CN104946923B - Copper-based composite material and preparation method thereof - Google Patents
Copper-based composite material and preparation method thereof Download PDFInfo
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- CN104946923B CN104946923B CN201510385481.7A CN201510385481A CN104946923B CN 104946923 B CN104946923 B CN 104946923B CN 201510385481 A CN201510385481 A CN 201510385481A CN 104946923 B CN104946923 B CN 104946923B
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Abstract
The invention discloses a copper-based composite material and a preparation method of the material. An electronic beam physical vapor deposition device is adopted, a separation layer is deposited firstly, then, a copper ingot material and a second phase material are heated through electron-beam current, constant beam current is used for heating the copper ingot material, the second phase material is heated through periodically-changed beam current, a copper-based material is deposited on the separation layer, and cooling and separation are carried out, so that the copper-based composite material is obtained; the manufactured copper-based composite material contains second phase particles, the second phase particles are Mo or Nb or Al2O3 or Y2O3, the volume size of the second phase particles ranges from 0.4% to 2%, the content of the second phase particles is periodically changed in the thickness direction of the copper-based composite material, and the size of the second phase particles is smaller than 50nm;and the yield strength Rp0.2 of the material is larger than or equal to 460MPa, the tensile strength Rm is larger than or equal to 500MPa, the conductivity is larger than or equal to 80%IACS, and the ductility is larger than or equal to 6%. According to the method, the nanometer particle enhanced copper-based composite material high in strength and good in conductivity is prepared.
Description
Technical field
The present invention relates to a kind of Cu-base composites are and in particular to a kind of Second Phase Particle through-thickness cyclically-varying
Cu-base composites.
Background technology
Copper and Cu alloy material are a kind of important nonferrous materials, due to having excellent physical and mechanical properties,
Exist in the industry and be widely applied.But the intensity of fine copper and thermostability are not enough, and degenerate state tensile strength is about 209mpa, cold change
After shape, the intensity of material can reach 400mpa, but elongation percentage is low, and cold working effect is quickly in subsequent drawing process
Disappear it is impossible to meet the part using at high temperature.Dispersion strengthening copper alloy is with nanoscale refractory metal particulate or pottery
Grain is as the Cu-base composites strengthening phase.Second Phase Particle diameter is generally less than 100nm, and the electric conductivity of alloy is affected not
Greatly, and tiny Second Phase Particle can stop the movement of dislocation and the generation of recrystallization, alloy shows high intensity and height
Softening temperature.Second Phase Particle typically has oxide, refractory metal etc..
The method preparing such material at present mainly has internal oxidation, powder metallurgy process, Mechanical Alloying and electricity
Beamlet physical vaporous deposition etc..Internal oxidation is to occur selective oxidation to form oxygen using aluminum in albronze under hypoxia condition
The technique changing aluminum second phase particles, this technique is currently used for preparation cu-al2o3The main technique of dispersion strengthening composites, system
Standby material property is good, but this technique haves the shortcomings that also to there is complex procedures, cycle length, high cost.Powder metallurgic method is
By the copper powder of certain proportioning with enhancing particle through mechanical mixture, molding, sinter under the conditions of vacuum or protective atmosphere, multiple pressure, multiple
Burn the technique to prepare material.Although this technique can prepare the composite that various sizes strengthen particle distribution, also exist
The poor mechanical property of composite of preparation, operation are many, high cost shortcoming.Mechanical Alloying is to adopt high energy ball mill
By copper powder with strengthen mix particles uniform after, molding, sinter under the conditions of vacuum or protective atmosphere, multiple press, resintering is preparing material
Technique.This technique there is also that poor mechanical property, operation be many and the shortcoming of high cost.Electro beam physics vapour deposition technique be with
Electron beam is thermal source, heats target, evaporation, deposits on substrate, and cooling separates, the technique obtaining sheet material.With above several works
Skill is compared, and this technique has the characteristics that operation is simple, low cost.At present, it has been reported that adopting electron beam physical vapor in document
Depositing operation is prepared for copper-carbonization molybdenum composite material, and its tensile strength is 486mpa, and electrical conductivity is 82%iacs, but elongation percentage
For 3.9%.But this material with compared with the requirement to contact material for the growing electric and electronic technology, material comprehensive
Can be still not high enough, and in material, molybdenum carbide particles are to be uniformly distributed.Theoretical research shows, suitable Second Phase Particle non-all
Even distribution can obtain the more excellent material of performance.In consideration of it, the present invention has prepared nanoparticle by controlling technological parameter
The Cu-base composites of through-thickness periodic distribution, this material has more excellent combination property.
