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CN101391901B - Brazing method Al2O3 ceramic and metallic material - Google Patents

Brazing method Al2O3 ceramic and metallic material Download PDF

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Publication number
CN101391901B
CN101391901B CN2008101374834A CN200810137483A CN101391901B CN 101391901 B CN101391901 B CN 101391901B CN 2008101374834 A CN2008101374834 A CN 2008101374834A CN 200810137483 A CN200810137483 A CN 200810137483A CN 101391901 B CN101391901 B CN 101391901B
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ceramics
active
alloy
metal material
brazing method
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CN101391901A (en
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张丽霞
王颖
冯吉才
徐富家
张春光
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Harbin Institute of Technology Shenzhen
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Harbin Institute of Technology Shenzhen
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Abstract

The invention discloses a braze welding method of AI2O3 ceramics and metal material, and relates to the connection method of the AI2O3 ceramics and the metal material. The invention solves the problem of the existing method for connecting the AI2O3 ceramics and the metal material that the strength of a connector after connection is low and the air tightness of a connecting piece is low. The brazewelding method of the AI2O3 ceramics and the metal material of the invention is carried out according to the following steps: 1. the cleaning of the ceramics, and the decoating of a chaff; 2. the preparation of active metalized ceramics; 3. metal cleaning; and 4. braze welding; thus obtaining a welding part of the ceramics and the metal material. Another method of the invention is carried out according to the following steps: 1. the cleaning of the ceramics, and the preparation of active metalized powder paste; 2. the preparation of the active metalized ceramics; 3. metal cleaning; and 4. braze welding; thus obtaining the welding part of the ceramics and the metal material. The connection strength of the connector of the welding part welded by the method of the invention can reach up to 50 to 100 MPa, and the leakage rate of the connector is less than 1.0 multiplied by 10<-8>Pa question mark m<3>/s.

Description

Al 2O 3The method for welding of pottery and metallic substance
Technical field
The present invention relates to Al 2O 3The method of attachment of pottery and metallic substance.
Background technology
Al 2O 3Pottery has premium propertiess such as intensity height, hardness height, high temperature resistant, anticorrosive, wear-resisting and good insulation preformance, is widely used in fields such as power electronics, aerospace, energy traffic.Make it be difficult to processing and make but the stupalith inherent is rigid with fragility, need unite use with metal, the complementation on realization and the metallicity.And aluminium and alloy thereof are widely used metallic substance, and plasticity is good, density is little, thermal conductance and specific conductivity height, Al 2O 3Pottery and aluminium is the composite component of excellent properties separately, and wide application prospect is arranged.Therefore how with Al 2O 3Pottery couples together with aluminium or its alloy, and the joint that obtains high strength, high-air-tightness just becomes problem demanding prompt solution.Because Al 2O 3Pottery is huge with the aluminium alloy nature difference, and aluminium, aluminium alloy fusing point are low, and active soldering method (connect temperature and be higher than 700 ℃) can not be used for connecting Al 2O 3Pottery and aluminium or its alloy.And adopt Al-Si, the Al-Cu, the Al-Mg solder that do not contain Ti, Zr isoreactivity element to connect Al 2O 3When pottery and aluminium, strength of joint can only reach about 30MPa, and linkage interface exists a large amount of not holes of seam, joint leak rate〉10 -5Pam 3/ s is difficult to satisfy the requirement of high-air-tightness.Al 2O 3Pottery is connected with the diffusion of aluminium then needs to apply the long time of bigger pressure, insulation, even like this, also has not seam zone in the junction and occurs; Diffusion simultaneously connects the joint form that also is not suitable for complexity, and the application in actual production is restricted.
Summary of the invention
The present invention is in order to solve the existing Al of connection 2O 3Pottery and strength of joint after the method for metallic substance is connected hang down the low problem of resistance to air loss with web member, and Al is provided 2O 3The method for welding of pottery and metallic substance.
Al of the present invention 2O 3Pottery carries out according to following steps with the method for welding of metallic substance: one, be that medium is to Al with acetone 2O 3Pottery carries out ultrasonic cleaning, will clean with acetone behind the active metallization alloy foil sheet surface deoxidation film; Two, the active metallization alloy foil sheet is placed Al 2O 3On the pre-connection face of pottery, foil thickness is 10～400 μ m, and the workpiece that assembles is put into vacuum furnace, vacuumizes, and treats that vacuum tightness reaches 1.0 * 10 -3Behind the Pa, be warming up to 700～1000 ℃ and be incubated 5～15min with the speed of 10～30 ℃/min, the speed with 5～10 ℃/min is cooled to 300～500 ℃ then, turns off power supply and naturally cools to room temperature, promptly obtains the Al of active metallization 2O 3Pottery; Three, metallic substance is cleaned, remove surface and oil contaminant with degreaser after, be earlier NaOH solution cleaning 1～20min of 6%～10% with 40～60 ℃, mass concentration, be 30% HNO again with mass concentration 3Solution cleans 1～20min, and dry naturally water flushing back then; Four, with the Al of active metallization 2O 3Pottery joins with the pre-connection face of metallic substance, puts into vacuum furnace, vacuumizes, and treats that vacuum tightness reaches 1.0 * 10 -3Be warming up to 400～650 ℃ and be incubated 5～20min with the speed of 20～30 ℃/min behind the Pa, the speed with 5～10 ℃/min is cooled to 200～300 ℃ then, turns off power supply and naturally cools to room temperature; Promptly obtain Al 2O 3The weldment of pottery and metallic substance; Reactive metal alloy in the step 1 contains 0.5%～20% active element and 65%～99.3% Al eutectic element according to weight percent; Wherein active element is one or more the combination among Ti, Zr, Hf, V, Nb and the Ta.
