CN108907500A - A kind of high temperature auri active solder and preparation method thereof - Google Patents
A kind of high temperature auri active solder and preparation method thereof Download PDFInfo
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- CN108907500A CN108907500A CN201810876173.8A CN201810876173A CN108907500A CN 108907500 A CN108907500 A CN 108907500A CN 201810876173 A CN201810876173 A CN 201810876173A CN 108907500 A CN108907500 A CN 108907500A
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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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3013—Au as the principal constituent
-
- 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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0233—Sheets, foils
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
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Abstract
A kind of high temperature auri active solder, the solder are AuNiPdCrVMo alloy, wherein Ni 30~37wt%, Pd 3~10wt%, Cr 1.0~5.0wt%, V 1.0~5.0wt%, Mo 1.0~2.0wt%, Au surplus.It is prepared using discharge plasma sintering technique.The solder is suitble to Si3N4The connection of ceramic high temperature activity, has high activity, low-expansion coefficient, has good elevated temperature strength after welding.It solves V, Cr, Mo element to be difficult to be added in AuNi alloy, the problems such as generating gross segregation, uneven chemical components in the alloy, and the difference of linear expansion for solving metal material and ceramics is larger, leads to solder and the unmatched phenomenon of ceramics after welding.
Description
Technical field
The present invention relates to a kind of AuNiPdCrVMo high temperature active solders and preparation method thereof, which is mainly used in electricity
The Si of sub-information industry3N4The connection of ceramic high temperature activity, belongs to field of welding material.
Background technique
With the development of electronic information industry, the especially development in Aeronautics and Astronautics field, the performance of traditional metal materials is
It is unable to satisfy engineering development demand, such as its high temperature resistance, antioxygenic property, corrosion resistance etc..Ceramic material
With its excellent high temperature resistant, creep resistant and anti-oxidant, corrosion-resistant, wear-resistant, a series of excellent performances such as high rigidity are in state
It is used widely in the fields such as anti-, aerospace, the energy, automobile, electronics.Wherein Si3N4Ceramics have high intensity, high rigidity, resistance to
Mill property and its excellent mechanical behavior under high temperature and thermal stability, one of the structural ceramics as most application prospect.But
Si3N4The brittleness of ceramics is big, ductility is low, the disadvantages of being unlikely to deform, and the component for making it be difficult to manufacture into complicated shape constrains it
Extensive use in engineering.
Active metal brazing technology is simple with its operating method, cost of investment is low, size adaptability is good, and bonding strength
The advantages that height, experimental repeatability is good, is widely used in ceramic component connection.Currently, being suitable for Si3N4The pricker of ceramic active connection
Material is mainly based on AgCuTi solder alloy, and joint mechanical property is excellent, and room temperature bending resistance can reach 550MPa or more,
But the use temperature of its connector is usually no more than 500 DEG C, limits such connector and uses in a high temperauture environment.It researchs and develops
A kind of suitable Si3N4Ceramic high temperature activity connects the auri solder used, has important practical application value.
The preparation of existing high temperature auri brazing material is usually using solid phase alloying, that is, with high-energy mills or ball milling
Machine is ground metal powder, so that powder is subjected to deformation repeatedly, cold welding, broken, to reach atom water between element
Flat alloying, also referred to as mechanical alloying.It is mostly physical mixed, the intermetallic compound of formation between the solder metal of this method preparation
It is less, therefore fusion temperature is uneven.
Discharge plasma sintering technique has heating rate is fast, sintering time is short, sintering is high-efficient, sintering process is simple etc.
Feature is usually applied to prepare functional material, and preparing the application in solder, there is not been reported.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of AuNiPdCrVMo active solder, and it is suitable to have
Active, good spreading property and lower linear expansion coefficient are suitble to Si3N4The activity connection of ceramics, and it is brazed rear joint
With good mechanical behavior under high temperature.Meanwhile the preparation method that the present invention provides the solder is solved using conventional sintering process
Leading to the problem of gross segregation in alloy when adding Cr, V, Mo in AuNi base-material leads to uneven components.
