CN108118178A - A kind of in-situ synthesis of boride titanium-titanium carbide complex phase ceramic enhancing Cu-base composites and its preparation method and application - Google Patents
A kind of in-situ synthesis of boride titanium-titanium carbide complex phase ceramic enhancing Cu-base composites and its preparation method and application Download PDFInfo
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- CN108118178A CN108118178A CN201711397493.7A CN201711397493A CN108118178A CN 108118178 A CN108118178 A CN 108118178A CN 201711397493 A CN201711397493 A CN 201711397493A CN 108118178 A CN108118178 A CN 108118178A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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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
- B23K11/00—Resistance welding; Severing by resistance heating
- B23K11/30—Features relating to electrodes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0005—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The present invention provides a kind of fabricated in situ TiB2The method that TiC complex phase ceramics enhance Cu-base composites, comprises the following steps:Titanium simple substance and boron carbide are subjected to ball milling, obtain TiB2TiC complex phase ceramic presomas;In the TiB2The surface of TiC complex phase ceramic presomas carries out chemical nickel plating, obtains nickel wetting enhancing particle;The nickel is soaked into enhancing particle and copper source mixing and ball milling, obtains ball milling mixing material;The ball milling mixing material is cold-pressed, obtains green compact;The green compact is sintered in an oxygen-free atmosphere, obtains sintered body;The sintered body is forged and pressed, obtains fabricated in situ TiB2TiC complex phase ceramics enhance Cu-base composites.The higher fabricated in situ TiB of hardness performance can be prepared in preparation method provided by the invention2TiC complex phase ceramics enhance Cu-base composites.
Description
Technical field
The invention belongs to metal-base composites technical field, more particularly to a kind of fabricated in situ TiB2- TiC complex phases are made pottery
Porcelain enhancing Cu-base composites and its preparation method and application.
Background technology
Resistance spot welding is be unable to do without during automobile production, production motor passenger vehicle needs to weld 3000 points/, and production car then needs
Want 7000~12000 points/;The spot welding cost of any reaches 150 dollars by 5 cents of calculating, the spot welding cost of motor passenger vehicle, sedan-chair
The spot welding cost of vehicle then reaches 350~600 dollars, accounts for the 1/2~3/4 of vehicle production cost, this promotes people constantly to study newly
Spot-wedling electrode material, to reduce the cost of spot welding during automobile production.
In pinpoint welding procedure, spot-wedling electrode is inevitably plastically deformed, spot welding under the action of mechanical force and heat
After electrode is plastically deformed, current density can be caused to reduce, reduce the Joule heat that electric current generates, finally influence quality of welding spot,
Therefore, plastic deformation becomes one of principal element of spot-wedling electrode failure.To inhibit the plastic deformation of spot-wedling electrode, extending it makes
With the service life, the component with reinforcing material wear-resisting property effect is applied to the preparation of spot-wedling electrode material by researcher.
TiC、TiB2One-component ceramic is relatively early by the enhancing phase as dispersion-strengtherning, is answered using what one-component ceramic enhanced
For pure copper material, wearability is improved condensation material, but improvement is unsatisfactory;Later, enhance mutually gradual
Develop into complex phase ceramic, TiB2- TiC is exactly a kind of widely used composite ceramics enhancing phase.It has excellent performance in order to obtain
TiB2- TiC complex phase ceramics enhance copper-based composite material, and researcher proposes SHS process, mechanical alloying etc.
Different preparation method, such as by TiB2, TiC directly mixes and adds in Copper substrate or by Ti, B4C is added in Copper substrate, is prepared into
TiB is arrived2- TiC complex phase ceramics enhance copper-based composite material.It is preferably multiple that although wearability can be prepared in the above method
Condensation material, but its hardness performance cannot still meet spot-wedling electrode and obtain demand to material wear-resistant performance.
The content of the invention
To solve the above problems, the present invention provides a kind of fabricated in situ TiB2- TiC complex phase ceramics enhance copper-based composite wood
Material and its preparation method and application, fabricated in situ TiB provided by the invention2- TiC complex phase ceramics enhance the side of Cu-base composites
The preferable composite material of wearability can be prepared in method.
In order to achieve the above object, the present invention provides following technical scheme:
The present invention provides a kind of fabricated in situ TiB2- TiC complex phase ceramics enhance the preparation method of Cu-base composites, bag
Include following steps:
1) titanium simple substance and boron carbide are subjected to ball milling, obtain TiB2- TiC complex phase ceramic presomas;
2) in the TiB2The surface of-TiC complex phase ceramic presomas carries out chemical nickel plating, obtains nickel wetting enhancing particle;
3) nickel is soaked into enhancing particle and copper source mixing and ball milling, obtains ball milling mixing material;
4) the ball milling mixing material is cold-pressed, obtains green compact;
5) green compact is sintered in an oxygen-free atmosphere, obtains sintered body;
6) sintered body is forged and pressed, obtains fabricated in situ TiB2- TiC complex phase ceramics enhance Cu-base composites.
Preferably, the molar ratio of the titanium simple substance and boron carbide is 3:1.
Preferably, in the step 1) speed of ball milling for 300~500r/min, time of ball milling for 12~for 24 hours.
Preferably, the temperature of the nickel plating solution of chemical nickel plating is 45~50 DEG C in the step 2), the nickel plating solution
PH value be 9~11.
Preferably, nickel wetting enhancing particle and the mass ratio in copper source are 0.5~5 in the step 3):95~99.
Preferably, the pressure of the step 4) cold pressing is 300~500MPa, and the time of cold pressing is 1~3min
Preferably, the temperature of sintering is 900~1050 DEG C in the step 5), and the time of sintering is 10~30min.
Preferably, the temperature of forging and stamping is 500~550 DEG C in the step 6).