Content of the invention
It is an object of the invention to provide a kind of Cu-base composites with excellent mechanical performance, electrical property.
The Cu-base composites of indication of the present invention, Second Phase Particle volume content is 0.4-2%, and Second Phase Particle content exists
In matrix, through-thickness is in periodic distribution, and Second Phase Particle is smaller in size than 50nm, and Second Phase Particle includes refractory metal, oxygen
Compound etc..Here refractory metal includes mo, nb etc., and oxide includes al2o3、y2o3Deng.
For achieving the above object, the present invention adopts the following technical scheme that.
A kind of preparation method of Cu-base composites, the method comprising the steps of:
(1) adopt electro beam physics vapour deposition equipment, copper ingot material and the second phase material are respectively put into vacuum interior
In two crucibles, and put stratum disjunctum raw material on copper ingot material；Described second phase material is mo, nb, al2o3Or y2o3；
(2) vacuum chamber, evacuation are shut；Starting substrate rotating device makes substrate rotate, and heats substrate, makes substrate temperature
For 600-900 DEG C (preferably 650-700 DEG C)；
(3) when vacuum reaches 1 × 10-2During below pa, open the isolation baffle plate between substrate and crucible, open electronics
Rifle, electron gun launching electronics line, the stratum disjunctum raw material above Heated Copper ingot, on substrate, deposition obtains stratum disjunctum；
(4) after stratum disjunctum deposition finishes, electronic beam current Heated Copper ingot and second phase material respectively of electron gun transmitting, its
In with constant line Heated Copper ingot, the second phase material is heated with periodically variable line, Copper base material is deposited on stratum disjunctum
Material, when deposit thickness reaches desired thickness, closes electron gun, pulls on isolation baffle plate, stops substrate heating and rotates；
(5) when substrate temperature is cooled to less than 200 DEG C, stop evacuation, take off substrate, separate and obtain sedimentary, as
Described Cu-base composites.
In described step (1), described stratum disjunctum raw material is caf2Or zro2.
In described step (2), the rotary speed of substrate is 2-40rev/min, preferably 8～36rev/min.
In described step (4), described with periodically variable line heat the second phase material, described periodically variable bundle
Stream refers to that cycle period changes line size according to the following steps:
A, line are gradually increased to ma from 0a；The scope of m is 1～1.8；
B, line gradually decrease to 0.2a from ma；
C, line are gradually increased to ma from 0.2a；
D, repeat step b～c；
The described speed increasing or reducing is generally 0.5～4a/min
In described step (4), with constant line Heated Copper ingot, its line size is 1.4a.
In described step (4), general pass through to change sedimentation time and electronic beam current size control deposition materials thickness and
Thing phase composition.
The present invention also provides the Cu-base composites preparing according to the method described above.
Described Cu-base composites contain Second Phase Particle, and described Second Phase Particle is mo, nb, al2o3Or y2o3, second
The average external volume content of phase granule is 0.4-2%, and Second Phase Particle content is in periodically in Cu-base composites through-thickness
Distribution, Second Phase Particle is smaller in size than 50nm.
The mensure of described volume content passes through first quality measurement content, is then converted to volume content, this is this area skill
Detection method known to art personnel.