The another kind of Al of the present invention 2O 3Pottery carries out according to following steps with the method for welding of metallic substance: one, be that medium is to Al with acetone 2O 3Pottery carries out ultrasonic cleaning, with granularity be 100～500 purpose active metallization powdered alloys and binding agent according to 1～20: 1 mass ratio mixed the active metallization powder paste; Two, the active metallization powder paste that step 1 is made is coated in Al 2O 3On the pre-connection face of pottery, coat-thickness is 100～300 μ m, will apply back Al 2O 3Pottery put into vacuum furnace, vacuumize, treat that vacuum tightness reaches 1.0 * 10 -3Behind the Pa, be warming up to 700～1000 ℃ and be incubated 5～15min with the speed of 10～30 ℃/min, the speed with 5～10 ℃/min is cooled to 300～500 ℃ then, turns off power supply and naturally cools to room temperature, promptly obtains the Al of active metallization 2O 3Pottery; Three, metallic substance is cleaned, remove surface and oil contaminant with degreaser after, be earlier NaOH solution cleaning 1～20min of 6%～10% with 40～60 ℃, mass concentration, be 30% HNO again with mass concentration 3Solution cleans 1～20min, and dry naturally water flushing back then; Four, with the Al of active metallization 2O 3Pottery joins with the pre-connection face of metallic substance, puts into vacuum furnace, vacuumizes, and treats that vacuum tightness reaches 1.0 * 10 -3Be warming up to 400～650 ℃ and be incubated 5～20min with the speed of 20～30 ℃/min behind the Pa, the speed with 5～10 ℃/min is cooled to 200～300 ℃ then, turns off power supply and naturally cools to room temperature; Promptly obtain Al 2O 3The weldment of pottery and metallic substance; Active metallization powdered alloy in the step 1 contains 0.5%～20% active element and 65%～99.3% Al eutectic element according to weight percent; Wherein active element is one or more the combination among Ti, Zr, Hf, V, Nb and the Ta.
Two kinds of Al of the present invention 2O 3Pottery has the following advantages with the method for welding of metallic substance: 1, can obtain bonding strength height, metal level that compactness is good in ceramic side, reactive metal layer again can be as the middle layer that connects aluminium alloy simultaneously, need not to add other solder, brazing flux, particularly for the actual complex structure, solve solder and added difficult problems such as form, the accurate control of thickness, joint strength of joint height can reach 50～100MPa, joint resistance to air loss height, leak rate＜1.0 * 10 -8Pam 3/ s; 2, compare with traditional Mn-Mo sintered powder method, greatly reduce treatment temp and time, do not need gases such as hydrogen, nitrogen, coal gas simultaneously, more simple to the requirement of working condition; Insensitive to ceramics component, kind, can be used for 95 porcelain, 99 porcelain, other oxide ceramics even non-oxide ceramics, to use extensivelyr, adaptability is stronger; 3, compare with methods such as chemistry, vapour depositions, higher with the bonding strength of pottery; Because ceramic surface reaction thing is a complex compound, more stable than metal, it is little influenced by the secondary soldering processes, more easy to control simultaneously; Also can eliminate for a long time and under comparatively high temps, use, the hidden danger that metal level and Al interact and cause ceramic side interfacial layer thickness to reduce gradually so that lost efficacy.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment Al 2O 3Pottery carries out according to following steps with the method for welding of metallic substance: one, be that medium is to Al with acetone 2O 3Pottery carries out ultrasonic cleaning, will clean with acetone behind the active metallization alloy foil sheet surface deoxidation film; Two, the active metallization alloy foil sheet is placed Al 2O 3On the pre-connection face of pottery, foil thickness is 10～400 μ m, and the workpiece that assembles is put into vacuum furnace, vacuumizes, and treats that vacuum tightness reaches 1.0 * 10 -3Behind the Pa, be warming up to 700～1000 ℃ and be incubated 5～15min with the speed of 10～30 ℃/min, the speed with 5～10 ℃/min is cooled to 300～500 ℃ then, turns off power supply and naturally cools to room temperature, promptly obtains the Al of active metallization 2O 3Pottery; Three, metallic substance is cleaned, remove surface and oil contaminant with degreaser after, be earlier NaOH solution cleaning 1～20min of 6%～10% with 40～60 ℃, mass concentration, be 30% HNO again with mass concentration 3Solution cleans 1～20min, and dry naturally water flushing back then; Four, with the Al of active metallization 2O 3Pottery joins with the pre-connection face of metallic substance, puts into vacuum furnace, vacuumizes, and treats that vacuum tightness reaches 1.0 * 10 -3Be warming up to 400～650 ℃ and be incubated 5～20min with the speed of 20～30 ℃/min behind the Pa, the speed with 5～10 ℃/min is cooled to 200～300 ℃ then, turns off power supply and naturally cools to room temperature; Promptly obtain Al 2O 3The weldment of pottery and metallic substance; Reactive metal alloy in the step 1 contains 0.5%～20% active element and 65%～99.3% Al eutectic element according to weight percent.