The present invention also provides the fabricated in situ TiB that above-mentioned technical proposal the method is prepared2- TiC complex phase ceramics
Enhance Cu-base composites, including TiB2- TiC complex phase ceramics enhance phase, Copper substrate phase and are coated on the TiB2- TiC complex phases are made pottery
Porcelain enhances the nickel wetting phase of phase surface, the TiB of surface cladded with nickel wetting phase2- TiC complex phase ceramic Dispersion of Reinforcement is in Copper substrate
The inside and surface of phase.
Fabricated in situ TiB of the present invention2The method of-TiC complex phase ceramics enhancing Cu-base composites comprises the following steps:
Titanium simple substance and boron carbide are subjected to ball milling, obtain TiB2- TiC complex phase ceramic presomas;In the TiB2- TiC complex phase ceramic forerunners
The surface of body carries out chemical nickel plating, obtains nickel wetting enhancing particle;The nickel is soaked into enhancing particle and copper source mixing and ball milling, is obtained
To ball milling mixing material;The ball milling mixing material is cold-pressed, obtains green compact;The green compact is burnt in an oxygen-free atmosphere
Knot, obtains sintered body;The sintered body is forged and pressed, obtains fabricated in situ TiB2- TiC complex phase ceramics enhance copper-based composite wood
Material.It is of the invention first in TiB2- TiC complex phase ceramics enhancing plating nickel on surface, is then combined again with copper, using nickel improve enhancing phase with
Wetability between copper improves the combination power of enhancing phase core matrix phase, and the performance to enhance phase separation provides advantage, and then
Make gained composite material that there is higher hardness and wearability.Embodiment the result shows that, the method for the invention is prepared
Fabricated in situ TiB2- TiC complex phase ceramics enhancing Cu-base composites hardness (HV50g) reach more than 258, electrode life
Reach more than 1300 solder joints.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the copper product metallograph that comparative example 1 is prepared;
Fig. 2 is the carbon/carbon-copper composite material metallograph that comparative example 2 is prepared;
Fig. 3 is the carbon/carbon-copper composite material metallograph that comparative example 3 is prepared;
Fig. 4 is the fabricated in situ TiB that embodiment 1 is prepared2- TiC complex phase ceramics enhancing Cu-base composites metallographic shines
Piece;
Fig. 5 is the fabricated in situ TiB that embodiment 2 is prepared2- TiC complex phase ceramics enhancing Cu-base composites metallographic shines
Piece;
Fig. 6 is the fabricated in situ TiB that embodiment 3 is prepared2- TiC complex phase ceramics enhancing Cu-base composites metallographic shines
Piece;
Fig. 7 is the fabricated in situ TiB that embodiment 4 is prepared2- TiC complex phase ceramics enhancing Cu-base composites metallographic shines
Piece;
Fig. 8 is the fabricated in situ TiB that embodiment 5 is prepared2- TiC complex phase ceramics enhancing Cu-base composites metallographic shines
Piece;
Fig. 9 is spot-wedling electrode structural front view of the present invention;
Figure 10 be the material that is prepared of comparative example 1~3 and Examples 1 to 5 as spot-wedling electrode when electrode life unite
Meter figure.
Specific embodiment
The present invention provides a kind of fabricated in situ TiB2- TiC complex phase ceramics enhance the preparation method of Cu-base composites, bag
Include following steps:
1) titanium simple substance and boron carbide are subjected to ball milling, obtain TiB2- TiC complex phase ceramic presomas;
2) in the TiB2The surface of-TiC complex phase ceramic presomas carries out chemical nickel plating, obtains nickel wetting enhancing particle;
3) nickel is soaked into enhancing particle and copper source mixing and ball milling, obtains ball milling mixing material;
4) the ball milling mixing material is cold-pressed, obtains green compact;
5) green compact is sintered in an oxygen-free atmosphere, obtains sintered body;
6) sintered body is forged and pressed, obtains fabricated in situ TiB2- TiC complex phase ceramics enhance Cu-base composites.
Titanium simple substance and boron carbide are carried out ball milling by the present invention, obtain TiB2- TiC complex phase ceramic presomas.
In the present invention, the titanium simple substance provides preferably in the form of titanium valve, and the grain size of the titanium valve is preferably 100~
200 mesh, further preferably 120~200 mesh, more preferably 140~170 mesh.In the present invention, the grain size of the boron carbide is excellent
Elect 200~400 mesh as, further preferably 230~400 mesh.The present invention does not appoint the specific source of titanium simple substance and boron carbide
What particular determination, using commercial product well known to those skilled in the art.In the present invention, the titanium valve and boron carbide it is pure
Degree is preferably more than 99.99%.The present invention makes titanium and boron carbide fully connect preferably by controlling the grain size of titanium simple substance and boron carbide
It touches, to generate TiB2- TiC complex phase ceramics presoma provides condition.
In the present invention, the molar ratio of the titanium simple substance and boron carbide is preferably 3:1;The present invention is preferably by controlling titanium list
The dosage of matter and boron carbide, avoids impurity from generating, to obtain TiB2The complex phase ceramic presoma of-TiC provides advantage.
In the present invention, the ball milling of the titanium simple substance and boron carbide is preferably dry ball milling.In the present invention, the ball milling
Speed be preferably 300~500r/min, further preferably 350~450r/min;More preferably 360~420r/min;Institute
The time for stating ball milling is preferably 12~for 24 hours, further preferably 16~22h, more preferably 18~20h.In the present invention, it is described
The ratio of grinding media to material of ball milling is preferably 10~30:1, further preferably 14~28:1, more preferably 18~26:1.In the present invention,
The ball milling is preferably 5~10mm with the diameter of abrading-ball, further preferably 5mm.In the present invention, the abrading-ball of the ball milling
Material with spherical tank is preferably aluminium oxide.In the present invention, the ball milling preferably carries out in an oxygen-free atmosphere, the oxygen-free atmosphere
Preferably argon gas.In the present invention, the purity of the argon gas is preferably greater than 99.9%.The present invention is specific to the oxygen-free atmosphere
Presentation mode does not do any particular determination, using well known to those skilled in the art.The present invention is preferably by ball milling side
The restriction of formula makes titanium and boron carbide are sufficiently mixed under oxygen-free atmosphere, influence of the oxygen to raw material components is avoided, to obtain purity
Higher TiB2- TiC complex phase ceramics presoma provides advantage.
