CN107363359A - A kind of method of compound high-entropy alloy solder ceramic soldering and metal - Google Patents
A kind of method of compound high-entropy alloy solder ceramic soldering and metal Download PDFInfo
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- CN107363359A CN107363359A CN201710677144.4A CN201710677144A CN107363359A CN 107363359 A CN107363359 A CN 107363359A CN 201710677144 A CN201710677144 A CN 201710677144A CN 107363359 A CN107363359 A CN 107363359A
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
- B23K1/206—Cleaning
Abstract
The present invention relates to a kind of method of compound high-entropy alloy solder ceramic soldering and metal, solves ceramet brazing process center tap interface and produces substantial amounts of weld metal zone brittle intermetallic thing, causes the problem of joint performance difference.Wherein compound high-entropy alloy pricker solder is formed by upper and lower two layers, and upper strata is the high-entropy alloy foil close to metal side, and lower floor is the titanium foil close to ceramic side.After matrix to be welded and the cleaning of solder foil, sandwich structure is assembled into, and the pressure for applying thereon 0.01 0.03MPa is placed in diffusion in vacuum stove to ensure that matrix fully contacts with solder layer, after the completion of assembling and carries out soldering.The present invention is simple to operate, utilize the high entropic effect of high-entropy alloy, FCC and BCC solid solution tissues are formed in brazed seam, without being generated between brittle metal in joint, the generation of weld metal zone brittle intermetallic thing in joint can effectively be suppressed, reacted simultaneously using active Ti elements in titanium foil with ceramics, form toughness compound in interface, realize effective metallurgical binding of ceramics and metal.
Description
Technical field
The invention belongs to technical field of dissimilar material connection, and in particular to a kind of compound high-entropy alloy solder ceramic soldering with
The method of metal
Background technology
Ceramics have the premium properties such as wear-resisting, high temperature resistant, corrosion-resistant and high rigidity, therefore have in fields such as space flight, the energy
Important application.But toughness is poor at normal temperatures for ceramics, it is difficult to is processed into complex-shaped structure member, this is just largely
On limit the application of ceramic material.And if ceramics are prepared into composite component with metal using interconnection technique, so
Both the excellent high-temperature behavior of ceramic material can be utilized, the plasticity and toughness of metal material can be played again, so as to effectively expand
Big ceramic-metal composite material application field, meets the needs of modern project application.
The connection of ceramics and metal has had substantial amounts of research at present, by ceramic surface pre-metallization and in metal pricker
The method that active element is added in material solves the problems, such as that metal solder is difficult to wetting on ceramics to a certain extent, some researchs
Person's proposition uses ternary system aluminium base solder, such as the crystalline state such as AlSiCu or AlSiMg solder to carry out high temperature brazing, and brazing temperature is
1100 DEG C, it is improved in some ceramics using interfacial reaction, such as the wetability on SiC.But due to elements such as Si, Cu, Mg
Addition, with ceramic matrix react after occur substantial amounts of weld metal zone brittle intermetallic thing in ceramic-metal joint, pass through optimization
Welding procedure, it is more difficult to which effectively species, quantity, form and the distribution of control weld metal zone brittle intermetallic thing phase, this is largely
On have impact on the mechanical property of soldered fitting.
The content of the invention
For insufficient existing for above-mentioned prior art processes, it is an object of the invention to provide a kind of compound high-entropy alloy solder
The method of ceramic soldering-metal, suppressed using the high entropic effect of high-entropy alloy during ceramic-metal brazing between brittle metal
The generation of compound.One layer of active titanium foil is placed between high-entropy alloy solder and ceramics simultaneously, is sent out by Ti elements and ceramics
Raw reaction, toughness compound is formed in interface, so as to realize effective metallurgical binding of ceramics and metal.