To achieve the above object, the present invention uses following technical scheme：
A kind of high temperature auri active solder, the solder are AuNiPdCrVMo alloy, wherein Ni 30~37wt%, Pd 3
~10wt%, Cr 1.0~5.0wt%, V 1.0~5.0wt%, Mo 1.0~2.0wt%, Au surplus.
High temperature auri active solder as described above, it is preferable that the 31~35wt% of Ni, Pd 5~8wt%, Cr
1.0~3.0wt%, V 4.0~5.0wt%, Mo 1.0~1.5wt%, Au surplus.
On the other hand, the present invention provides a kind of preparation method of high temperature auri active solder, and this approach includes the following steps：
I. the Pd that Ni powder, granularity that Au powder, granularity that granularity is 50-100 μm are 50-100 μm are 50-100 μm is filtered out
The Mo powder that V powder that Cr powder that powder, granularity are 20-30 μm, granularity are 20-30 μm, granularity are 10-20 μm；
II. Au powder, Ni powder described in step I, Pd powder, Cr powder, V powder and Mo powder are subjected to mechanical alloying in the ball mill
Processing, mass percent are：Ni powder 30%-37%, Pd powder 3%-10%, Cr powder 1.0%-5.0%, V powder 1.0%-5.0%,
Mo powder 1.0%-2.0%, bronze surplus, mechanical alloying time are 120~180 minutes；
III. by mixed-powder obtained in step II in H2Reduction treatment is carried out in protective atmosphere；
IV. the mixed-powder obtained after step III reduction is sintered in discharge plasma sintering furnace mold, sintering ginseng
Number is：Pressure 30-50MPa, 1050-1080 DEG C of temperature, 130-150 DEG C of heating rate/min, sintering time 1-5min, atmosphere are
Then vacuum cools to room temperature with the furnace, obtain AuNiPdCrVMo alloy blank.
Preparation method as described above, it is preferable that Ni 31~35wt%, Pd 5~8wt%, Cr in the step II
1.0~3.0wt%, V 4.0~5.0wt%, Mo 1.0~1.5wt%, Au surplus.
Preparation method as described above, it is preferable that it further include cold working step after step IV, i.e., it will be in step IV
It is sintered obtained AuNiPdCrVMo alloy blank surface to be handled, removes the graphite flake on surface layer, then carry out cold rolling processing,
Obtain the AuNiPdCrVMo alloy sheet material with a thickness of 0.15~2.0mm.
Preparation method as described above, it is preferable that the Au powder purity used in the step I is greater than 99.99wt%, Ni powder
Purity is greater than 99.99wt%, Pd powder purity and is greater than greater than 99.99wt%, Cr powder purity greater than 99.99wt%, V powder purity
99.99wt% and Mo powder purity is greater than 99.99wt%.
Preparation method as described above, it is preferable that in the step II, rotational speed of ball-mill 50-100r/min.
Preparation method as described above, it is preferable that in the step III, mixed-powder is in H2300 DEG C -500 is carried out in furnace
DEG C, the reduction treatment of heat preservation 3-5 hours.
Another aspect, the present invention provide a kind of high temperature auri activity brazing material, which is using method system as described above
Standby.
In another aspect, the present invention provides high temperature auri activity brazing material as described above in Si3N4Application in ceramic welding.
Pd, Cr, V, Mo is added in AuNiPdCrVMo solder of the invention on the basis of AuNi, prepares even tissue and is suitble to
Si3N4Ceramic high temperature activity connects the solder alloy used.Wherein, alloy and Si can be improved in Cr, V active element3N4Ceramics
Alloy and Si can be improved in binding force, Pd element3N4Wettability, mechanical strength and the mechanical behavior under high temperature of ceramics, Mo element can
To drop low-alloyed linear expansion coefficient.Meanwhile the Pd of too high amount will affect the mechanical strength and mechanical behavior under high temperature of solder；It crosses
Cr, V, Mo of high-content are difficult to dissolve each other with alloy, will increase the brittleness of solder, influence the welding performance of solder.Pricker of the invention
Each ingredient mutually restricts the properties of joint effect solder, the AuNiPdCrVMo alloy pricker of the component content in material alloy
Material is in soldering Si3N4Good wetability, higher joint mechanical strength, elevated temperature strength and appropriate are shown in the application of ceramics
The coefficient of expansion.