In the present invention, the TiB2- TiC complex phase ceramic presoma presomas are made of metastable Ti, C and B element
Phase titanizing carbon-boronation titanium compound, physical stability is poor, undergoes phase transition to obtain stable TiB during follow-up sintering2-
TiC complex phase ceramics enhance phase, and enhancing Cu-base composites for in-situ synthesizing TiC provides possibility.
Obtain TiB2After-TiC complex phase ceramic presomas, the present invention is in the TiB2The surface of-TiC complex phase ceramic presomas
Chemical nickel plating is carried out, obtains nickel wetting enhancing particle.The nickel dosage that the present invention soaks the nickel in enhancing particle is not done any
Particular determination can coat TiB with nickel2Subject to-TiC complex phase ceramic presomas;The present invention is thick to the cladding of the nickel wetting phase
Degree does not do any particular determination.In the present invention, the chemical nickel plating preferably includes following steps:
By TiB2After-TiC complex phase ceramic presomas are mixed with nickel plating solution, carry out chemical nickel plating and mixture is obtained by the reaction
Liquid;
The mixed liquor is filtered, washed and dried successively, obtains nickel wetting enhancing particle.
In the present invention, the temperature of the nickel plating solution is preferably 40~50 DEG C, further preferably 42~48 DEG C, more
Preferably 45 DEG C.The present invention does not do any particular determination to the temperature control mode of the nickel plating solution, using art technology
Control mode known to personnel.The present invention does not do any particular determination to the component and manner of formulation of the nickel plating solution,
Using well known to those skilled in the art.The present invention controls the temperature of the nickel plating solution, can be by chemical nickel plating
Speed control in OK range, it is ensured that nickel wetting phase can be uniformly wrapped on TiB2- TiC complex phase ceramic presomas surface.
In the present invention, the pH value of the nickel plating solution is preferably 9~11, and further preferably 9.5~10.5.The present invention
Any particular determination is not done to the pH regulative modes of the nickel plating solution, can realize nickel plating solution in the range of above-mentioned pH i.e.
It can.The pH of nickel plating solution is carried out above-mentioned restriction by the present invention, is coordinated temperature conditionss, is effectively controlled the rate of chemical nickel plating, make nickel
It can uniformly coat and TiB2The surface of-TiC complex phase ceramic presomas.
The present invention does not do the time that the chemical nickel plating reacts any particular determination, and bubble-free is produced in the mixed liquor
Life can stop chemical nickel plating reaction.In the present invention, the chemical nickel plating reaction preferably carries out under agitation.The present invention
Any particular determination is not done to the specific embodiment of the stirring, using well known to those skilled in the art.In this hair
In bright, the stirring is preferably magnetic agitation.The present invention is by TiB2- TiC complex phase ceramic presomas are mixed with nickel plating solution, are being stirred
Under the conditions of mixing, nickel salt component and the nickel simple substance of reducing agent reaction generation in nickel plating solution is made to be coated on TiB2Before-TiC complex phase ceramics
The surface of body is driven, and then obtains the mixed liquor of nickeliferous wetting enhancing particle.
After obtaining mixed liquor, the present invention is preferably filtered, washs and dries to the mixed liquor successively, obtains nickel
Soak granular precursor.The present invention does not do any particular determination to the specific embodiment of the filtering, using art technology
Known to personnel.The present invention does not do any particular determination to the washing, using well known to those skilled in the art.
In the present invention, the mode of the drying is preferably to spontaneously dry or be dried in vacuo.In the present invention, it is described to spontaneously dry preferably
It is dried in air;The time of the natural drying is preferably 24~48h, further preferably 30~45h;The nature
Dry temperature is preferably room temperature.In the present invention, the vacuum drying vacuum degree is preferably 0.8 × 10-2~1.2 × 10-2MPa, further preferably 1.0 × 10-2MPa;The vacuum drying temperature is preferably 90~110 DEG C, further preferably
95~100 DEG C;The vacuum drying time is preferably 18~for 24 hours, further preferably 20~22h.
In the present invention, described be filtered, washed and dried handles the nickel salt that can remove nickel wetting presoma grain surface, reduction
Agent and moisture impurity subsequently to provide advantage with being sufficiently mixed for copper source, while avoid impurity from generating.
After obtaining nickel wetting granular precursor, the present invention, which soaks the nickel, increases granular precursor and copper source mixing and ball milling,
Obtain ball milling mixing material.In the present invention, nickel wetting granular precursor and the mass ratio in copper source are preferred in the ball milling mixing material
For 0.5~5:95~99, further preferably 0.5~3:97~99.In the present invention, copper source is preferably copper simple substance;Institute
Copper simple substance is stated to provide preferably in the form of copper powder.In the present invention, the purity of the copper powder is preferably 97~99.9%, further
Preferably 99.9%.The present invention does not have particular/special requirement to the grain size of the copper powder, is using well-known to those skilled in the art
It can.In the present invention, the grain size of the copper powder is preferably 100~200 mesh, further preferably 120~200 mesh.The present invention is right
The concrete mode of the mixing does not do any particular determination, using well known to those skilled in the art.