Present embodiment is applicable to that the pre-connection face is the welding of planar pottery and metal, and the shape of paillon foil is identical with the pre-connection face of pottery with size in the step 1.
Embodiment two: the difference of present embodiment and embodiment one is: Al in the step 1 2O 3Pottery is 95 porcelain or 99 porcelain.Other step and parameter are identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment one is: the reactive metal alloy in the step 1 contains 5%～15% active element and 70%～85% Al eutectic element according to weight percent.Other step and parameter are identical with embodiment one.
Embodiment four: the difference of present embodiment and embodiment one is: the reactive metal alloy in the step 1 contains 10% active element and 90% Al eutectic element according to weight percent.Other step and parameter are identical with embodiment one.
Embodiment five: the difference of present embodiment and embodiment one is: the reactive metal alloy in the step 1 also contains 0.1～5% element according to weight percent, and element is one or more the combination among Ce, La and the Y.Other step and parameter are identical with embodiment one.
Press the arbitrary proportion combination when element is made up of two kinds or two or more material in the present embodiment.
Embodiment six: the difference of present embodiment and embodiment one is: the reactive metal alloy in the step 1 also contains 3% element according to weight percent.Other step and parameter are identical with embodiment one.
Embodiment seven: the difference of present embodiment and embodiment one is: the reactive metal alloy in the step 1 also contains 0.1～10% particle wild phase according to weight percent, and the particle wild phase is Al 2O 3, SiO 2, TiC, C and B one or more combination.Other step and parameter are identical with embodiment one.
Press the arbitrary proportion combination when particle wild phase is made up of two kinds or two or more material in the present embodiment.
Embodiment eight: the difference of present embodiment and embodiment one is: the reactive metal alloy in the step 1 also contains 5% particle wild phase according to weight percent.Other step and parameter are identical with embodiment one.
Embodiment nine: the difference of present embodiment and embodiment one is: the active element in the reactive metal alloy in the step 1 is one or more the combination among Ti, Zr, Hf, V, Nb and the Ta.Other step and parameter are identical with embodiment one.
Press the arbitrary proportion combination when active element is made up of two kinds or two or more material in the present embodiment.
Embodiment ten: the difference of present embodiment and embodiment one is: the Al eutectic element in the reactive metal alloy in the step 1 is one or more the combination among Mg, Si, Cu, Zn, Ge, Ni and the Ag.Other step and parameter are identical with embodiment one.
Press the arbitrary proportion combination when Al eutectic element is made up of two kinds or two or more material in the present embodiment.
Embodiment 11: the difference of present embodiment and embodiment one is: foil thickness is 160～320 μ m in the step 2.Other step and parameter are identical with embodiment one.
Embodiment 12: the difference of present embodiment and embodiment one is: foil thickness is 240 μ m in the step 2.Other step and parameter are identical with embodiment one.
Embodiment 13: the difference of present embodiment and embodiment one is: the speed with 15～25 ℃/min in the step 2 is warming up to 800～900 ℃.Other step and parameter are identical with embodiment one.
Embodiment 14: the difference of present embodiment and embodiment one is: the speed with 20 ℃/min in the step 2 is warming up to 850 ℃.Other step and parameter are identical with embodiment one.
Embodiment 15: the difference of present embodiment and embodiment one is: back insulation 8～12min heats up in the step 2.Other step and parameter are identical with embodiment one.
Embodiment 16: the difference of present embodiment and embodiment one is: back insulation 10min heats up in the step 2.Other step and parameter are identical with embodiment one.
Embodiment 17: the difference of present embodiment and embodiment one is: the speed with 7～9 ℃/min in the step 2 is cooled to 350～450 ℃.Other step and parameter are identical with embodiment one.
Embodiment 18: the difference of present embodiment and embodiment one is: the speed with 8 ℃/min in the step 2 is cooled to 400 ℃.Other step and parameter are identical with embodiment one.
Embodiment 19: the difference of present embodiment and embodiment one is: the metallic substance in the step 3 is Al, Al-Cu alloy, Al-Mn alloy, Al-Si alloy, Al-Mg alloy, Al-Mg-Si alloy, Al-Zn-Mg-Cu alloy or Al-Li alloy.Other step and parameter are identical with embodiment one.
Embodiment 20: the difference of present embodiment and embodiment one is: the degreaser in the step 3 is gasoline or acetone.Other step and parameter are identical with embodiment one.