High-entropy alloy free energy is low, is easily formed BCC or FCC solid solution simple in construction, and there is microstructure to simplify,
It is not inclined to and intermetallic compound occurs, there is the feature such as nano-scaled precipitate and amorphous structure, so as to hard with high intensity, height
The premium properties such as degree, resistance to temper softening, wear-resisting, with being closed containing a kind of conventional solder of essential element atomic percent more than 50%
Metallographic ratio, it has broad application prospects in soldering field.And high-entropy alloy system is numerous, most of fusing points it is higher (
More than 1200 DEG C), for ceramics and the soldering of metal, AlNiCu ternarys high-entropy alloy, AlNdNiCuFe, AlNdNiCuCo,
Five yuan of high-entropy alloys of MgAgCuPdY, and the hexa-atomic high-entropy alloys of AlNiFeCrCoCu have it is high prolong plasticity and elevated temperature strength,
BCC or FCC solid solution are formed after soldering, can effectively reduce soldering interface residual stress, improves strength of joint.Wherein
AlNiCu fusing points are 1069.80 DEG C；Al15Nd60Ni10Cu10Fe5Fusing point is 1037.13 DEG C, Al11Nd61Ni8Cu15Co5Fusing point is
1043.18℃、Mg65Ag5Cu15Pd5Y10Fusing point is 812.64 DEG C etc.；Al1.8-2.8NiFeCrCoCu fusing points are 1090.21-
1268.22 DEG C, meet ceramics and the temperature range of metallic high temperature soldering.This patent focal selection is closed using the high entropys of ternary AlNiCu
Gold is illustrated.
The compound high-entropy alloy solder of the present invention, is formed, upper strata is high-entropy alloy layer, and lower floor is active titanium layer by two layers.
The method of a kind of compound high-entropy alloy solder ceramic soldering and metal of the present invention, is to carry out according to the following steps：
Steady
Behind ceramic and metal surface to be welded and AlNiCu high-entropy alloys foil and the titanium foil pretreatment prepared, it is placed in
Cleaned in acetone using ultrasonic wave, to remove the greasy dirt and impurity of matrix and solder surface.And solder is placed in alcohol and preserved,
Avoid polluting.
Two assemblings
Lower floor's solder, upper strata solder and metal to be welded are up sequentially placed from ceramic surface to be welded, forms a sandwich
Structure (see accompanying drawing 1), and apply on braze-welded structure 0.01-0.03MPa pressure, ensure while fixed sandwich structure multiple
Solder layer is closed fully to contact with matrix.
Three solderings
Assembly parts in step 3 are placed in diffusion in vacuum stove, vacuum is less than 5.0 × 10-3After Pa, with 10 DEG C/min liter
Warm speed rises to 900 DEG C, is incubated 10min, then rises to 1100 DEG C with same programming rate, after being incubated 10-30min, cut-out
Power supply, after cooling to room temperature with the furnace, sample is taken out, completes soldering.
In such scheme, solder used is foil shape AlNiCu high-entropy alloys and titanium foil, and the thickness of AlNiCu foils is 50-
100 μm, the thickness of titanium foil is 50-100 μm.Width is 5mm.
In such scheme, used ceramics can be oxide ceramics, nitride ceramics and carbide ceramics.
In such scheme, oxide ceramics can be Al2O3Ceramics, ZrO2Ceramics etc.；Nitride ceramics can be Si3N4Pottery
Porcelain, AlN ceramic；Carbide ceramics can be SiC ceramic, WC ceramics etc..
In such scheme, metal can be stainless steel, titanium alloy etc..
In such scheme, the mass fraction of Cu, Ni, Al in step 1 are respectively：43.0%, 38.9%, 18.1%
In such scheme, in step 1 AlNiCu high-entropy alloys use the purity 99.0% of copper raw material, nickel raw material it is pure
Degree 99.5%, the purity of aluminum feedstock are 99.2%.The purity of titanium material is 99.6%.
In such scheme, substrate pretreated method is in step 2：Using 400 mesh, 600 mesh, 800 mesh water-proof abrasive paper pair
Matrix welding surface is polished, and the diamond grinding fluid for reusing 0.5M is processed by shot blasting, is finally placed in acetone and is utilized
Ultrasonic wave cleans 20min, dried for standby.
Beneficial effects of the present invention are compared with prior art：
Using high-entropy alloy solder system, under the high entropy of mixing change effect of system, by several physical chemistry compatibilities compared with
The high-entropy alloy of good element composition only generates one or more of solid solution phases, solves active element and mother metal in solder system
The directly problem of reaction generation weld metal zone brittle intermetallic thing.