However, can not obtain AuNiPdCrVMo alloy using traditional founding+milling method, technical difficulty is：1)
Cr, V, Mo are difficult to the alloy cpd with base metallization symphysis at target content；2) gross segregation of Cr, V, Mo in the alloy
Seriously, uneven chemical components.The method that the present invention is combined using mechanical alloying+discharge plasma sintering technique, is prepared
The uniform AuNiPdCrVMo solder alloy of ingredient.In mechanical alloying step, the granularity selection of metal powder ensure that subsequent
The compactness of alloy sintering, granularity is bigger than normal or the compactness less than normal for being unfavorable for subsequent alloy sintering, leads to following process mistake
Alloy cracks or is not capable of processing in journey.During discharge plasma sintering, pass through point discharge effect, powder particle surface
Oxidation film abolished, particle surface is activated, and intergranular diffusion is strengthened, and is made existing solid between metal powder
Diffusion also has alloying reaction, while accelerating the process of densification.The control of discharge plasma sintering temperature 1050~
1080 DEG C, close to pure gold fusing point, the liquid phase that sub-fraction is had in sintering process the temperature occurs, realizes liquid-phase sintering, mentions
The high consistency of material, is conducive to subsequent machine-shaping.
The beneficial effects of the present invention are the following aspects：
1. the alloy sheet material can directly weld Si3N4Ceramics, ceramic surface are not necessarily to nickel plating, meet electronics and information industry
Use demand.
2. the solder is for welding Si3N4Ceramic wetability is good, and sprawling angle is about 17 °.
3. the solder is for welding Si3N4Ceramics, bending strength reaches 253MPa, bending strength under 500 DEG C of high temperature under room temperature
Reach 156MPa, the Si of welding3N4Ceramics can be used in the case where being higher than 500 DEG C of environment.
4. the linear expansion coefficient of alloy of the present invention is 12 × 10-6K-1, make ceramics with metal be directly connected to after internal stress
It is lower, it avoids leading to Joint Cracking since stress is excessive after connecting.
5. the present invention prepares AuNiPdCrVMo solder alloy sheet material, V in alloy using discharge plasma sintering technique for the first time
Content, which can achieve 5.0%, Cr content and can achieve 5.0%, Mo content, can achieve 2.0%, and alloy may finally be processed into
With a thickness of the sheet material of 0.15mm.
6. the consistency of the alloy material reaches 99% or more.
7. preparing AuNiPdCrVMo alloy using discharge plasma sintering technique, sintering time is short, and heating rate is fast, can
Grain coarsening is significantly inhibited, tiny, uniform tissue can be obtained, is convenient for subsequent cold working.Using random dispersion sampling side
Method carries out composition detection to the auri high-temp solder, and ingredient is uniform.
8. preparing AuNiPdCrVMo alloy using discharge plasma sintering technique, preparation process is simple, and production procedure is short.
9. there is the higher V element of content in alloy, so that alloy activity with higher, it can direct welding ceramics.
Detailed description of the invention
Fig. 1 is to weld Si using AuNiPdCrVMo alloy finished product obtained in embodiment 13N4After ceramics, Solder Spread in
The photo of ceramic surface.
Specific embodiment
Embodiment 1
(1) it is greater than Au powder, Ni powder, Pd powder, Cr powder, V powder and the Mo powder of 99.99wt% using purity, wherein Au powder, Ni
Powder, Pd dressing sieve select particle of the granularity between 50 μm -100 μm, and Cr powder and V Powder Particle Size select 20-30 μm, and Mo Powder Particle Size is selected
10-20μm。
(2) according to mass percent be 32% pure Ni powder, 5% pure Pd powder, 1% pure Cr powder, 5% pure V powder and
1.0% pure Mo powder, pure Au powder are that surplus carries out mixing and ball milling, and Ball-milling Time is 120 minutes.