Embodiment 21: the difference of present embodiment and embodiment one is: in the step 3 earlier be NaOH solution alkali cleaning 6～14min of 7%～9% with 45～55 ℃, mass concentration to metallic substance.Other step and parameter are identical with embodiment one.
Embodiment 22: the difference of present embodiment and embodiment one is: in the step 3 earlier be 8% NaOH solution cleaning 10min with 50 ℃, mass concentration to metallic substance.Other step and parameter are identical with embodiment one.
Embodiment 23: the difference of present embodiment and embodiment one is: use HNO again after in the step 3 metallic substance being cleaned with NaOH solution 3Solution cleans 5～15min.Other step and parameter are identical with embodiment one.
Embodiment 24: the difference of present embodiment and embodiment one is: use HNO again after in the step 3 metallic substance being cleaned with NaOH solution 3Solution cleans 10min.Other step and parameter are identical with embodiment one.
Embodiment 25: the difference of present embodiment and embodiment one is: be warming up to 480～570 ℃ and be incubated 10～15min with the speed of 22～28 ℃/min in the step 4.Other step and parameter are identical with embodiment one.
Embodiment 26: the difference of present embodiment and embodiment one is: be warming up to 525 ℃ and be incubated 12min with the speed of 25 ℃/min in the step 4.Other step and parameter are identical with embodiment one.
Embodiment 27: the difference of present embodiment and embodiment one is: the speed with 6～8 ℃/min in the step 4 is cooled to 220～280 ℃.Other step and parameter are identical with embodiment one.
Embodiment 28: the difference of present embodiment and embodiment one is: the speed with 7 ℃/min in the step 4 is cooled to 250 ℃.Other step and parameter are identical with embodiment one.
Embodiment 29: present embodiment Al 2O 3Pottery (95 porcelain) carries out according to following steps with the method for welding of metallic substance (5A05 aluminium alloy): one, be that medium is to Al with acetone 2O 3Pottery carries out ultrasonic cleaning, will clean with acetone behind the active metallization alloy foil sheet surface deoxidation film; Two, the active metallization alloy foil sheet is placed Al 2O 3On the pre-connection face of pottery, foil thickness is 100 μ m, and the workpiece that assembles is put into vacuum furnace, vacuumizes, and treats that vacuum tightness reaches 1.0 * 10 -3Behind the Pa, be warming up to 850 ℃ and be incubated 10min with the speed of 20 ℃/min, the speed with 8 ℃/min is cooled to 400 ℃ then, naturally cools to room temperature then, promptly obtains the Al of active metallization 2O 3Pottery; Three, metallic substance is cleaned, remove surface and oil contaminant with gasoline after, be earlier 8% NaOH solution cleaning 5min with 50 ℃, mass concentration, be 30% HNO again with mass concentration 3Solution cleans 3min, and dry naturally water flushing back then; Four, with the Al of active metallization 2O 3Pottery joins with the pre-connection face of metallic substance, puts into vacuum furnace, vacuumizes, and treats that vacuum tightness reaches 1.0 * 10 -3Be warming up to 550 ℃ and be incubated 15min with the speed of 25 ℃/min behind the Pa, the speed with 8 ℃/min is cooled to 260 ℃ then, naturally cools to room temperature; Promptly obtain Al 2O 3The weldment of pottery and metallic substance; Reactive metal alloy in the step 1 is made up of 10% active element, 79.5% Al eutectic element, 0.5% element and 10% particle wild phase according to weight percent.
Active element in the present embodiment reactive metal alloy is Ti, and Al eutectic element is Cu, and element is Ce, and the particle wild phase is Al 2O 3
Present embodiment obtains Al 2O 3Pottery is 100MPa with the strength of joint of the weldment of metallic substance, and the joint leak rate is 3 * 10 -9Pam 3/ s.
Embodiment 30: present embodiment Al 2O 3Pottery carries out according to following steps with the method for welding of metallic substance: one, be that medium is to Al with acetone 2O 3Pottery carries out ultrasonic cleaning, with granularity be 100～500 purpose active metallization powdered alloys and binding agent according to the mass ratio of 1～20:1 mixed the active metallization powder paste; Two, the active metallization powder paste that step 1 is made is coated in Al 2O 3On the pre-connection face of pottery, coat-thickness is 100～300 μ m, will apply back Al 2O 3Pottery put into vacuum furnace, vacuumize, treat that vacuum tightness reaches 1.0 * 10 -3Behind the Pa, be warming up to 700～1000 ℃ and be incubated 5～15min with the speed of 10～30 ℃/min, the speed with 5～10 ℃/min is cooled to 300～500 ℃ then, naturally cools to room temperature then, promptly obtains the Al of active metallization 2O 3Pottery; Three, metallic substance is cleaned, remove surface and oil contaminant with degreaser after, be earlier NaOH solution cleaning 1～20min of 6%～10% with 40～60 ℃, mass concentration, be 30% HNO again with mass concentration 3Solution cleans 1～20min, and dry naturally water flushing back then; Four, with the Al of active metallization 2O 3Pottery joins with the pre-connection face of metallic substance, puts into vacuum furnace, vacuumizes, and treats that vacuum tightness reaches 1.0 * 10 -3Be warming up to 400～650 ℃ and be incubated 5～20min with the speed of 20～30 ℃/min behind the Pa, the speed with 5～10 ℃/min is cooled to 200～300 ℃ then, naturally cools to room temperature; Promptly obtain Al 2O 3The weldment of pottery and metallic substance; Active metallization powdered alloy in the step 1 contains 0.5%～20% active element and 65%～99.3% Al eutectic element according to weight percent.
