connected after drying up;
Three, diffusion in vacuum connects: the interface to be connected with Hf/Zr layer of two samples to be connected step 2 obtained stacks up, and is placed in diffusion in vacuum stove, Bonding pressure be 20MPa, vacuum tightness is 1.3 × 10
-4the condition of Pa, with the heating rate of 10 DEG C/min to 700 DEG C, then 20min is incubated, then be warming up to the speed of 5 DEG C/min and connect temperature 1300 DEG C, after the insulation 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.
In the present embodiment, magnetron sputtering technique specific operation process is as follows: put into by material to be sputtered in magnetron sputtering equipment vacuum oven, starts to vacuumize, when vacuum tightness reaches 5.6E after aiming at sputtering source
-6during mbar, employing ion beam bombardment treats sputter material successively and equipment sputtering target cleans, and subsequently, under the condition of plasma body, start sputtering, sputter rate is 2nm/65s; Material to be sputtered is the ceramic mother metal after two removing surfaces obtaining of two ceramic mother metals with reactive metal layer or step one.
The shearing resistance of the joint that the present embodiment connects is 231MPa.
Embodiment 4: a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application of the present embodiment, carry out according to the following steps:
One, removing surface: first adopt ZrC to be connected to two in 500#, 800#, 1000# and 1500#
0.95pottery mother metal is polished step by step, then refines step by step with the silicon carbide paper of 1500# and 2000#, finally to the ZrC that two after fine grinding are to be connected
0.95after pottery mother metal carries out polishing, be placed in acetone, then be the ultrasonic cleaning 30min of 88Hz through frequency, be then placed in dehydrated alcohol, ultrasonic cleaning 10min, be finally placed in loft drier, dry 10h at 60 DEG C, namely obtains the ZrC after two removing surfaces
0.95pottery mother metal;
Two, preset reactive metal layer: the preset a layer thickness in ceramic mother metal surface after two removing surfaces adopting magnetron sputtering technique to obtain in step one is the Ti layer of 10 μm, obtains the ceramic mother metal that two have Ti layer; Second layer active metal selects thickness to be the Zr paillon foil of 30 μm, is the hydrofluoric acid aqueous solution ultrasonic cleaning 1min of 5%, then uses washes of absolute alcohol 10min, dry up rear stand-by by Zr paillon foil mass concentration;
Three, diffusion in vacuum connects: two that step 2 are obtained sample to be connected and Zr paillon foils with Ti layer, get up according to the laminated structure of " sample to be connected/Zr paper tinsel/sample to be connected ", be placed in diffusion in vacuum stove, Bonding pressure be 20MPa, vacuum tightness is 1.3 × 10
-4the condition of Pa, with the heating rate of 10 DEG C/min to 700 DEG C, then 20min is incubated, then be warming up to the speed of 5 DEG C/min and connect temperature 1300 DEG C, after the insulation 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.
In the present embodiment, magnetron sputtering technique specific operation process is as follows: put into by material to be sputtered in magnetron sputtering equipment vacuum oven, starts to vacuumize, when vacuum tightness reaches 5.6E after aiming at sputtering source
-6during mbar, employing ion beam bombardment treats sputter material successively and equipment sputtering target cleans, and subsequently, under the condition of plasma body, start sputtering, sputter rate is 2nm/65s; Material to be sputtered is the ceramic mother metal after two removing surfaces obtaining of two ceramic mother metals with reactive metal layer or step one.
The shearing resistance of the joint that the present embodiment connects is 240MPa.
Embodiment 5: a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application of the present embodiment, carry out according to the following steps:
One, removing surface: first adopt HfN to be connected to two in 500#, 800#, 1000# and 1500#
0.95pottery mother metal is polished step by step, then refines step by step with the silicon carbide paper of 1500# and 2000#, finally to the HfN that two after fine grinding are to be connected
0.95after pottery mother metal carries out polishing, be placed in acetone, then be the ultrasonic cleaning 30min of 88Hz through frequency, be then placed in dehydrated alcohol, ultrasonic cleaning 10min, be finally placed in loft drier, dry 10h at 60 DEG C, namely obtains the HfN after two removing surfaces
0.95pottery mother metal;
Two, preset reactive metal layer: the HfN after two removing surfaces adopting magnetron sputtering technique to obtain in step one
0.95pottery mother metal surface pre-set thickness is the Ti layer of 5 μm, obtains the HfN that two have Ti layer
0.95pottery mother metal, then at two HfN
0.95the Ti layer of pottery mother metal carries out secondary magnetron sputtering, and pre-set thickness is the Zr layer of 5 μm, obtains the HfN that two have double-layer active metal level
0.95pottery mother metal, has the HfN of double-layer active metal level with acetone and dehydrated alcohol to obtain two successively
0.95pottery mother metal cleaning coating surface 5min, obtains two samples to be connected after drying up;
Three, diffusion in vacuum connects: the interface to be connected with Ti/Zr layer of two samples to be connected step 2 obtained stacks up, and is placed in diffusion in vacuum stove, Bonding pressure be 20MPa, vacuum tightness is 1.3 × 10
-4the condition of Pa, with the heating rate of 10 DEG C/min to 700 DEG C, then 20min is incubated, then be warming up to the speed of 5 DEG C/min and connect temperature 1300 DEG C, after the insulation 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.