The present invention is simple to operate, does not have to carry out any surface modification treatment to substrate surface before soldering.Cycle is short, efficiency
It is high.The soldering of multiple products can be carried out simultaneously, beneficial to batch production.
Brief description of the drawings
Fig. 1 is the brazed coupon installation diagram in specific implementation, and wherein A is metal, and B is high-entropy alloy foil, and C is active titanium
Paper tinsel, D are ceramics.
Fig. 2 is the soldering processes curve in specific implementation.
Embodiment
Embodiment 1
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the ceramic mother metal of selection is ZrO2Ceramics, examination
Sample ruler cun is 5 × 5 × 10mm, metal Ti-6Al-4V, and specific composition is：Al6.0%, V3.5%, remaining is Ti.Sample chi
Very little is 10 × 10 × 30mm, and high-entropy alloy AlNiCu foils thickness is 100 μm, and the thickness of titanium foil is 50 μm.Width is 5mm.
After ceramics to be welded are polished with the water-proof abrasive paper of 400 mesh, 600 mesh, 800 mesh respectively with titanium alloy substrate, then use
0.5M diamond grinding fluid is processed by shot blasting to matrix, is placed in acetone with cleaning 20min in ultrasonic wave, dried for standby,
High-entropy alloy foil and titanium foil are placed in acetone and clean 20min, removes the greasy dirt and impurity on solder surface, dried for standby.
After treated matrix and compound high entropy solder foil assembling, apply 0.01MPa pressure on metal, with
Ensure that matrix is in close contact with composite soldering foil.
Braze-welded structure is placed in diffusion in vacuum stove, when vacuum is less than 5.0 × 10 in stove-3After Pa, with 10 DEG C/min's
Pre-incubation 10min after programming rate rises to 900 DEG C, then risen to same programming rate after 1100 DEG C and be incubated 10min, afterwards with stove
Room temperature is cooled to, completes ZrO2The connection of ceramics and Ti-6Al-4V.
Result of the test shows that experiment realizes ZrO2Effective connection of ceramics and Ti-6Al-4V alloys.Interface Microstructure is allusion quotation
FCC the and BCC solid solution tissues of type, joint room temperature shear strength are 91.7MPa.
Embodiment 2
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the ceramic mother metal of selection is Si3N4Ceramic sample
Chi is 5 × 5 × 10mm, metal is 304 stainless steels.Specimen size is 10 × 10 × 30mm, high-entropy alloy AlNiCu foil thickness
For 100 μm, titanium foil thickness is 50 μm.Width is 5mm.
After ceramics to be welded are polished with the water-proof abrasive paper of 400 mesh, 600 mesh, 800 mesh respectively with 304 stainless steels, then use 0.5M
Diamond grinding fluid matrix is processed by shot blasting, be placed in acetone with cleaning 20min, dried for standby in ultrasonic wave.By height
Entropy Alloy Foil band and titanium foil, which are placed in acetone, cleans 20min, removes the greasy dirt and impurity on solder surface, dried for standby.
After treated matrix and compound high entropy brazing filler metal alloy foil assembling, apply 0.02MPa pressure on metal
Power, to ensure that matrix is in close contact with composite soldering foil.
Braze-welded structure is placed in diffusion in vacuum stove, when vacuum is less than 5.0 × 10 in stove-3After Pa, with 10 DEG C/min's
Pre-incubation 10min is risen to after 1100 DEG C with same programming rate be incubated 30min again after programming rate rises to 900 DEG C, afterwards with stove
Room temperature is cooled to, completes Si3N4The connection of ceramic 304 stainless steels.
Result of the test shows, realizes Si3N4Effective connection of ceramics and 304 stainless steels, Interface Microstructure is typical FCC
With BCC solid solution tissues, room temperature shear strength has reached 72.6MPa.
Embodiment 3
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the ceramic mother metal of selection is Al2O3Ceramic sample chi
For 5 × 5 × 10mm, metal Ti-6Al-4V, specific composition is：Al6.0%, V3.5%, remaining is Ti.Specimen size is 10
× 10 × 30mm, the thickness of high-entropy alloy AlNiCu foils is 100 μm, and titanium foil thickness is 50 μm.Width is 5mm.