Present embodiment is applicable to that the pre-connection face is not planar pottery and Metal Material Welding.
The embodiment hentriaconta-: the difference of present embodiment and embodiment 30 is: Al in the step 1 2O 3Pottery is 95 porcelain or 99 porcelain.Other step and parameter are identical with embodiment 30.
Embodiment 32: the difference of present embodiment and embodiment 30 is: the granularity of the active metallization powdered alloy in the step 1 is 200～300 orders.Other step and parameter are identical with embodiment 30.
Embodiment 33: the difference of present embodiment and embodiment 30 is: the granularity of the active metallization powdered alloy in the step 1 is 250 orders.Other step and parameter are identical with embodiment 30.
Embodiment 34: the difference of present embodiment and embodiment 30 is: the active metallization powdered alloy in the step 1 contains 5%～15% active element and 70%～85% Al eutectic element according to weight percent.Other step and parameter are identical with embodiment 30.
Embodiment 35: the difference of present embodiment and embodiment 30 is: the active metallization powdered alloy in the step 1 contains 10% active element and 90% Al eutectic element according to weight percent.Other step and parameter are identical with embodiment 30.
Embodiment 36: the difference of present embodiment and embodiment 30 is: the active metallization powdered alloy in the step 1 also contains 0.1～5% element according to weight percent, and element is one or more the combination among Ce, La and the Y.Other step and parameter are identical with embodiment 30.
Press the arbitrary proportion combination when element is made up of two kinds or two or more material in the present embodiment.
Embodiment 37: the difference of present embodiment and embodiment 30 is: the active metallization powdered alloy in the step 1 also contains 3% element according to weight percent.Other step and parameter are identical with embodiment 30.
Embodiment 38: the difference of present embodiment and embodiment 30 is: the active metallization powdered alloy in the step 1 also contains 0.1～10% particle wild phase according to weight percent, and the particle wild phase is Al 2O 3, SiO 2, TiC, C and B one or more combination.Other step and parameter are identical with embodiment 30.
Press the arbitrary proportion combination when particle wild phase is made up of two kinds or two or more material in the present embodiment.
Embodiment 39: the difference of present embodiment and embodiment 30 is: the active metallization powdered alloy in the step 1 also contains 5% particle wild phase according to weight percent.Other step and parameter are identical with embodiment 30.
Embodiment 40: the difference of present embodiment and embodiment 30 is: the active element in the active metallization powdered alloy in the step 1 is one or more the combination among Ti, Zr, Hf, V, Nb and the Ta.Other step and parameter are identical with embodiment 30.
Press the arbitrary proportion combination when active element is made up of two kinds or two or more material in the present embodiment.
Embodiment 41: the difference of present embodiment and embodiment 30 is: the Al eutectic element in the active metallization powdered alloy in the step 1 is one or more the combination among Mg, Si, Cu, Zn, Ge, Ni and the Ag.Other step and parameter are identical with embodiment 30.
Press the arbitrary proportion combination when Al eutectic element is made up of two kinds or two or more material in the present embodiment.
Embodiment 42: present embodiment with the difference of embodiment 30 is: active metallization powdered alloy and binding agent mix according to the mass ratio of 6～16:1 in the step 1.Other step and parameter are identical with embodiment 30.
Embodiment 43: present embodiment with the difference of embodiment 30 is: active metallization powdered alloy and binding agent mix according to the mass ratio of 11:1 in the step 1.Other step and parameter are identical with embodiment 30.
Embodiment 44: the difference of present embodiment and embodiment 30 is: the binding agent in the step 1 is a glycerol.Other step and parameter are identical with embodiment 30.
Embodiment 45: the difference of present embodiment and embodiment 30 is: step 2 floating coat thickness is 150～250 μ m.Other step and parameter are identical with embodiment 30.
Embodiment 46: the difference of present embodiment and embodiment 30 is: step 2 floating coat thickness is 200 μ m.Other step and parameter are identical with embodiment 30.
Embodiment 47: the difference of present embodiment and embodiment 30 is: the speed with 15～25 ℃/min in the step 2 is warming up to 800～900 ℃.Other step and parameter are identical with embodiment 30.
Embodiment 48: the difference of present embodiment and embodiment 30 is: the speed with 20 ℃/min in the step 2 is warming up to 850 ℃.Other step and parameter are identical with embodiment 30.
Embodiment 49: the difference of present embodiment and embodiment 30 is: back insulation 8～12min heats up in the step 2.Other step and parameter are identical with embodiment 30.
Embodiment 50: the difference of present embodiment and embodiment 30 is: back insulation 10min heats up in the step 2.Other step and parameter are identical with embodiment 30.