(3) alloyed powder after mixing and ball milling is heated in hydrogen shield atmosphere 500 DEG C, 3 hours is kept the temperature, to alloyed powder
Carry out reduction treatment.
(4) mixed powder is put into discharge plasma sintering furnace (the SE-607 discharge plasma sintering that German FCT company produces
Furnace) in be sintered obtained AuNiPdCrVMo alloy blank, wherein sintering temperature be 1050 DEG C, sintering pressure 50MPa, heating
Speed is 150 DEG C/min, keeps the temperature 5min, and atmosphere is vacuum, and the sotck thinkness of acquisition is 8mm.
(5) sintered AuNiPdCrVMo alloy blank surface is handled, using milling machine by the graphite of blank surface
It cleans out, until blank surface is metal surface entirely, until graphite.
(6) cold rolling processing+vacuum annealing process is carried out to AuNiPdCrVMo alloy blank, annealing temperature is 650 DEG C, is added
Work is to 0.15mm, surface-brightening zero defect.
The solder of acquisition carries out random dispersion sampling, carries out composition detection, detection knot with chemical titration analysis method
Fruit is：Ni (32 ± 0.05) %, Pd (5.0 ± 0.02) %, Cr (1.0 ± 0.02) %, V (5.0 ± 0.02) %, Mo (1.0 ±
0.02) %, Au surplus.Illustrate the solder alloy even tissue, the gross segregation of no Cr, V, Mo in the alloy.
The consistency of the solder is 99.9%, and linear expansion coefficient is 12 × 10-6K-1.It is welded using the solder
Si3N4Ceramics, 1200 DEG C of brazing temperature, bending strength is 253MPa under obtained welding point room temperature, is bent under 500 DEG C of high temperature
Intensity is 156MPa.Fig. 1 is to weld Si using the AuNiPdCrVMo alloy3N4After ceramics, Solder Spread is in the photograph of ceramic surface
Piece.It can be seen that wetting effect is good, meet welding need, angle of wetting is 17 °.
Embodiment 2
The process conditions of the present embodiment are same as Example 1, are only changed to the mass percent of Ni powder in alloyed powder
35.0%, the mass percent that the mass percent of Pd powder is changed to 6.0%, Cr powder is changed to the quality percentage of 2.0%, V powder
It is surplus that mass percent than being changed to 4.0%, Mo powder, which is changed to 1.5%, Au powder,.Obtained AuNiPdCrVMo alloy
The consistency of blank is 99.9%, and linear expansion coefficient is 11 × 10-6K-1.Si is welded using the solder3N4Ceramics, soldering temperature
1200 DEG C are spent, bending strength is 233MPa under obtained welding point room temperature, and bending strength is 165MPa under 500 DEG C of high temperature.Weldering
It connects and works well, angle of wetting is 17 °.
Embodiment 3
The process conditions of the present embodiment are same as Example 1, are only changed to the mass percent of Ni powder in alloyed powder
33.0%, the mass percent that the mass percent of Pd powder is changed to 8.0%, Cr powder is changed to the quality percentage of 3.0%, V powder
It is surplus that mass percent than being changed to 4.0%, Mo powder, which is changed to 1.3%, Au powder,.Obtained AuNiPdCrVMo alloy
The consistency of blank reaches 99.9%, is worked into 0.15mm, surface-brightening zero defect.Solder linear expansion coefficient be 12 ×
10-6K-1, the solder prepared using above-mentioned technique, welding Si3N4Ceramics, bending strength is 229MPa, 500 DEG C of height under room temperature
The lower bending strength of temperature is 138MPa.
Embodiment 4
The process conditions of the present embodiment are same as Example 1, are only modified the related process parameters of sintering, wherein burning
Junction temperature is 1080 DEG C, sintering pressure 30MPa, and heating rate is 130 DEG C/min, keeps the temperature 1min, atmosphere is vacuum.Using this work
AuNiPdCrVMo alloy blank consistency made from skill can achieve 99.9%.It is worked into 0.15mm, surface-brightening zero defect.