In the present embodiment, magnetron sputtering technique specific operation process is as follows: put into by material to be sputtered in magnetron sputtering equipment vacuum oven, starts to vacuumize, when vacuum tightness reaches 5.6E after aiming at sputtering source
-6during mbar, employing ion beam bombardment treats sputter material successively and equipment sputtering target cleans, and subsequently, under the condition of plasma body, start sputtering, sputter rate is 2nm/65s; Material to be sputtered is the ceramic mother metal after two removing surfaces obtaining of two ceramic mother metals with reactive metal layer or step one.
The shearing resistance of the joint that the present embodiment connects is 223MPa.
Embodiment 5: a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application of the present embodiment, carry out according to the following steps:
One, removing surface: first adopt ZrC to be connected to two in 500#, 800#, 1000# and 1500#
0.95/ HfN
0.95pottery mother metal is polished step by step, then refines step by step with the silicon carbide paper of 1500# and 2000#, finally to the ZrC that two after fine grinding are to be connected
0.95/ HfN
0.95after pottery mother metal carries out polishing, be placed in acetone, then be the ultrasonic cleaning 30min of 88Hz through frequency, be then placed in dehydrated alcohol, ultrasonic cleaning 10min, be finally placed in loft drier, dry 10h at 60 DEG C, namely obtains the ZrC after two removing surfaces
0.95/ HfN
0.95pottery mother metal;
Two, preset reactive metal layer: the ZrC after two removing surfaces adopting magnetron sputtering technique to obtain in step one
0.95/ HfN
0.95pottery mother metal surface pre-set thickness is the Ti layer of 5 μm, obtains the ZrC that two have Ti layer
0.95/ HfN
0.95pottery mother metal, then at two ZrC
0.95/ HfN
0.95the Ti layer of pottery mother metal carries out secondary magnetron sputtering, and pre-set thickness is the Zr layer of 5 μm, obtains the HfN that two have double-layer active metal level
0.95pottery mother metal, has the ZrC of double-layer active metal level with acetone and dehydrated alcohol to obtain two successively
0.95/ HfN
0.95pottery mother metal cleaning coating surface 5min, obtains two samples to be connected after drying up;
Three, diffusion in vacuum connects: the interface to be connected with Ti/Zr layer of two samples to be connected step 2 obtained stacks up, and is placed in diffusion in vacuum stove, Bonding pressure be 20MPa, vacuum tightness is 1.3 × 10
-4the condition of Pa, with the heating rate of 10 DEG C/min to 700 DEG C, then 20min is incubated, then be warming up to the speed of 5 DEG C/min and connect temperature 1300 DEG C, after the insulation 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.
In the present embodiment, magnetron sputtering technique specific operation process is as follows: put into by material to be sputtered in magnetron sputtering equipment vacuum oven, starts to vacuumize, when vacuum tightness reaches 5.6E after aiming at sputtering source
-6during mbar, employing ion beam bombardment treats sputter material successively and equipment sputtering target cleans, and subsequently, under the condition of plasma body, start sputtering, sputter rate is 2nm/65s; Material to be sputtered is the ceramic mother metal after two removing surfaces obtaining of two ceramic mother metals with reactive metal layer or step one.
The shearing resistance of the joint that the present embodiment connects is 223MPa.
Claims (9)
1., based on the composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link of high temperature application, it is characterized in that the method is carried out according to the following steps:
One, removing surface: adopt the diamond disk of two kinds in 500# ~ 1500# or wherein two or more model to polish step by step to two ceramic mother metals to be connected, refine step by step with the silicon carbide paper of two in 1500# ~ 2000# kind or wherein two or more model again, after finally polishing being carried out to the ceramic mother metal that two after fine grinding are to be connected, be placed in acetone, ultrasonic cleaning 15min ~ 30min, then dehydrated alcohol is placed in, ultrasonic cleaning 10min ~ 15min, finally be placed in loft drier and dry, namely obtain the ceramic mother metal after two removing surfaces; Wherein said ceramic mother metal is MCx one-component ceramic, MNx one-component ceramic, MNx/MNx complex phase ceramic, MCx/MCx complex phase ceramic or MNx/MCx complex phase ceramic;
Two, preset reactive metal layer: the ceramic mother metal surface pre-set thickness after two removing surfaces adopting the mode of magnetron sputtering technique or electronics evaporation to obtain in step one is the reactive metal layer A of 2 ~ 10 μm, obtain the ceramic mother metal that two have reactive metal layer, then in the reactive metal layer of two ceramic mother metals, secondary magnetron sputtering or electronics evaporation is carried out, pre-set thickness is the reactive metal layer B of 5 ~ 20 μm, obtain the ceramic mother metal that two have double-layer active metal level, to obtain two, there is the ceramic mother metal cleaning coating surface 5min ~ 10min of double-layer active metal level with acetone and dehydrated alcohol successively, two samples to be connected are obtained after drying up, active metal in wherein said reactive metal layer A and B is Ti, Zr, Hf, V, Nb or Ta, and the active metal in reactive metal layer A and B is two kinds of metals,
Three, diffusion in vacuum connects: the interface to be connected with reactive metal layer of two samples to be connected step 2 obtained stacks up, and is placed in diffusion in vacuum stove, Bonding pressure be 15MPa ~ 25MPa, vacuum tightness is 0.8 × 10
-3pa ~ 1.3 × 10
-4under the condition of Pa, with the heating rate of 5 ~ 10 DEG C/min to 700 DEG C, then 10 ~ 180min is incubated, then be warming up to the speed of 5 ~ 10 DEG C/min and connect temperature 1300 ~ 1400 DEG C, after insulation 10 ~ 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.