In the present invention, the nickel wetting granular precursor and the speed of copper source mixing and ball milling are preferably 120~240r/
Min, further preferably 150~220r/min, more preferably 180~200r/min;The time of the mixing and ball milling is preferably 8
~12h, further preferably 9~11h, more preferably 10h.In the present invention, the ratio of grinding media to material of the mixing and ball milling is preferably (2
~10):1, further preferably (5~10):1.In the present invention, the nickel wetting granular precursor and the mixing and ball milling in copper source
Preferably wet ball grinding, the medium of the wet ball grinding is preferably absolute ethyl alcohol.The present invention is to the specific use of the ball-milling medium
Amount does not do any particular provisions, using well known to those skilled in the art.In the present invention, the nickel wetting enhancing particle
With the material of abrading-ball and spherical tank it is preferably aluminium oxide with the ball milling of the mixture in copper source.The present invention is preferably enhanced by being soaked to nickel
Particle and the mixture in copper source carry out ball milling, and nickel wetting enhancing particle is made to come into full contact with, spread with copper, mutually uniform to obtain enhancing
The composite material of distribution provides advantage.
After the mixing and ball milling, the present invention is preferably dried the material after ball milling, obtains ball milling mixing material.In this hair
In bright, the drying is preferably to be dried in vacuo.In the present invention, the vacuum drying vacuum degree is preferably >=1 × 10-2MPa,
Further preferably 0.01~0.1MPa, further preferably 0.05~0.1MPa, more preferably 0.08~0.1MPa;It is described
Vacuum drying temperature is preferably 80~100 DEG C, further preferably 85~100 DEG C, more preferably 90~100 DEG C;It is described true
The sky dry time is preferably 12~for 24 hours, further preferably 15~for 24 hours.After the present invention is by being dried in vacuo removal ball milling
Absolute ethyl alcohol in material reduces influence of the residual ethanol to ball milling mixing material molding effect.
After obtaining ball milling mixing material, the present invention is cold-pressed the ball milling mixing material, obtains green compact.In the present invention,
The pressure of the cold pressing is preferably 300~500MPa, further preferably 350~450MPa;The time of the cold pressing is preferably 1
~3min, further preferably 1.5~2.5min.In the present invention, the temperature of the cold pressing is preferably room temperature.In the present invention
In, the cold pressing is preferably completed by way of bidirectional pressing;The present invention does not have the specific embodiment of the bidirectional pressing
Particular/special requirement, using embodiment well-known to those skilled in the art.The present invention makes scattered mixture using cold pressing
Shaping, while make ball milling mixing material each component densification consolidation, and then improve the fabricated in situ TiB being finally prepared2- TiC increases
The consistency of strong Cu-base composites.In the present invention, the diameter of the green compact is preferably 40mm;The draw ratio of the green compact is excellent
It elects as (1.8~2.2):1, further preferably 2:1;The relative density of the green compact is preferably 99.4~99.8%.
After obtaining green compact, the green compact is sintered by the present invention in an oxygen-free atmosphere, obtains sintered body.In the present invention
In, the oxygen-free atmosphere is preferably argon gas atmosphere.In the present invention, the flow of the argon gas is preferably 1~3L/min, further
Preferably 3L/min.In the present invention, the temperature of the sintering is preferably 900~1050 DEG C, further preferably 1000~
1050℃;The time of the sintering is 10~30min;Further preferably 15~25min.The present invention is warming up to the sintering temperature
The rate of degree is preferably 10~15 DEG C/min, further preferably 10 DEG C/min.The present invention is to the specific embodiment party of the sintering
Formula does not do any particular determination, using well known to those skilled in the art.
Further by the way that sintering condition is limited to above range, the alloying reaction for each component in green compact carries the present invention
For condition;In the sintering process, the TiB of alloying reaction generation surface cladded with nickel occurs for nickel wetting granular precursor2-TiC
Complex phase ceramic enhances phase, and suitable sintered body is provided to obtain target product.
After obtaining sintered body, the present invention forges and presses the sintered body, obtains fabricated in situ TiB2- TiC complex phase ceramics
Enhance Cu-base composites.The present invention improves TiB by forging and pressing2- TiC complex phase ceramics enhance the durometer properties of Cu-base composites
Energy.In the present invention, the fabricated in situ TiB2- TiC complex phase ceramics enhancing Cu-base composites relative density be preferably
More than 95%, further preferably 96~99.5%, more preferably 98.0~99.4%.
In the present invention, the forging and stamping are preferably 100~300% in the deflection of length direction, and further preferably 200
~300%;It is preferably 40~50% in diametric deflection, further preferably 50%.In the present invention, the forging and stamping
Temperature be preferably 500~550 DEG C, further preferably 510~540 DEG C.The present invention is to the specific embodiment of the forging and stamping
Any particular determination is not done, and use is well known to those skilled in the art, can realize the control of above-mentioned deflection and relative density
.In the present invention, the forging and stamping number is preferably 5~10 times, further preferably 10 times.
The present invention also provides the fabricated in situ TiB that the method described in above-mentioned technical proposal is prepared2- TiC complex phases are made pottery
Porcelain enhances Cu-base composites, including TiB2- TiC complex phase ceramics enhance phase, Copper substrate phase and are coated on the TiB2- TiC complex phases
The nickel wetting phase on ceramic enhancement phase surface, the TiB of surface cladded with nickel wetting phase2- TiC complex phase ceramic Dispersion of Reinforcement is in copper-based
The inside and surface of body phase.
In the present invention, the fabricated in situ TiB2TiB in-TiC complex phase ceramics enhancing Cu-base composites2- TiC complex phases
The mass ratio of ceramic enhancement phase and Copper substrate phase is preferably 0.5~2:48~49.5, further preferably 0.5~1.5:48.5~
49.5。
In the present invention, the fabricated in situ TiB2- TiC complex phase ceramics enhance the hardness (HV of Cu-base composites50g)
Preferably more than 255, further preferably 258~293;The fabricated in situ TiB2The enhancing of-TiC complex phase ceramics is copper-based compound
The electrode life of material is preferably more than 1300 solder joints further preferably 1400~2900 solder joints;The fabricated in situ
TiB2The conductivity of-TiC complex phase ceramics enhancing Cu-base composites is preferably more than 82%, further preferably 82.7~
89.9。
The present invention also provides the multistep processes fabricated in situ TiB described in above-mentioned technical proposal2- TiC complex phase ceramics enhance copper
Application of the based composites as spot-wedling electrode material, by the multistep processes fabricated in situ TiB2- TiC complex phase ceramics enhance copper
Based composites are machined out successively and cold extrusion, obtain spot-wedling electrode material.