The performance indications of the Cu-base composites of present invention preparation are: tensile strength rm >=500mpa, yield strength rp0.2
>=460mpa, elongation percentage >=6%, electrical conductivity >=80%iacs.
Compared with prior art beneficial effect is the present invention:
The present invention adopts periodically variable line heating deposition second phase material, and the content making Second Phase Particle is in cuprio
Composite through-thickness is in periodic distribution, the Cu-base composites tensile strength rm >=500mpa obtaining, yield strength
rp0.2>=460mpa, elongation percentage >=6%, electrical conductivity >=80%iacs, and the room-temperature yield strength of fine copper is 33mpa, tension is strong
Spend for 209mpa.
Brief description
Fig. 1 is the Cu-base composites section tem photo of embodiment 1 preparation.
Fig. 2 is enlarged drawing at a in Fig. 1.
Specific embodiment
Below by preferred embodiment, technical scheme is described further, but should not be construed as to this
The restriction of invention protection domain.
Electro beam physics vapour deposition equipment used by the embodiment of the present invention is gekont l-5
Embodiment 1:
Copper ingot material and molybdenum ingot are respectively put in two indoor crucibles of vacuum, put 5g caf on copper ingot material2；
Shut vacuum chamber, start evacuation；Starting tumbler makes substrate rotate with the speed of 10rev/min, and opens substrate heating
Device, heating substrate temperature makes it stable at 700 DEG C；When vacuum reaches 1 × 10-2During pa, open between substrate and crucible
Isolation baffle plate, unlatching electron gun, deposition separating layer caf2；Then with 1.4a line constant Heated Copper ingot, with line size
0.2-1.2a heats molybdenum ingot, and the line that during deposition, heating molybdenum is expected surely first gradually increases to 1.2a from 0a, more gradually subtracts from 1.2a
Little then progressively increase to 1.2a from 0.2a to 0.2a, repeat said process and terminate until preparation process, the line increaseing or decreasing
Speed is 2a/min.After deposition 1h terminates, close electron gun, pull on baffle plate, close heater, close substrate rotating device；
When substrate temperature drops to below 200 DEG C, open vacuum chamber, take off substrate, separate and obtain thickness 0.3mm, diameter 1000mm's
Cu-base composites.In the composite of preparation, the average external volume content of molybdenum is 1.2vol%, according to national standard gb/t
228.1-2010 Mechanics Performance Testing is carried out to final products, its yield strength rp0.2=470mpa, tensile strength rm=
530mpa, elongation percentage 12%.With four probe method, the electrical conductivity of material is detected, its electrical conductivity is 82%iacs.Fig. 1 is system
Standby Cu-base composites section tem photo, Fig. 2 is the enlarged drawing in figure a.It can be seen that, thickness direction exists periodically
Structure, at black wire position, mo granule is big, content is big, and between black wire position, mo granule is little, content is few, and mo particle size is little
In 50nm.
Embodiment 2:
Copper ingot material and niobium ingot are respectively put in two indoor crucibles of vacuum, put 5g caf on copper ingot material2；
Shut vacuum chamber, start evacuation；Starting tumbler makes substrate rotate with the speed of 20rev/min, and opens substrate heating
Device, heating substrate temperature makes it stable at 700 DEG C；When vacuum reaches 1 × 10-2During pa, open between substrate and crucible
Isolation baffle plate, unlatching electron gun, deposition separating layer caf2；Then with 1.4a line constant Heated Copper ingot, with line size
0.2-1.5a heats niobium ingot, and the line heating niobium ingot during deposition first gradually increases to 1.5a from 0a, more gradually subtracts from 1.5a
Little then progressively increase to 1.5a from 0.2a to 0.2a, repeat said process and terminate until preparation process, the line increaseing or decreasing
Speed is 4a/min.After deposition 1h terminates, close electron gun, pull on baffle plate, close heater, close substrate rotating device；
When substrate temperature drops to below 200 DEG C, open vacuum chamber, take off substrate, separate and obtain thickness 0.3mm, diameter 1000mm's
Cu-base composites.In the composite of preparation, the average external volume content of niobium is 1.3vol%, according to national standard gb/t
228.1-2010 Mechanics Performance Testing is carried out to final products, its yield strength rp0.2=490mpa, tensile strength rm=
560mpa, elongation percentage 10%.With four probe method, the electrical conductivity of material is detected, its electrical conductivity is 85%iacs.