2. a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application according to claim 1, it is characterized in that the M in the MCx one-component ceramic described in step one is Ti, Zr, Hf, V, Nb or Ta, x is: 0.55≤x≤1; M in MNx one-component ceramic described in step one is Ti, Zr, Hf, V, Nb or Ta, and x is: 0.55≤x≤1; M in MNx/MNx complex phase ceramic described in step one is Ti, Zr, Hf, V, Nb or Ta, and x is: 0.55≤x≤1; M in MCx/MCx complex phase ceramic described in step one is Ti, Zr, Hf, V, Nb or Ta, and x is 0.55≤x≤1; In MNx/MCx complex phase ceramic described in step one, the M in MNx is Ti, Zr, Hf, V, Nb or Ta, and x is: 0.55≤x≤1, and the M in MCx is Ti, Zr, Hf, V, Nb or Ta, and x is: 0.55≤x≤1.
3. a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application according to claim 1, is characterized in that the silicon carbide paper described in step one is silicon carbide silicon carbide paper or aluminum oxide silicon carbide paper.
4. a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application according to claim 1, is characterized in that the ultrasonic frequency described in step one is 88Hz.
5. a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application according to claim 1, is characterized in that the oven dry described in step one refers to dry 10h at 60 DEG C.
6. a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application according to claim 1, if it is characterized in that, the thickness of reactive metal layer A and reactive metal layer B is greater than 10 μm, the then operation of replacement step two or the operation according to step 2 in the steps below: to be the active metal paillon foil A of 10 ~ 30 μm and thickness by thickness the be active metal paillon foil B of 10 ~ 30 μm, with the hydrofluoric acid aqueous solution ultrasonic cleaning 1min that mass concentration is 5%, use washes of absolute alcohol 10min again, dry up rear stand-by; The size of wherein said active metal paillon foil A and active metal paillon foil B is greater than ceramic mother metal to be connected; Active metal in reactive metal layer A and B is Ti, Zr, Hf, V, Nb or Ta, and the active metal in reactive metal layer A and B is two kinds of metals.
7. a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application according to claim 6, if it is characterized in that, the thickness of reactive metal layer A and reactive metal layer B is greater than 10 μm, the then operation of replacement step three or the operation according to step 3 in the steps below: in the middle of two samples to be connected that tinsel A and B step 2 obtained obtains in step one according to the laminated structure of A/B/A, the sample assembled is placed in diffusion in vacuum stove, be 15MPa ~ 25MPa at Bonding pressure, vacuum tightness is 0.8 × 10
-3pa ~ 1.3 × 10
-4under the condition of Pa, with the heating rate of 5 ~ 10 DEG C/min to 700 DEG C, then 10 ~ 180min is incubated, then be warming up to the speed of 5 ~ 10 DEG C/min and connect temperature 1300 ~ 1400 DEG C, after insulation 10 ~ 180min time, be down to 800 DEG C so that the speed of 5 DEG C/min is cold, be then cooled to 100 DEG C with the speed of 10 DEG C/min, cool to room temperature with the furnace afterwards, namely complete.
8. a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application according to claim 1, it is characterized in that the magnetron sputtering technique specific operation process described in step 2 is as follows: put into by material to be sputtered in magnetron sputtering equipment vacuum oven, start to vacuumize, when vacuum tightness reaches 5.6E after aiming at sputtering source
-6during mbar, employing ion beam bombardment treats sputter material successively and equipment sputtering target cleans, and subsequently, under the condition of plasma body, start sputtering, sputter rate is 2nm/65s.
9. a kind of composite reactive middle layer diffusion connection method realizing interstitial carbon compound or nitride ceramics seamless link based on high temperature application according to claim 1, it is characterized in that the described electronics evaporation specific operation process described in step 2 is as follows: check the air-conditioning system of decontamination chamber and the humidity of instrument room, confirm normally, instrumentation master menu selects auto-programming, put deposition material into steaming and cross stove, after the ceramic mother metal had two after two removing surfaces that the ceramic mother metal of reactive metal layer or step one obtain puts into vacuum chamber, start to vacuumize, reach 1 × 10
-4after the vacuum tightness of Pa, unlocking electronic bundle high-voltage power supply, run the program write, until program end of run, plated film completes, and namely completes.
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