CN104878240B - Add the TiB in situ of rare earth La2Strengthen Cu-base composites - Google Patents
Add the TiB in situ of rare earth La2Strengthen Cu-base composites Download PDFInfo
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- CN104878240B CN104878240B CN201510330692.0A CN201510330692A CN104878240B CN 104878240 B CN104878240 B CN 104878240B CN 201510330692 A CN201510330692 A CN 201510330692A CN 104878240 B CN104878240 B CN 104878240B
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- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 34
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 32
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 30
- 239000010949 copper Substances 0.000 claims abstract description 43
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910033181 TiB2 Inorganic materials 0.000 claims abstract description 27
- 229910052802 copper Inorganic materials 0.000 claims abstract description 26
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000006698 induction Effects 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- 238000002844 melting Methods 0.000 claims description 15
- 229910045601 alloy Inorganic materials 0.000 claims description 13
- 239000000956 alloy Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000007531 graphite casting Methods 0.000 claims description 7
- 229910017945 Cu—Ti Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 22
- 239000011159 matrix material Substances 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000005275 alloying Methods 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract description 2
- 230000008023 solidification Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- 238000009826 distribution Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QDIYZGWZTHZFNM-UHFFFAOYSA-N [F].[K] Chemical compound [F].[K] QDIYZGWZTHZFNM-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000001540 jet deposition Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The present invention provides a kind of TiB in situ for adding rare earth La2Strengthen Cu-base composites, the TiB in situ of the addition rare earth La2Strengthen Cu-base composites, including the following each component of weight proportion:0.5 2wt% TiB2, 0.02 0.10wt% La, surplus be Cu.The present invention is by alloying, in Cu TiB2A certain amount of rare-earth elements La is added in composite, the higher La of surface-active can make TiB2Tiny TiB is generated in generation phase2Particle, disperses TiB in the composite material solidification stage2Particle, is allowed to even dispersion in copper metal matrix, therefore obtains the Cu TiB with good combination property2Cu-base composites.The TiB in situ of rare earth La is added after testing2Strengthen Cu-base composites intensity high, electric conductivity is good.
Description
Technical field
The present invention relates to composite technology, more particularly to a kind of TiB in situ for adding rare earth La2Strengthen copper-based composite wood
Material.
Background technology
It is also continuous to copper alloy performance with developing rapidly for the fields such as electrotechnical, electronic, track traffic and Aero-Space
Propose higher requirement.Such as track traffic contact line, magnetic artillery guide rail not only needs higher electrical conductivity, while needing tool
There are higher intensity, good wearability and high temperature resistance softening performance etc..Copper is solid-solution in conductivity theory, copper alloy
Scattering process of the lattice distortion caused by atom in matrix to electronics is more much better than than scattering process caused by the second phase, therefore copper
Electrical conductivity can be all greatly lowered in the raising of intensity in alloy, and complex intensifying is because second between copper atom, can't
Copper is solid-solution in, therefore will not substantially reduce the electric conductivity of Copper substrate, simultaneously because the effect of hardening constituent further improves the room of matrix
Temperature and high-temperature behavior, as the main reinforcing means for obtaining high-strength highly-conductive copper-based material.Therefore Cu-base composites in future
Development and application in great potential.
Many methods for preparing composite, such as mechanical alloying method, internal oxidation, jet deposition are developed at present
Method, conventional casting methods and hot pressing sintering method etc..Wherein, prepared using XD method and conventional casting methods copper-based compound
Material has with low cost, it is easy to obtain, the advantages of can preparing large scale sample.The second phase particles of Dispersed precipitate can be fine
Strengthen Copper substrate, TiB in ground2Not only conductive, thermal conductivity is good for particle, with high-melting-point, hardness, chemical stability, corrosion resistance and
Excellent wearability, makes the conductance thermal conductivity decline of metal smaller compared with other ceramic base particles, makes TiB2/ Cu composite woods
Material has higher electrical conductivity and high temperature resistance softening performance, and its standard Gibbs free energy is relatively low, can be by potassium fluoborate, fluorine
Potassium titanate complex salt is synthesized, and can also be directly generated by titanium, boron in high temperature, therefore can react generation in metallic matrix situ,
Composite enhancing and the Problem of Wettability of matrix prepared by common outer adding method are solved, becomes metal-base composites
In the enhancing phase particle that adds extensively.