Embodiment 51: the difference of present embodiment and embodiment 30 is: the speed with 7～9 ℃/min in the step 2 is cooled to 350～450 ℃.Other step and parameter are identical with embodiment 30.
Embodiment 52: the difference of present embodiment and embodiment 30 is: the speed with 8 ℃/min in the step 2 is cooled to 400 ℃.Other step and parameter are identical with embodiment 30.
Embodiment 53: the difference of present embodiment and embodiment 30 is: the metallic substance in the step 3 is Al, Al-Cu alloy, Al-Mn alloy, Al-Si alloy, Al-Mg alloy, Al-Mg-Si alloy, Al-Zn-Mg-Cu alloy or Al-Li alloy.Other step and parameter are identical with embodiment 30.
Embodiment 54: the difference of present embodiment and embodiment 30 is: the degreaser in the step 3 is gasoline or acetone.Other step and parameter are identical with embodiment 30.
Embodiment 55: the difference of present embodiment and embodiment 30 is: in the step 3 earlier be NaOH solution alkali cleaning 6～14min of 7%～9% with 45～55 ℃, mass concentration to metallic substance.Other step and parameter are identical with embodiment 30.
Embodiment 56: the difference of present embodiment and embodiment 30 is: in the step 3 earlier be 8% NaOH solution cleaning 10min with 50 ℃, mass concentration to metallic substance.Other step and parameter are identical with embodiment 30.
Embodiment 57: the difference of present embodiment and embodiment 30 is: use HNO again after in the step 3 metallic substance being cleaned with NaOH solution 3Solution cleans 5～15min.Other step and parameter are identical with embodiment 30.
Embodiment 58: the difference of present embodiment and embodiment 30 is: use HNO again after in the step 3 metallic substance being cleaned with NaOH solution 3Solution cleans 10min.Other step and parameter are identical with embodiment 30.
Embodiment 59: the difference of present embodiment and embodiment 30 is: be warming up to 480～570 ℃ and be incubated 10～15min with the speed of 22～28 ℃/min in the step 4.Other step and parameter are identical with embodiment 30.
Embodiment 60: the difference of present embodiment and embodiment 30 is: be warming up to 525 ℃ and be incubated 12min with the speed of 25 ℃/min in the step 4.Other step and parameter are identical with embodiment 30.
Embodiment 61: the difference of present embodiment and embodiment 30 is: the speed with 6～8 ℃/min in the step 4 is cooled to 220～280 ℃.Other step and parameter are identical with embodiment 30.
Embodiment 62: the difference of present embodiment and embodiment 30 is: the speed with 7 ℃/min in the step 4 is cooled to 250 ℃.Other step and parameter are identical with embodiment 30.
Embodiment 63: present embodiment Al 2O 3Pottery (95 porcelain) carries out according to following steps with the method for welding of metallic substance (5A05 aluminium alloy): one, be that medium is to Al with acetone 2O 3Pottery carries out ultrasonic cleaning, with granularity be 500 purpose active metallization powdered alloys and binding agent according to the mass ratio of 12:1 mixed the active metallization powder paste; Two, the active metallization powder paste that step 1 is made is coated in Al 2O 3On the pre-connection face of pottery, coat-thickness is 200 μ m, will apply back Al 2O 3Pottery put into vacuum furnace, vacuumize, treat that vacuum tightness reaches 1.0 * 10 -3Behind the Pa, be warming up to 800 ℃ and be incubated 10min with the speed of 20 ℃/min, the speed with 8 ℃/min is cooled to 400 ℃ then, naturally cools to room temperature then, promptly obtains the Al of active metallization 2O 3Pottery; Three, metallic substance is cleaned, remove surface and oil contaminant with acetone after, be earlier 8% NaOH solution cleaning 10min with 50 ℃, mass concentration, be 30% HNO again with mass concentration 3Solution cleans 3min, and dry naturally water flushing back then; Four, with the Al of active metallization 2O 3Pottery joins with the pre-connection face of metallic substance, puts into vacuum furnace, vacuumizes, and treats that vacuum tightness reaches 1.0 * 10 -3Be warming up to 500 ℃ and be incubated 12min with the speed of 25 ℃/min behind the Pa, the speed with 8 ℃/min is cooled to 250 ℃ then, naturally cools to room temperature; Promptly obtain Al 2O 3The weldment of pottery and metallic substance; Active metallization powdered alloy in the step 1 is made up of 10% active element, 82.3% Al eutectic element, 0.7% element and 7% particle wild phase according to weight percent.
Active element in the present embodiment reactive metal alloy is Ti, and Al eutectic element is Cu, and element is Y, and the particle wild phase is C.
Present embodiment obtains Al 2O 3Pottery is 90MPa with the strength of joint of the weldment of metallic substance, and the joint leak rate is 1 * 10 -9Pam 3/ s.