The present invention is to the multistep processes fabricated in situ TiB2The physical dimension of-TiC spot-wedling electrodes does not have any particular/special requirement,
Using well known to those skilled in the art.In the present invention, the structural front view of the spot-wedling electrode is as shown in Figure 9.This
Invention does not do any particular determination to the specific embodiment of the machining and cold extrusion, can obtain the electric welding of said structure
Electrode.The present invention does not do any particular determination to the specific size of the spot-wedling electrode, ripe using those skilled in the art
Know.In the present invention, the physical dimension of described spot-wedling electrode is (unit mm) as shown in Figure 9.
In order to further illustrate the present invention, with reference to embodiment and attached drawing to fabricated in situ TiB provided by the invention2-
TiC complex phase ceramics enhancing Cu-base composites and its preparation method and application are described in detail, but cannot be interpreted as them
Limiting the scope of the present invention.
Comparative example 1
By the pure copper powder that grain size is 200 mesh, by bidirectional pressing, pressurize 2min, green compact are a diameter of under 350MPa pressure
40mm, green compact draw ratio are 1:2.In the case where flow is 2L/min ar gas environment, green compact is sintered at 950 DEG C, soaking time
30min.Under the conditions of control single deflection is less than 10%, forging and stamping 10 times repeatedly are carried out at 550 DEG C to sintered green compact, most
Whole diametric(al) deflection is 50%, and length direction deflection is 300%, and copper spot-wedling electrode material is obtained after processing.Material is straight
Footpath is 20mm, and length 40mm, relative density 99.2%, metallographic structure is as shown in Figure 1.
Will treated copper spot-wedling electrode material by machining and subsequent cold-extrusion technology, be processed into shape shown in Fig. 9
And the spot-wedling electrode of physical dimension (unit mm).According to 1 bronze medal spot-wedling electrode material preparation institute invocation point of IACS standard testings comparative example
The conductivity of welding electrode, test result are shown in Table 1;It is tested according to metal material Vickers hardness experimental standard GB/T 4340.1-2009
The hardness performance of 1 resulting materials of comparative example, test result are shown in Table 1;According to 1 material system of AWS-W-6858A standard testings comparative example
The service life of standby gained spot-wedling electrode, test result are shown in Table 1 and Figure 10.
Comparative example 2
By titanium simple substance (Ti powder, purity >=99.99%), the boron carbide (B that grain size is 200 mesh4C, purity >=99.99%) with
And pure copper powder carries out mechanical ball mill, titanium valve is 3 with boron carbide molar ratio:1, titanium valve accounts for the 1% of raw material gross mass with boron carbide, copper
Mass fraction of the powder in raw material total amount is 99%.Ball-milling technology is rotating speed 400r/min, Ball-milling Time for for 24 hours, ratio of grinding media to material be
20:1, abrading-ball and spherical tank material are aluminium oxide, ball radius 5mm, and mechanical milling process is completed under argon gas protection environment, and argon gas is pure
Degree is more than 99.9%.By the powder after ball milling by bidirectional pressing, pressurize 3min, green compact are a diameter of under 500MPa pressure
40mm, green compact draw ratio are 1:2.In the case where flow is 3L/min ar gas environment, it is warming up to according to the heating rate of 10 DEG C/min
After 1050 DEG C, soaking time 30min.Control single deflection be less than 10% under the conditions of, to sintered green compact 550 DEG C into
Row forges and presses 10 times repeatedly, and final diameter Direction distortion amount is 50%, and length direction deflection is 300%, obtains copper after processing and answers
Condensation material, a diameter of 20mm, length 40mm, relative density 99.1%, metallographic structure is as shown in Figure 2.
The carbon/carbon-copper composite material obtained after processing is processed into shape shown in Fig. 9 and size spot welding according to the method for comparative example 1
Electrode.For performance test methods with comparative example 1, test result is shown in Table 1 and Figure 10.
Comparative example 3
Weigh the TiB that 0.5g grain sizes are 200 mesh2- TiC powder (TiB2:TiC molar ratios 2:1), exist with 49.5g pure copper powders
Rotational speed of ball-mill 200r/min, Ball-milling Time 10h, ratio of grinding media to material 10:1, abundant mixing, abrading-ball and ball under soaked in absolute ethyl alcohol environment
Tank material is aluminium oxide, ball radius 5mm.Powder after ball milling is more than 1 × 10 in vacuum degree-2Under MPa environment, at 95 DEG C
Drying time is for 24 hours.By the powder after vacuum drying, by bidirectional pressing, 3min is kept the temperature under 500MPa, green compact is a diameter of
40mm.Green compact after shaping is sintered (gas flow 3L/min) under argon gas protection environment, and sintering temperature temperature is 1050 DEG C,
Sintering time 30min.Under the conditions of control single deflection is less than 10%, sintered green compact is forged repeatedly at 550 DEG C
Pressure 10 times, final diameter Direction distortion amount are 50%, and length direction deflection is 300%, and carbon/carbon-copper composite material material is obtained after processing
Material.
A diameter of 20mm of gained carbon/carbon-copper composite material, length 40mm, relative density 99.2%, metallographic structure such as Fig. 3
It is shown.The carbon/carbon-copper composite material obtained after processing is processed into shape shown in Fig. 9 and size spot welding electricity according to the method for comparative example 1
Pole.For performance test methods with comparative example 1, test result is shown in Table 1 and Figure 10.