Embodiment 3:
Copper ingot material and yittrium oxide ingot are respectively put in two indoor crucibles of vacuum, on copper ingot material, put 5g
caf2；Shut vacuum chamber, start evacuation；Starting tumbler makes substrate rotate with the speed of 8rev/min, and opens substrate
Heater, heating substrate temperature makes it stable at 650 DEG C；When vacuum reaches 1 × 10-2During pa, open substrate and crucible it
Between isolation baffle plate, open electron gun, deposition separating layer caf2；Then with 1.4a line constant Heated Copper ingot, big with line
Little 0.2-1a heated oxide yttrium ingot, during deposition, the line of heated oxide yttrium ingot first gradually increases to 1a from 0a, then from 1a by
Gradually it is reduced to 0.2a, then progressively increases to 1a from 0.2a, repeat said process and terminate until preparation process, the bundle increaseing or decreasing
Flow velocity rate is 1a/min.After deposition 1h terminates, close electron gun, pull on baffle plate, close heater, close substrate rotating dress
Put；When substrate temperature drops to below 200 DEG C, open vacuum chamber, take off substrate, separate and obtain thickness 0.3mm, diameter 1000mm
Cu-base composites.The average external volume content of the composite yittrium oxide of preparation is 0.4vol%, according to national standard gb/t
228.1-2010 Mechanics Performance Testing is carried out to final products, its yield strength rp0.2=470mpa, tensile strength rm=
530mpa, elongation percentage 15%.With four probe method, the electrical conductivity of material is detected, its electrical conductivity is 90%iacs.
Embodiment 4:
Copper ingot material and aluminium oxide ingot are respectively put in two indoor crucibles of vacuum, on copper ingot material, put 5g
caf2；Shut vacuum chamber, start evacuation；Starting tumbler makes substrate rotate with the speed of 36rev/min, and opens substrate
Heater, heating substrate temperature makes it stable at 700 DEG C；When vacuum reaches 1 × 10-2During pa, open substrate and crucible it
Between isolation baffle plate, open electron gun, deposition separating layer caf2；Then with 1.4a line constant Heated Copper ingot, big with line
Little 0.2-1.8a heated oxide aluminium ingot material, during deposition, the line of heated oxide aluminium ingot material first gradually increases to 1.8a from 0a, then from
1.8a gradually decreases to 0.2a, then progressively increases to 1.8a from 0.2a, repeats said process and terminates until preparation process, increase or
The line speed reducing is 0.5a/min.After deposition 1h terminates, close electron gun, pull on baffle plate, close heater, close base
Plate rotary apparatuss；When substrate temperature drops to below 200 DEG C, open vacuum chamber, take off substrate, separate and obtain thickness 0.3mm, directly
The Cu-base composites of footpath 1000mm.In the composite of preparation, the average external volume content of aluminium oxide is 2vol%, according to country
Standard gb/t 228.1-2010 carries out Mechanics Performance Testing to final products, its yield strength rp0.2=500mpa, tensile strength
Rm=540mpa, elongation percentage 6%.With four probe method, the electrical conductivity of material is detected, its electrical conductivity is 80%iacs.