Claims (9)

1.一种Al2O3陶瓷与金属材料的钎焊方法，其特征在于Al2O3陶瓷与金属材料的钎焊方法是按照以下步骤进行的：一、以丙酮为介质对Al2O3陶瓷进行超声清洗，将活性金属化合金箔片表面去氧化膜后用丙酮清洗；二、将厚度为10～400μm的活性金属化合金箔片置于Al2O3陶瓷的预连接面上，然后放入真空加热炉中，抽真空，待真空度达到1.0×10-3Pa后，以10～30℃/min的速度升温至700～1000℃并保温5～15min，然后以5～10℃/min的速度降温至300～500℃，然后自然冷却至室温，即得到活性金属化的Al2O3陶瓷；三、对金属材料进行清洗，用除油剂去除表面油污后，先用40～60℃、质量浓度为6％～10％的NaOH溶液清洗1～20min，再用质量浓度为30％的HNO3溶液清洗1～20min，然后用水冲洗后自然晾干；四、将活性金属化的Al2O3陶瓷与金属材料的预连接面相接，放入真空加热炉中，抽真空，待真空度达到1.0×10-3Pa后以20～30℃/min的速度升温至400～650℃并保温5～20min，然后以5～10℃/min的速度降温至200～300℃，自然冷却至室温；即得到Al2O3陶瓷与金属材料的焊接件；步骤一中的活性金属化合金按照重量百分比含有0.5％～20％的活性元素和65％～99.3％的Al共晶元素；其中活性元素为Ti、Zr、Hf、V、Nb和Ta中的一种或几种的组合。1. a kind of Al2O3 brazing method of ceramics and metal material, it is characterized in that Al2O3 The brazing method of ceramics and metal material is carried out according to the following steps: one , take acetone as medium to Al2O3 Ceramics are ultrasonically cleaned, and the surface of the active metallized alloy foil is cleaned with acetone after the oxide film is removed; 2. The active metallized alloy foil with a thickness of 10-400 μm is placed on the pre-connected surface of the Al 2 O 3 ceramic, and then placed in Vacuumize in a vacuum heating furnace. After the vacuum degree reaches 1.0×10 -3 Pa, raise the temperature to 700-1000°C at a speed of 10-30°C/min and keep it warm for 5-15min, then at a rate of 5-10°C/min Slowly cool down to 300-500°C, and then naturally cool to room temperature to obtain active metallized Al 2 O 3 ceramics; 3. Clean the metal material, remove the surface oil with a degreasing agent, and then use 40-60°C, Wash with a NaOH solution with a mass concentration of 6% to 10% for 1 to 20 minutes, then wash with a HNO 3 solution with a mass concentration of 30% for 1 to 20 minutes, then rinse with water and dry naturally; 4. Active metallized Al 2 O 3 Connect the pre-connected surfaces of ceramics and metal materials, put them into a vacuum heating furnace, and vacuumize. After the vacuum degree reaches 1.0×10 -3 Pa, raise the temperature to 400-650°C at a speed of 20-30°C/min and keep it warm 5-20min, then cool down to 200-300°C at a rate of 5-10°C/min, and cool naturally to room temperature; that is, a welded piece of Al 2 O 3 ceramic and metal material is obtained; the active metallized alloy in step 1 is calculated according to the weight The percentage contains 0.5% to 20% of active elements and 65% to 99.3% of Al eutectic elements; wherein the active elements are one or a combination of Ti, Zr, Hf, V, Nb and Ta. 2.根据权利要求1所述的Al2O3陶瓷与金属材料的钎焊方法，其特征在于步骤一中Al2O3陶瓷为95瓷或99瓷。2. The brazing method of Al 2 O 3 ceramics and metal materials according to claim 1, characterized in that in step 1, the Al 2 O 3 ceramics are 95 porcelain or 99 porcelain. 3.根据权利要求1所述的Al2O3陶瓷与金属材料的钎焊方法，其特征在于步骤一中的活性金属化合金按照重量百分比还含有0.1～5％的第三元素，第三元素为Ce、La和Y中的一种或几种的组合。3. The brazing method of Al 2 O 3 ceramics and metal materials according to claim 1, characterized in that the active metallization alloy in step 1 also contains 0.1 to 5% of the third element according to the weight percentage, the third element It is one or a combination of Ce, La and Y. 4.根据权利要求1所述的Al2O3陶瓷与金属材料的钎焊方法，其特征在于步骤一中的活性金属化合金按照重量百分比还含有0.1～10％的颗粒增强相，颗粒增强相为Al2O3、SiO2、TiC、C和B的一种或几种的组合。4. The brazing method of Al 2 O 3 ceramics and metal materials according to claim 1, characterized in that the active metallization alloy in step 1 also contains 0.1 to 10% of the particle reinforcement phase according to the weight percentage, and the particle reinforcement phase It is one or a combination of Al 2 O 3 , SiO 2 , TiC, C and B. 5.根据权利要求1所述的Al2O3陶瓷与金属材料的钎焊方法，其特征在于步骤三中的金属材料为Al、Al-Cu合金、Al-Mn合金、Al-Si合金、Al-Mg合金、Al-Mg-Si合金、Al-Zn-Mg-Cu合金或Al-Li合金。