By Al to be welded2O3Ceramics are with Ti-6Al-4V alloys respectively with after the water-proof abrasive paper polishing of 400 mesh, 600 mesh, 800 mesh
Matrix is processed by shot blasting with 0.5M diamond grinding fluid again, is placed in acetone with 20min is cleaned in ultrasonic wave, drying is treated
With, high-entropy alloy foil and titanium foil are placed in acetone and clean 20min, the greasy dirt and impurity on removing solder surface, dried for standby.
After treated matrix and compound high entropy brazing filler metal alloy foil assembling, apply 0.02MPa pressure on part,
To ensure that matrix is in close contact with composite soldering foil.
Braze-welded structure is placed in diffusion in vacuum stove, when vacuum is less than 5.0 × 10 in stove-3After Pa, with 10 DEG C/min's
Pre-incubation 10min is risen to after 1100 DEG C with same programming rate be incubated 30min again after programming rate rises to 900 DEG C, afterwards with stove
Room temperature is cooled to, completes Al2O3The connection of ceramic Ti-6Al-4V alloys.
Result of the test shows, realizes Al2O3Effective connection of ceramics and Ti-6Al-4V alloys.Interface Microstructure type is allusion quotation
FCC the and BCC solid solution of type, shearing strength of joint have reached 80.6MPa.
Embodiment 4
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 1, difference is what is applied
Pressure is 0.02MPa, when temperature rises to 1100 DEG C, soaking time 10min.
Obtain ZrO2The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 81.3MPa.
Embodiment 5
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the pressure applied with embodiment 1, difference
For 0.02MPa, when temperature rises to 1100 DEG C, soaking time 20min.
Obtain ZrO2The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 74.5MPa.
Embodiment 6
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the pressure applied with embodiment 1, difference
For 0.02MPa, when temperature rises to 1100 DEG C, soaking time 30min.
Obtain ZrO2The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 76.8MPa.
Embodiment 7
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 1, difference is what is applied
Pressure is 0.03MPa, when temperature rises to 1100 DEG C, soaking time 10min.
Obtain ZrO2The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 68.5MPa.
Embodiment 8
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the pressure applied with embodiment 1, difference
For 0.03MPa, when temperature rises to 1100 DEG C, soaking time 20min.
Obtain ZrO2The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 73.9MPa.
Embodiment 9
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the pressure applied with embodiment 1, difference
For 0.03MPa, when temperature rises to 1100 DEG C, soaking time 30min.
Obtain ZrO2The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 69.9MPa.
Embodiment 10
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the pressure applied with embodiment 2, difference
0.01MPa, when temperature rises to 1100 DEG C, soaking time 20min.
Obtain Si3N4The joint of ceramics/Ti/AlNiCu/304 stainless steels, its room temperature shear strength are 69.2MPa.
Embodiment 11
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the pressure applied with embodiment 2, difference
For 0.03MPa, when temperature rises to 1100 DEG C, soaking time 30min.
Obtain Si3N4The joint of ceramics/Ti/AlNiCu/304 stainless steels, its room temperature shear strength are 77.9MPa.
Embodiment 12
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the pressure applied with embodiment 2, difference
For 0.03MPa, when temperature rises to 1100 DEG C, soaking time 20min.
Obtain Si3N4The joint of ceramics/Ti/AlNiCu/304 stainless steels, its room temperature shear strength are 81.5MPa.
Embodiment 13
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, the pressure applied with embodiment 3, difference
For 0.01MPa, when temperature rises to 1100 DEG C, soaking time 10min.
Obtain Al2O3The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 64.8MPa.
Embodiment 14
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 3, difference is what is applied
Pressure is 0.03MPa, when temperature rises to 1100 DEG C, soaking time 20min.
Obtain Al2O3The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 63.4MPa.
Embodiment 15
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 1, is a difference in that high-entropy alloy
The thickness of foil is 80 μm, and the thickness of titanium foil is 80 μm.
Obtain ZrO2The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 67.3MPa.
Embodiment 16
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 2, is a difference in that high-entropy alloy
The thickness of foil is 80 μm, and the thickness of titanium foil is 80 μm.
Obtain Si3N4The joint of ceramics/Ti/AlNiCu/304 stainless steels, its room temperature shear strength 74.3MPa.
Embodiment 17
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 3, is a difference in that high-entropy alloy
The thickness of foil is 80 μm, and the thickness of titanium foil is 80 μm.