Claims (6)
1. a kind of Cu-base composites are it is characterised in that described Cu-base composites contain Second Phase Particle, described second phase
Grain is mo, nb, al2o3Or y2o3, the average external volume content of Second Phase Particle is 0.4-2%, and Second Phase Particle content is multiple in cuprio
Condensation material through-thickness is in periodic distribution, and Second Phase Particle is smaller in size than 50nm；
The preparation method of described Cu-base composites comprises the following steps:
(1) adopt electro beam physics vapour deposition equipment, copper ingot material and the second phase material are respectively put into indoor two of vacuum
In crucible, and put stratum disjunctum raw material on copper ingot material；Described second phase material is mo, nb, al2o3Or y2o3；
(2) vacuum chamber, evacuation are shut；Starting substrate rotating device makes substrate rotate, and heats substrate, makes the substrate temperature be
600-900℃；
(3) when vacuum reaches 1 × 10-2During below pa, open the isolation baffle plate between substrate and crucible, open electron gun, electricity
Sub- rifle launching electronics line, the stratum disjunctum raw material above Heated Copper ingot, on substrate, deposition obtains stratum disjunctum；
(4) after stratum disjunctum deposition finishes, electronic beam current respectively Heated Copper ingot and second phase material of electron gun transmitting, wherein with
Constant line Heated Copper ingot, heats the second phase material with periodically variable line, deposits copper-based material in stratum disjunctum, when
When deposit thickness reaches desired thickness, close electron gun, pull on isolation baffle plate, stop substrate heating and rotate；
(5) when substrate temperature is cooled to less than 200 DEG C, stop evacuation, take off substrate, separate and obtain sedimentary, as described
Cu-base composites.
2. Cu-base composites as claimed in claim 1 are it is characterised in that in described step (1), described stratum disjunctum raw material is
caf2Or zro2.
3. Cu-base composites as claimed in claim 1 are it is characterised in that in described step (2), the rotary speed of substrate is
2-40rev/min.
4. Cu-base composites as claimed in claim 1 are it is characterised in that in described step (4), described with cyclically-varying
Line heat the second phase material, described periodically variable line refer to line size according to the following steps cycle period change:
A, line are gradually increased to ma from 0a；The scope of m is 1～1.8；
B, line gradually decrease to 0.2a from ma；
C, line are gradually increased to ma from 0.2a；
D, repeat step b～c.
5. Cu-base composites as claimed in claim 4 it is characterised in that described line increase or reduce speed be 0.5～
4a/min.
6. Cu-base composites as claimed in claim 1 are it is characterised in that the performance indications of described Cu-base composites are: anti-
Tensile strength rm >=500mpa, yield strength rp0.2>=460mpa, elongation percentage >=6%, electrical conductivity >=80%iacs.
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| CN108517438A (en) * | 2018-05-22 | 2018-09-11 | 芜湖卓越线束系统有限公司 | A kind of alloy material for high-strength wearable Wiring harness terminal |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1404943A (en) * | 2002-11-05 | 2003-03-26 | 清华大学 | Grain-rein forced gradient composite material and preparation method thereof |
| CN1702191A (en) * | 2005-05-27 | 2005-11-30 | 哈尔滨工业大学 | Method for preparing alloy sheet |
| CN103643075A (en) * | 2013-11-29 | 2014-03-19 | 浙江工业大学 | Nano-particle reinforced copper-based composite material and preparation method thereof |
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| US20070251818A1 (en) * | 2006-05-01 | 2007-11-01 | Wuwen Yi | Copper physical vapor deposition targets and methods of making copper physical vapor deposition targets |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1404943A (en) * | 2002-11-05 | 2003-03-26 | 清华大学 | Grain-rein forced gradient composite material and preparation method thereof |
| CN1702191A (en) * | 2005-05-27 | 2005-11-30 | 哈尔滨工业大学 | Method for preparing alloy sheet |
| CN103643075A (en) * | 2013-11-29 | 2014-03-19 | 浙江工业大学 | Nano-particle reinforced copper-based composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| EB-PVD制备Cu/Mo-Ti微叠层复合材料及性能研究;卜范雨等;《热加工工艺》;20140331;第43卷(第6期);第1-3页 * |
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