However, the TiB that directly casting is obtained2TiB in/Cu composites2Strengthen particle diameter larger, substantially all micro-
Not, from Orowan equation, micron-sized particle enhancing effect is not very obvious for meter level.In addition, in order to reduce reinforcement TiB2
Particle shows free energy, tends to reunite to the overall performance of the infringement composite that together, this can be more serious.
The content of the invention
It is an object of the present invention to be directed to above-mentioned existing TiB2TiB in/Cu composites2Particle diameter is larger asks for enhancing
Topic, proposes a kind of TiB in situ for adding rare earth La2Strengthen TiB in Cu-base composites, the composite2Particle is tiny and disperse
Distribution, makes the composite have the advantages that intensity is higher, electric conductivity is good.
To achieve the above object, the technical solution adopted by the present invention is:A kind of TiB in situ for adding rare earth La2Strengthen copper
Based composites, including the following each component of weight proportion:0.5-2wt% TiB2, 0.02-0.10wt% La, surplus be
Cu。
Further, the TiB in situ of rare earth La is added2Strengthening Cu-base composites includes the following each group of weight proportion
Point:0.1-1.5wt% TiB2, 0.04-0.08wt% La, surplus be Cu.
Another object of the present invention additionally provides a kind of TiB in situ of the addition rare earth La2Strengthen copper-based composite wood
The method of material, comprises the following steps:
(1) fine copper is placed in vacuum intermediate-frequency induction melting furnace burner hearth;
(2) vacuum intermediate-frequency induction melting furnace burner hearth is vacuumized into rear reversely charging argon gas;
(3) fine copper is heated to be completely melt and be warming up to 1200-1300 DEG C;
(4) Cu-La intermediate alloys are added to vacuum intermediate-frequency induction melting furnace burner hearth, keeps 3-15min, preferably 5-
10min, makes Cu-La intermediate alloys uniform melt in fine copper;
(5) Cu-B intermediate alloys and Cu-Ti intermediate alloys are added to vacuum intermediate-frequency induction melting furnace burner hearth successively, protected respectively
Warm 3-15min, preferably 5-10min;The step generates TiB in Cu matrix situs2Particle reaction formula is as follows:[Ti]+2
[B]→TiB2;
(6) adjustment melt temperature is to 1200-1300 DEG C, and is cast in the graphite casting die of preheating, obtains addition rare earth La
TiB in situ2Strengthening in Cu-base composites, the material not only strengthens phase TiB2Particle is more tiny, and Dispersed precipitate is in copper
In matrix.
Further, step (2) vacuum intermediate-frequency induction melting furnace burner hearth is evacuated to after 5-10Pa, and reversely charging argon gas is extremely
0.02-0.1MPa, preferably 0.05-0.08MPa.
Further, the graphite casting die of step (6) described preheating is the graphite casting die of 250-400 DEG C of preheating, is preferably
300-350℃。
Further, it is necessary to raw material before step (1) adds the raw material into vacuum intermediate-frequency induction melting furnace burner hearth
Pre-processed, comprised the following steps:
(1) fine copper, Cu-La, Cu-B and Cu-Ti intermediate alloy are cleaned with watery hydrochloric acid, washes away oxide on surface and miscellaneous
Matter;
(2) above-mentioned raw materials are placed in supersonic wave cleaning machine, using washes of absolute alcohol raw material surface, wash away raw material residual
Hydrochloric acid and impurity;
(3) raw material after ultrasonic cleaning is dried into 2-3h, preferably 100-130 in air dry oven at 100-150 DEG C
2-2.5h is dried at DEG C.
The TiB in situ of present invention addition rare earth La2Enhancing Cu-base composites scientific formulation, reasonable, its preparation method letter
It is single, easy, compared with prior art with advantages below:
(1) present invention is by alloying, in Cu-TiB2A certain amount of rare-earth elements La, surface are added in composite
The higher La of activity can make TiB2Tiny TiB is generated in generation phase2Particle, disperses TiB in the composite material solidification stage2
Grain, is allowed to even dispersion in copper metal matrix, therefore obtain the Cu-TiB with good combination property2Copper-based composite wood
Material.The TiB in situ of rare earth La is added after testing2Strengthen Cu-base composites intensity high, electric conductivity is good.
(2) preparation method of the present invention can realize the TiB in situ of addition rare earth La2Strengthen the industrialization batch of Cu-base composites
Amount production.