Solder linear expansion coefficient is 11 × 10-6K-1, the solder prepared using above-mentioned technique, welding Si3N4Ceramics, under room temperature
Bending strength is 202MPa, and bending strength is 129MPa under 500 DEG C of high temperature.
The implementation of AuNiPdCrVMo alloy material of the present invention and preparation method thereof part is only enumerated in above-described embodiment
Example, in the technical solution of aforementioned present invention：Described alloying component, sintering temperature, sintering pressure, sintering rate etc. are providing
In range can unrestricted choice, will not enumerate herein, thus it is above to illustrate that included technical solution should be regarded as illustrative, and
The non-protection scope to limit the present patent application patent.
Claims (10)
1. a kind of high temperature auri active solder, which is characterized in that the solder is AuNiPdCrVMo alloy, wherein Ni 30~
37wt%, Pd 3~10wt%, Cr 1.0~5.0wt%, V 1.0~5.0wt%, Mo 1.0~2.0wt%, Au surplus.
2. high temperature auri active solder as described in claim 1, which is characterized in that the 31~35wt% of Ni, Pd 5~
8wt%, Cr 1.0~3.0wt%, V 4.0~5.0wt%, Mo 1.0~1.5wt%, Au surplus.
3. a kind of preparation method of high temperature auri active solder, which is characterized in that this approach includes the following steps：
I. the Pd powder, grain that Ni powder, granularity that Au powder, granularity that granularity is 50-100 μm are 50-100 μm are 50-100 μm are filtered out
Spend the Mo powder that the Cr powder for being 20-30 μm, the V powder that granularity is 20-30 μm, granularity are 10-20 μm；
II. Au powder, Ni powder described in step I, Pd powder, Cr powder, V powder and Mo powder are carried out at mechanical alloying in the ball mill
Reason, mass percent are：Ni powder 30%-37%, Pd powder 3%-10%, Cr powder 1.0%-5.0%, V powder 1.0%-5.0%, Mo
Powder 1.0%-2.0%, bronze surplus, mechanical alloying time are 120~180 minutes；
III. by mixed-powder obtained in step II in H2Reduction treatment is carried out in protective atmosphere；
IV. the mixed-powder obtained after step III reduction is sintered in discharge plasma sintering furnace mold, sintering parameter
For：Pressure 30-50MPa, 1050-1080 DEG C of temperature, 130-150 DEG C of heating rate/min, sintering time 1-5min, atmosphere are true
Then sky cools to room temperature with the furnace, obtain AuNiPdCrVMo alloy blank.
4. preparation method as claimed in claim 3, which is characterized in that Ni 31~35wt%, Pd 5 in the step II~
8wt%, Cr 1.0~3.0wt%, V 4.0~5.0wt%, Mo 1.0~1.5wt%, Au surplus.
5. preparation method as described in claim 3 or 4, which is characterized in that it further include cold working step after step IV,
The AuNiPdCrVMo alloy blank surface being sintered in step IV is handled, removes the graphite flake on surface layer, with laggard
Row cold rolling processing, obtains the AuNiPdCrVMo alloy sheet material with a thickness of 0.15~2.0mm.
6. preparation method as described in claim 3 or 4, which is characterized in that the Au powder purity used in the step I is greater than
99.99wt%, Ni powder purity are greater than 99.99wt%, Pd powder purity and are greater than 99.99wt%, Cr powder purity greater than 99.99wt%, V
Powder purity is greater than 99.99wt% and Mo powder purity and is greater than 99.99wt%.
7. preparation method as described in claim 3 or 4, which is characterized in that in the step II, rotational speed of ball-mill 50-100r/
min。
8. preparation method as described in claim 3 or 4, which is characterized in that in the step III, mixed-powder is in H2In furnace into
300 DEG C -500 DEG C of row, the reduction treatment of heat preservation 3-5 hours.
9. a kind of high temperature auri activity brazing material, which is characterized in that the solder is using side described in any one of claim 3-8
Method preparation.
10. application of the high temperature auri activity brazing material as claimed in claim 9 in Si3N4 ceramic welding.
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Cited By (1)
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