Obtain Al2O3The joint of ceramics/Ti/AlNiCu/Ti-6Al-4V alloys, its room temperature shear strength are 51.6MPa
Embodiment 18
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 2, it is a difference in that pottery used
Porcelain is SiC ceramic.
The joint of SiC ceramic/Ti/AlNiCu/304 stainless steel alloys is obtained, its room temperature shear strength is 64.9MPa.
Embodiment 19
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 1, it is a difference in that high entropy used
Alloy is Al15Nd60Ni10Cu10Fe5。
Obtain ZrO2Ceramics/Ti/Al15Nd60Ni10Cu10Fe5The joint of/Ti-6Al-4V alloys, its room temperature shear strength are
61.7MPa。
Embodiment 20
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 1, it is a difference in that high entropy used
Alloy is Mg65Ag5Cu15Pd5Y10。
Obtain ZrO2Ceramics/Ti/Mg65Ag5Cu15Pd5Y10The joint of/Ti-6Al-4V alloys, its room temperature shear strength are
59.5MPa。
Embodiment 21
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 1, it is a difference in that high entropy used
Alloy is Al11Nd61Ni8Cu15Co5。
Obtain ZrO2Ceramics/Ti/Al11Nd61Ni8Cu15Co5The joint of/Ti-6Al-4V alloys, its room temperature shear strength are
72.7MPa。
Embodiment 22
A kind of method of compound high-entropy alloy solder ceramic soldering and metal, with embodiment 1, it is a difference in that high entropy used
Alloy is Al1.8NiFeCrCoCu。
Obtain ZrO2Ceramics/Ti/Al1.8The joint of NiFeCrCoCu/Ti-6Al-4V alloys, its room temperature shear strength are
66.1MPa。
This patent is not limited to lift ceramet and corresponding high entropy system in text, and researcher can be according to specific
Matrix is connected, to select optimal high entropy system alloy proportion.
Claims (5)
1. a kind of method of compound high-entropy alloy solder ceramic soldering and metal, it is characterised in that braze-welded structure is a sandwich
Structure, upper strata are metal, and centre is composite soldering layer, and lower floor is ceramics；
Composite soldering layer is formed by two layers, and upper strata is high-entropy alloy foil, and lower floor is titanium foil；The thickness of upper strata high-entropy alloy foil
For 50-100 μm, the thickness of lower floor's titanium foil band is 50-100 μm；
High-entropy alloy includes AlNiCu ternarys high-entropy alloy, Al15Nd60Ni10Cu10Fe5Five yuan of high-entropy alloys,
Al11Nd61Ni8Cu15Co5Five yuan of high-entropy alloys, Mg65Ag5Cu15Pd5Y10Five yuan of high-entropy alloys or/and Al1.8-2.8NiFeCrCoCu
Hexa-atomic high-entropy alloy.
2. according to the method for claim 1, it is characterised in that：Metal is stainless steel or titanium alloy.
3. according to the method for claim 1, it is characterised in that：Used ceramics are oxide ceramics, nitride ceramics
Or carbide ceramics.
4. according to the method for claim 3, it is characterised in that：Oxide ceramics is Al2O3Ceramics, ZrO2Ceramics；Nitride
Ceramics are Si3N4Ceramics, BN ceramics, AlN ceramic；Carbide ceramics is SiC ceramic, WC ceramics.
5. according to the method for claim 1, it is characterised in that specifically soldering processes are：Brazing member is placed in diffusion in vacuum stove
In, the application 0.01-0.03MPa pressure on brazing member, when vacuum is less than 5.0 × 10-3After Pa, with 10 DEG C/min heating
Speed rises to 900 DEG C, is incubated 10min, then rises to 1100 DEG C with same programming rate, after being incubated 10-30min, cut-out electricity
Source, after cooling to room temperature with the furnace, sample is taken out, completes soldering.
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| CN110919232A (en) * | 2019-12-31 | 2020-03-27 | 华北水利水电大学 | Gold-based high-entropy brazing filler metal |
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| CN114951873A (en) * | 2022-06-14 | 2022-08-30 | 浙江亚通焊材有限公司 | Composite solder containing high-entropy alloy and method for connecting AlN and Cu through brazing |
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