Embodiment 1
Weighing 10g titanium valves and boron carbide, (titanium valve is 3 with boron carbide molar ratio:1, grain size be 200 mesh, purity >=
99.99%) ball milling is carried out, ball milling parameter is rotating speed 350r/min, Ball-milling Time 12h, ratio of grinding media to material 10:1, abrading-ball and spherical tank
Material is aluminium oxide, ball radius 5mm, and mechanical milling process is completed under argon gas protection environment, purity of argon 99.9%.By ball
Titanium valve and boron carbide powder after mill are put into the chemical nickel-plating solution that pH value is 9, at a temperature of 40 DEG C, pass through magnetic stirring apparatus
Agitating solution to bubble-free generate, then filter and be washed with deionized to neutrality, be placed in air spontaneously dry it is spare.It takes
Dried ball-milled powder 0.5g is pure copper powder that 49.5g grain sizes are 200 mesh in rotational speed of ball-mill 120r/min, ball milling with quality
Time 12h, ratio of grinding media to material 2:1, abundant mixing under soaked in absolute ethyl alcohol environment, abrading-ball is aluminium oxide with spherical tank material, and abrading-ball is straight
Footpath is 5mm.Powder after ball milling is dried in vacuo, vacuum degree is 1 × 10-2MPa, drying temperature are 90 DEG C, drying time
For 12h.By the powder after vacuum drying, by bidirectional pressing, 3min, a diameter of 40mm of green compact are kept the temperature under 300MPa.Shaping
Green compact afterwards is sintered (gas flow 2L/min) under argon gas protection environment, during sintering, heats up according to the speed of 10 DEG C/min
To after 950 DEG C, 20min is kept the temperature, obtains sintered body;Sintered body is less than 10%, under the conditions of 550 DEG C in control single deflection,
Sintered body being forged and pressed repeatedly 10 times, final diameter Direction distortion amount is 50%, and length direction deflection is 300%, after processing
To fabricated in situ TiB2- TiC complex phase ceramics enhance Cu-base composites.
Fabricated in situ TiB2- TiC complex phase ceramics enhance a diameter of 20mm, the length 40mm of Cu-base composites, relatively
Density is 98.2%, and metallographic structure is as shown in Figure 4.By fabricated in situ TiB2- TiC complex phase ceramics enhance Cu-base composites according to
The mode of comparative example 1 is processed into spot-wedling electrode.For performance test methods with comparative example 1, test result is shown in Table 1 and Figure 10.
Embodiment 2
Weighing 10g titanium valves and boron carbide, (titanium valve is 3 with boron carbide molar ratio:1, grain size be 200 mesh, purity >=
99.99%) ball milling is carried out, ball milling parameter is rotating speed 400r/min, Ball-milling Time 18h, ratio of grinding media to material 20:1, abrading-ball and spherical tank
Material is aluminium oxide, ball radius 5mm, and mechanical milling process is completed under argon gas protection environment, purity of argon 99.95%.By ball
Titanium valve and boron carbide powder after mill are put into the chemical nickel-plating solution that pH value is 9.5, at a temperature of 45 DEG C, pass through magnetic agitation
Device agitating solution to bubble-free generate, then filter and be washed with deionized to neutrality, be placed in air spontaneously dry it is spare.
Dried ball-milled powder 0.5g is taken, is pure copper powder that 49.5g grain sizes are 200 mesh in rotational speed of ball-mill 150r/min, ball with quality
Time consuming 8h, ratio of grinding media to material 5:1, abundant mixing under soaked in absolute ethyl alcohol environment, abrading-ball is aluminium oxide with spherical tank material, and abrading-ball is straight
Footpath is 5mm.Powder after ball milling is more than 1 × 10 in vacuum degree-2Under MPa environment, in 95 DEG C of drying time 18h.Vacuum is done
Powder after dry by bidirectional pressing, keeps the temperature 3min, a diameter of 40mm of green compact under 400MPa.Green compact after shaping is in argon gas
(gas flow 3L/min) is sintered under environmental protection, controls heating rate as 10 DEG C/min, is warming up to 1000 DEG C, sintering
30min obtains sintered body.It is less than 10%, under the conditions of 550 DEG C in control single deflection, 10 is forged and pressed repeatedly to sintered body
Secondary, final diameter Direction distortion amount is 50%, and length direction deflection is 300%, and fabricated in situ TiB is obtained after processing2-TiC
Complex phase ceramic enhances Cu-base composites.
Fabricated in situ TiB2- TiC complex phase ceramics enhance a diameter of 20mm, the length 40mm of Cu-base composites, relatively
Density is 98.6%, and metallographic structure is as shown in Figure 5.By fabricated in situ TiB2- TiC complex phase ceramics enhance Cu-base composites according to
The mode of comparative example 1 is processed into spot-wedling electrode.For performance test methods with comparative example 1, test result is shown in Table 1 and Figure 10.
Implementation column 3
Weighing 10g titanium valves and boron carbide, (titanium valve is 3 with boron carbide molar ratio:1, grain size be 200 mesh, purity >=
99.99) carry out ball milling, ball milling parameter is rotating speed 500r/min, Ball-milling Time for for 24 hours, ratio of grinding media to material 30:1, abrading-ball and spherical tank material
Expect for aluminium oxide, ball radius 5mm, mechanical milling process is completed under argon gas protection environment, and purity of argon is more than 99.9%.By ball
Titanium valve and boron carbide powder after mill are put into the chemical nickel-plating solution that pH value is 9.5, at a temperature of 50 DEG C, pass through magnetic agitation
Device agitating solution to bubble-free generate, then filter and be washed with deionized to neutrality, be placed in air spontaneously dry it is spare.