Fig. 1 is the TiB in situ for being not added with rare-earth elements La2Strengthen TiB in Cu-base composites2Granular size and distribution feelings
The SEM figures of condition;Fig. 2 adds La TiB in situ for the present invention2Strengthen TiB in Cu-base composites2Granular size and distribution situation
SEM figure, wherein TiB2Mass percent be 1%, La mass percent 0.04%;By can be with comparison diagram 1 and Fig. 2
, it is evident that when being not added with rare earth La, TiB in composite2Mean particle size is 1.5 μm, but after addition rare earth La,
TiB in composite2Particle diameter has been reduced to 0.5 μm or so, and polymerize situation and also obtained very big improvement.
Fig. 3 is addition different quality containing La TiB in situ2Strengthen the tensile strength and elongation percentage of Cu-base composites,
Wherein TiB2Weight/mass percentage composition be 1wt%, surplus is Cu;Therefrom, it is apparent that addition La after, Cu-TiB2It is compound
Tensile strength has one to be obviously improved, because after addition La, TiB2Particle is more tiny, and in Copper substrate
It is uniformly distributed, when being plastically deformed, strong hinders the germinating and extension of crackle, therefore significantly improves compound
The tensile strength of material.
The raising of tensile strength can be accompanied by, the decline of elongation is brought.This is because, TiB2Particle is in Copper substrate
Middle uneven distribution, in tension test, without TiB2Larger plastic deformation can occur for the position of particle, thus with compared with
High elongation.And after addition La, TiB2Particle is uniformly distributed in Copper substrate, when being plastically deformed, TiB2Particle has
The generation for preventing large plastometric set of power, therefore elongation is slightly decreased.
Fig. 4 is addition different quality containing La TiB in situ2Strengthen the conductance of Cu-base composites, wherein TiB2Matter
Amount percentage composition is 1wt%, and surplus is Cu.After addition rare earth La, electrical conductivity, which has, significantly to be lifted, and is carried by 66.5%IACS
Height has arrived 88.5%IACS, improves 33.1%.
Brief description of the drawings
Fig. 1 is the TiB in situ for being not added with rare-earth elements La2Strengthen TiB in Cu-base composites2Granular size and distribution feelings
The SEM figures of condition;
Fig. 2 adds La TiB in situ for the present invention2Strengthen TiB in Cu-base composites2Granular size and distribution situation
SEM schemes;
Fig. 3 is addition different quality containing La TiB in situ2Strengthen the tensile strength and elongation percentage of Cu-base composites;
Fig. 4 is addition different quality containing La TiB in situ2Strengthen the conductance of Cu-base composites.
Embodiment
The present invention is further described with reference to embodiments:
Embodiment 1
Present embodiment discloses a kind of TiB in situ for adding rare earth La2Strengthen Cu-base composites, including weight proportion is such as
Under each component:1wt% TiB2, 0.04wt% La-, surplus be Cu.
The present embodiment adds the TiB in situ of rare earth La2The preparation method for strengthening Cu-base composites is as follows:
Experiment material is pre-processed
By fine copper (purity >=99.97% (mass fraction, similarly hereinafter), the production of Dalian Xin Long foundary industries Co., Ltd), Cu-
10La (La contents 9.9%~10.1%, the coloured institute of Hunan rare earth), Cu-5B (B content 4.9%~5.1%, Ningbo economy technology
Be proficient in trade Co., Ltd's production in development zone), Cu-10Ti (in Ti contents 9.9%~10.1%, vacuum induction melting furnace prepare)
Intermediate alloy is cleaned with watery hydrochloric acid, washes away oxide on surface and impurity;Surface is cleaned in supersonic wave cleaning machine with absolute ethyl alcohol
5min, washes away the hydrochloric acid and impurity of residual;Material after ultrasonic cleaning is dried into 2h in air dry oven at 100 DEG C;On
State weight proportion weighing.