5. Al according to claim 1 2 O 3 The brazing method of ceramics and metal materials is characterized in that the metal materials in step 3 are Al, Al-Cu alloys, Al-Mn alloys, Al-Si alloys, Al - Mg alloy, Al-Mg-Si alloy, Al-Zn-Mg-Cu alloy or Al-Li alloy. 6.一种Al2O3陶瓷与金属材料的钎焊方法，其特征在于Al2O3陶瓷与金属材料的钎焊方法是按照以下步骤进行的：一、以丙酮为介质对Al2O3陶瓷进行超声清洗，将粒度为100～500目的活性金属化合金粉末和粘结剂按照1～20∶1的质量比混合制得活性金属化粉末膏；二、将步骤一制得的活性金属化粉末膏涂敷在Al2O3陶瓷的预连接面上，涂层厚度为100～300μm，将涂覆后的Al2O3陶瓷放入真空加热炉中，抽真空，待真空度达到1.0×10-3Pa后，以10～30℃/min的速度升温至700～1000℃并保温5～15min，然后以5～10℃/min的速度降温至300～500℃，然后自然冷却至室温，即得到活性金属化的Al2O3陶瓷；三、对金属材料进行清洗，用除油剂去除表面油污后，先用40～60℃、质量浓度为6％～10％的NaOH溶液清洗1～20min，再用质量浓度为30％的HNO3溶液清洗1～20min，然后用水冲洗后自然晾干；四、将活性金属化的Al2O3陶瓷与金属材料的预连接面相接，放入真空加热炉中，抽真空，待真空度达到1.0×10-3Pa后以20～30℃/min的速度升温至400～650℃并保温5～20min，然后以5～10℃/min的速度降温至200～300℃，自然冷却至室温；即得到Al2O3陶瓷与金属材料的焊接件；步骤一中的活性金属化合金粉末按照重量百分比含有0.5％～20％的活性元素和65％～99.3％的Al共晶元素，其中活性元素为Ti、Zr、Hf、V、Nb和Ta中的一种或几种的组合。6. A kind of Al 2 O 3 brazing method of ceramics and metal material, it is characterized in that Al 2 O 3 The brazing method of ceramics and metal material is carried out according to the following steps: one, take acetone as medium to Al 2 O 3 The ceramics are ultrasonically cleaned, and the active metallization alloy powder with a particle size of 100 to 500 meshes and the binder are mixed according to a mass ratio of 1 to 20:1 to obtain an active metallization powder paste; 2. The active metallization powder paste prepared in step 1 The powder paste is coated on the pre-connected surface of the Al 2 O 3 ceramics, and the coating thickness is 100-300 μm. Put the coated Al 2 O 3 ceramics into a vacuum heating furnace, and vacuum until the vacuum degree reaches 1.0× After 10 -3 Pa, heat up to 700-1000°C at a rate of 10-30°C/min and hold for 5-15 minutes, then cool down to 300-500°C at a rate of 5-10°C/min, and then cool naturally to room temperature. That is, active metallized Al 2 O 3 ceramics can be obtained; 3. Clean the metal material, remove the surface oil with a degreasing agent, and then wash it with NaOH solution at 40-60 °C and a mass concentration of 6%-10% for 1-2 20min, then wash with HNO 3 solution with a mass concentration of 30% for 1-20min, then rinse with water and dry naturally; 4. Connect the active metallized Al 2 O 3 ceramics to the pre-connected surface of the metal material, put In the vacuum heating furnace, vacuumize, after the vacuum degree reaches 1.0×10 -3 Pa, raise the temperature to 400-650°C at a speed of 20-30°C/min and keep it warm for 5-20min, and then heat it at a speed of 5-10°C/min Lower the temperature to 200-300°C, and cool naturally to room temperature; that is, to obtain a welded piece of Al 2 O 3 ceramics and metal materials; the active metallization alloy powder in step 1 contains 0.5%-20% active elements and 65% by weight ~99.3% Al eutectic element, wherein the active element is one or a combination of Ti, Zr, Hf, V, Nb and Ta. 7.根据权利要求6所述的Al2O3陶瓷与金属材料的钎焊方法，其特征在于步骤一中的活性金属化合金粉末中的Al共晶元素为Mg、Si、Cu、Zn、Ge、Ni和Ag中的一种或几种的组合。7. Al according to claim 6 O 3 The brazing method of ceramics and metal materials is characterized in that the Al eutectic element in the active metallization alloy powder in the step 1 is Mg, Si, Cu, Zn, Ge , Ni and Ag in one or more combinations. 8.根据权利要求6所述的Al2O3陶瓷与金属材料的钎焊方法，其特征在于步骤二中以15～25℃/min的速度升温至800～900℃。8. The brazing method of Al 2 O 3 ceramics and metal materials according to claim 6, characterized in that in step 2, the temperature is raised to 800-900°C at a rate of 15-25°C/min. 9.根据权利要求6所述的Al2O3陶瓷与金属材料的钎焊方法，其特征在于步骤四中以22～28℃/min的速度升温至480～570℃并保温10～15min。9. The brazing method of Al 2 O 3 ceramics and metal materials according to claim 6, characterized in that in step 4, the temperature is raised to 480-570°C at a rate of 22-28°C/min and kept for 10-15min.
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