Dried ball-milled powder 0.5g is taken, is pure copper powder that 49.5g grain sizes are 200 mesh in rotational speed of ball-mill 200r/min, ball with quality
Time consuming 10h, ratio of grinding media to material 10:1, abundant mixing under soaked in absolute ethyl alcohol environment, abrading-ball and spherical tank material are aluminium oxide, abrading-ball
A diameter of 5mm.Powder after ball milling is more than 1 × 10 in vacuum degree-2Under MPa environment, 100 DEG C of drying times for 24 hours.It will be true
Empty dried powder, by bidirectional pressing, keeps the temperature 3min, a diameter of 40mm of green compact under 500MPa.Green compact after shaping exists
(gas flow 3L/min) is sintered under argon gas protection environment, 1050 DEG C are warming up under 15 DEG C/min rates, keeps the temperature 30min,
Obtain sintered body.It is less than 10% in control single deflection, under conditions of temperature is 550 DEG C, sintered body is forged and pressed repeatedly
10 times, final diameter Direction distortion amount is 50%, and length direction deflection is 300%, and fabricated in situ TiB is obtained after processing2-
TiC complex phase ceramics enhance Cu-base composites.
Fabricated in situ TiB2- TiC complex phase ceramics enhance a diameter of 20mm, the length 40mm of Cu-base composites, relatively
Density is 99.6%, and metallographic structure is as shown in Figure 6.By fabricated in situ TiB2- TiC complex phase ceramics enhance Cu-base composites according to
The mode of comparative example 1 is processed into spot-wedling electrode.For performance test methods with comparative example 1, test result is shown in Table 1 and Figure 10.
Embodiment 4
Weighing 10g titanium valves and boron carbide, (titanium valve is 3 with boron carbide molar ratio:1, grain size be 200 mesh, purity >=
99.99) carry out ball milling, ball milling parameter is rotating speed 500r/min, Ball-milling Time for for 24 hours, ratio of grinding media to material 30:1, abrading-ball and spherical tank material
Expect for aluminium oxide, ball radius 5mm, mechanical milling process is completed under argon gas protection environment, and purity of argon is more than 99.9%.By ball
Titanium valve and boron carbide powder after mill are put into the chemical nickel-plating solution that pH value is 9.5, at a temperature of 50 DEG C, pass through magnetic agitation
Device agitating solution to bubble-free generate, then filter and be washed with deionized to neutrality, be placed in air spontaneously dry it is spare.
Dried ball-milled powder 1g is taken, is pure copper powder that 49g grain sizes are 200 mesh in rotational speed of ball-mill 200r/min, ball milling with quality
Between 10h, ratio of grinding media to material 10:1, abundant mixing under soaked in absolute ethyl alcohol environment, abrading-ball and spherical tank material are aluminium oxide, ball radius
For 5mm.Powder after ball milling is more than 1 × 10 in vacuum degree-2Under MPa environment, 100 DEG C of drying times for 24 hours.Vacuum is done
Powder after dry by bidirectional pressing, keeps the temperature 3min, a diameter of 40mm of green compact under 500MPa.Green compact after shaping is in argon gas
(gas flow 3L/min) is sintered under environmental protection, 1050 DEG C are warming up under 15 DEG C/min rates, 30min is kept the temperature, obtains
Sintered body.It is less than 10%, under conditions of temperature is 550 DEG C in control single deflection, sintered body is carried out to forge and press 10 times repeatedly,
Final diameter Direction distortion amount is 50%, and length direction deflection is 300%, and fabricated in situ TiB is obtained after processing2- TiC complex phases
Ceramic strengthening copper base composite.
Fabricated in situ TiB2- TiC complex phase ceramics enhance a diameter of 20mm, the length 40mm of Cu-base composites, relatively
Density is 98.9%, and metallographic structure is as shown in Figure 7.By fabricated in situ TiB2- TiC complex phase ceramics enhance Cu-base composites according to
The mode of comparative example 1 is processed into spot-wedling electrode.For performance test methods with comparative example 1, test result is shown in Table 1 and Figure 10.
Embodiment 5
Weighing 10g titanium valves and boron carbide, (titanium valve is 3 with boron carbide molar ratio:1, grain size be 200 mesh, purity >=
99.99) carry out ball milling, ball milling parameter is rotating speed 500r/min, Ball-milling Time for for 24 hours, ratio of grinding media to material 30:1, abrading-ball and spherical tank material
Expect for aluminium oxide, ball radius 5mm, mechanical milling process is completed under argon gas protection environment, and purity of argon is more than 99.9%.By ball
Titanium valve and boron carbide powder after mill are put into the chemical nickel-plating solution that pH value is 9.5, at a temperature of 50 DEG C, pass through magnetic agitation
Device agitating solution to bubble-free generate, then filter and be washed with deionized to neutrality, be placed in air spontaneously dry it is spare.
Dried ball-milled powder 1.5g is taken, is pure copper powder that 48.5g grain sizes are 200 mesh in rotational speed of ball-mill 200r/min, ball with quality
Time consuming 10h, ratio of grinding media to material 10:1, abundant mixing under soaked in absolute ethyl alcohol environment, abrading-ball and spherical tank material are aluminium oxide, abrading-ball
A diameter of 5mm.Powder after ball milling is more than 1 × 10 in vacuum degree-2Under MPa environment, 100 DEG C of drying times for 24 hours.It will be true
Empty dried powder, by bidirectional pressing, keeps the temperature 3min, a diameter of 40mm of green compact under 500MPa.Green compact after shaping exists
(gas flow 3L/min) is sintered under argon gas protection environment, 1050 DEG C are warming up under 15 DEG C/min rates, keeps the temperature 30min,
Obtain sintered body.It is less than 10% in control single deflection, under conditions of temperature is 550 DEG C, sintered body is forged and pressed repeatedly
10 times, final diameter Direction distortion amount is 50%, and length direction deflection is 300%, and fabricated in situ TiB is obtained after processing2-
TiC complex phase ceramics enhance Cu-base composites.