Add the TiB in situ of rare earth La2Strengthen Cu-base composites to prepare
(1) fine copper is added in vacuum intermediate-frequency induction melting furnace burner hearth, by Cu-La, Cu-B and Cu-Ti intermediate alloy
It is respectively put into loading hopper;
(2) vacuum intermediate-frequency induction melting furnace burner hearth is evacuated to after 5-10Pa, reversely charging argon gas to 0.06MPa;
(3) vacuum intermediate-frequency induction melting furnace intermediate frequency power supply is opened, tough cathode is heated to and is completely melt and is warming up to 1250
℃;
(4) Cu-10La intermediate alloys are added from hopper, is kept for 5 minutes, treats its uniform melt in Cu;
(5) Cu-5B and Cu-10Ti are sequentially added, 5 minutes are incubated respectively, following reaction occurs during this period:[Ti]+2
[B]→TiB2, TiB is generated in Cu situs2Particle.
(6) adjustment melt temperature is cast in the graphite casting die through 300 DEG C of preheatings to 1250 DEG C, obtains adding rare earth La
TiB in situ2Strengthen Cu-base composites.
The TiB in situ of rare earth La is added described in the present embodiment after testing2Enhancing Cu-base composites tensile strength be
196MPa, elongation percentage are that 39.5%, conductance is 88.5IACS%.
Embodiment 2
Present embodiment discloses a kind of TiB in situ for being not added with rare earth La2Strengthen Cu-base composites and embodiment 1 is basic
Identical, the difference is that described La contents are 0.08wt%, weight proportion is as follows:1wt%TiB2, 0.08wt% La, surplus
For Cu.
Its preparation method is same as Example 1.
After testing prepared by the present embodiment addition rare earth La TiB in situ2Strengthen the tensile strength of Cu-base composites
It is that 49.5%, conductance is 87.7IACS% for 180MPa, elongation percentage.
Reference examples
Reference examples are substantially the same manner as Example 1, the difference is that being not added with rare earth La during dispensing, i.e.,:1wt% TiB2, it is remaining
Measure as Cu.
Its preparation method is accordingly without the step (4) in embodiment 1.
The TiB in situ of rare earth La is not added with described in this reference examples after testing2Enhancing Cu-base composites tensile strength be
176MPa, elongation percentage are that 45.5%, conductance is 66.5IACS%.
Finally it should be noted that:Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations;To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that:Its according to
The technical scheme described in foregoing embodiments can so be modified, or which part or all technical characteristic are entered
Row equivalent substitution;And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (1)
1. a kind of TiB in situ for adding rare earth La2Strengthen Cu-base composites, it is characterised in that including following each of weight proportion
Component:0.1-1.5wt% TiB2, 0.04-0.08wt% La, surplus be Cu;
The TiB in situ of the addition rare earth La2Strengthen the method for Cu-base composites, it is characterised in that comprise the following steps:
(1) fine copper is placed in vacuum intermediate-frequency induction melting furnace burner hearth;Add the raw material into vacuum intermediate-frequency induction melting furnace burner hearth
Before, it is necessary to be pre-processed to raw material, comprise the following steps:
(a) fine copper, Cu-La, Cu-B and Cu-Ti intermediate alloy are cleaned with watery hydrochloric acid, washes away oxide on surface and impurity;
(b) above-mentioned raw materials are placed in supersonic wave cleaning machine, using washes of absolute alcohol raw material surface, wash away the salt of raw material residual
Acid and impurity;
(c) raw material after ultrasonic cleaning is dried into 2-3h in air dry oven at 100-150 DEG C;
(2) vacuum intermediate-frequency induction melting furnace burner hearth is evacuated to after 5-10Pa, reversely charging argon gas to 0.02-0.1MPa;
(3) fine copper is heated to be completely melt and be warming up to 1200-1300 DEG C;
(4) Cu-La intermediate alloys are added to vacuum intermediate-frequency induction melting furnace burner hearth, keeps 3-15min;
(5) Cu-B intermediate alloys and Cu-Ti intermediate alloys are added to vacuum intermediate-frequency induction melting furnace burner hearth successively, 3- is incubated respectively
15min;
(6) adjustment melt temperature is to 1200-1300 DEG C, and is cast in the graphite casting die of preheating, obtains the original of addition rare earth La
Position TiB2Strengthen Cu-base composites, the graphite casting die of the preheating is the graphite casting die of 250-400 DEG C of preheating.
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CN107354337B (en) * | 2017-07-21 | 2019-04-05 | 大连理工大学 | Diphase particles in situ enhance Cu-base composites |
CN107723501B (en) * | 2017-09-30 | 2019-06-14 | 河南科技大学 | A kind of TiB2The Cu-base composites and preparation method thereof of particle and carbon nanotube mixing enhancing |
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