Fabricated in situ TiB2- TiC complex phase ceramics enhance a diameter of 20mm, the length 40mm of Cu-base composites, relatively
Density is 98.0%, and metallographic structure is as shown in Figure 8.By fabricated in situ TiB2- TiC complex phase ceramics enhance Cu-base composites according to
The mode of comparative example 1 is processed into spot-wedling electrode.For performance test methods with comparative example 1, test result is shown in Table 1 and Figure 10.
Fig. 1 is the metallographic structure figure of 1 gained copper product of comparative example, and institutional framework is more uniform;Fig. 2 is 2 gained of comparative example
The metallographic structure figure of Cu-base composites, wherein black portions are enhancing phase of reuniting, and illustrate group obtained by the method that comparative example 2 provides
Knit that structural homogeneity is poor, the hardness performance of product is affected;Fig. 3 is the gold for the carbon/carbon-copper composite material that comparative example 3 is prepared
Phase constitution figure although caning be found that the agglomeration traits of enhancing phase are declined compared with comparative example 2 from figure, but exists;
Also know exist in no wetting phase by the metallographic structure figure of comparative example 2 and 3, the enhancing of gained carbon/carbon-copper composite material is mutually reunited
It is more serious, it can not be uniformly distributed in Copper substrate, enhancing the stress concentration for mutually reuniting or causing reunion region, so that splitting
Line easily generates in this region, so as to influence the performance of material.
Fig. 4~8 are corresponding in turn to fabricated in situ TiB obtained by Examples 1 to 52- TiC complex phase ceramics enhance Cu-base composites
Metallographic structure, uniform texture is distributed in figure, from metallographic structure figure, in the presence of having wetting phase, gained
Enhancing in product can be mutually uniformly distributed in the smaller graininess of grain size in Copper substrate, help to improve fabricated in situ
TiB2- TiC complex phase ceramics enhance the mechanical strength and hardness performance of Cu-base composites.
Figure 10 is is processed spot-wedling electrode in same weld parameter using 1~3 material of comparative example and Examples 1 to 5 material
Under life test as a result, life test it turns out that, using spot-wedling electrode prepared by Cu-base composites of the present invention have compared with
Long service life.
1 comparative example of table is compared with embodiment material property
Cu-base composites | Hardness (HV50g) | Electrical conductivity (%IACS) | Electrode life (weldering time) |
Comparative example 1 | 35 | 98.2 | 200 |
Comparative example 2 | 187 | 78.5 | 1050 |
Comparative example 3 | 191 | 78.7 | 1100 |
Embodiment 1 | 258 | 87.2 | 1650 |
Embodiment 2 | 262 | 87.4 | 2150 |
Embodiment 3 | 273 | 89.9 | 2850 |
Embodiment 4 | 286 | 83.8 | 1350 |
Embodiment 5 | 293 | 82.7 | 1450 |
According to the data that table 1 is recorded, the hardness performance for the carbon/carbon-copper composite material that comparative example 2 and 3 is prepared is carried
Height, but electric conductivity reduction is more apparent, and the fabricated in situ TiB that the application is prepared2The enhancing of-TiC complex phase ceramics is copper-based
The electric conductivity of composite material and being closer to for copper product, hardness performance is significantly larger than copper product;And it hardness performance and leads
Electrical property is superior to comparative example 1 and 2, is highly suitable as spot-wedling electrode material.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of fabricated in situ TiB2- TiC complex phase ceramics enhance the preparation method of Cu-base composites, comprise the following steps:
1) titanium simple substance and boron carbide are subjected to ball milling, obtain TiB2- TiC complex phase ceramic presomas;
2) in the TiB2The surface of-TiC complex phase ceramic presomas carries out chemical nickel plating, obtains nickel wetting enhancing particle;
3) nickel is soaked into enhancing particle and copper source mixing and ball milling, obtains ball milling mixing material;
4) the ball milling mixing material is cold-pressed, obtains green compact;
5) green compact is sintered in an oxygen-free atmosphere, obtains sintered body;
6) sintered body is forged and pressed, obtains fabricated in situ TiB2- TiC complex phase ceramics enhance Cu-base composites.
2. preparation method as described in claim 1, which is characterized in that the molar ratio of the titanium simple substance and boron carbide is 3:1.
3. preparation method as described in claim 1, which is characterized in that the speed of ball milling is 300~500r/ in the step 1)
Min, time of ball milling for 12~for 24 hours.
4. preparation method as described in claim 1, which is characterized in that the nickel plating solution of chemical nickel plating in the step 2)
Temperature is 45~50 DEG C, and the pH value of the nickel plating solution is 9~11.
5. preparation method as described in claim 1, which is characterized in that nickel wetting enhancing particle and copper source in the step 3)
Mass ratio is 0.5~5:95~99.
6. preparation method as described in claim 1, which is characterized in that the pressure of the step 4) cold pressing is 300~500MPa,
The time of cold pressing is 1~3min.
7. preparation method as described in claim 1, which is characterized in that the temperature of sintering is 900~1050 in the step 5)
DEG C, the time of sintering is 10~30min.
8. preparation method as described in claim 1, which is characterized in that the temperature of forging and stamping is 500~550 in the step 6)
℃。
9. the fabricated in situ TiB that any one of claim 1~8 the method is prepared2The enhancing of-TiC complex phase ceramics is copper-based compound
Material, including TiB2- TiC complex phase ceramics enhance phase, Copper substrate phase and are coated on the TiB2- TiC complex phase ceramics enhance phase surface
Nickel wetting phase, the TiB of surface cladded with nickel wetting phase2- TiC complex phase ceramics Dispersion of Reinforcement is in the inside of Copper substrate phase and table
Face.
10. the fabricated in situ TiB described in claim 92- TiC complex phase ceramics enhance Cu-base composites as spot-wedling electrode material
Application, by the TiB2-ZrB2Complex phase ceramic enhancing Cu-base composites are machined out successively and cold extrusion, obtain spot welding
Electrode.
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