CN107574332A - A kind of internal oxidation production alumina dispersion-strenghtened copper alloy oxidant and preparation method thereof - Google Patents
A kind of internal oxidation production alumina dispersion-strenghtened copper alloy oxidant and preparation method thereof Download PDFInfo
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- CN107574332A CN107574332A CN201710831296.5A CN201710831296A CN107574332A CN 107574332 A CN107574332 A CN 107574332A CN 201710831296 A CN201710831296 A CN 201710831296A CN 107574332 A CN107574332 A CN 107574332A
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Abstract
The present invention relates to a kind of internal oxidation production alumina dispersion-strenghtened copper alloy oxidant and preparation method thereof, belong to powder metallurgy powder-making technique field.Al content is 0.1~1.2wt% (percentage by weight) in the oxidant of the present invention, and hydrogen loss value is 8.0~11.1wt%, and average grain diameter is 1.0~8.0 μm.Methods described is included using the Cu Al alloyed powders of water atomization or nitrogen atomization as raw material, through the process such as peroxidating, calcining, broken, granularity regulation and control, prepare good dispersion, even particle size distribution, ultra-fine oxidant, alumina dispersion-strenghtened copper alloy is produced for internal oxidition raw material guarantee is provided, and then improve the combination property with its prepared alumina dispersion-strenghtened copper alloy.The inventive method undergoes technological transformation and extended on the basis of the existing working condition of enterprise, easily accomplishes scale production, and production efficiency is high, effect is good.
Description
Technical field
The invention belongs to copper alloy powder metallurgy powder-making technique field, and in particular to a kind of internal oxidation production aluminum oxide is more
Strengthened copper alloy oxidant and preparation method thereof is dissipated,
Technical background
Alumina dispersion-strenghtened copper alloy is a kind of excellent high-strength, high to lead alloy material.Due to the nanometer of Dispersed precipitate
Level Al2O3Particle serves the effect of dispersion-strengtherning to Copper substrate, and therefore, the alloy has high intensity, high rigidity, high conductivity
And the characteristic such as high softening temperature, there is tissue stabilization, high without phase transformation, yield strength and tensile strength.Normal temperature hardness is high,
Hardness is small with the rise fall of temperature, and high-temperature creep resistance is good.Heat, conductivity are high.Processing characteristics is excellent, softening temperature
Up to 930 DEG C of degree.As copper alloy with high strength and high conductivity, have both high intensity, highly conductive and thermal conductive resin, wear-resisting antiknock cracking resistance, resistance to
The combination properties such as corrosion.Dispersion copper can be widely applied to large scale integrated circuit, high-speed train contact wire, switch and touch bridge and continuous casting
The copper alloy with high strength and high conductivity material that the fields such as steel crystallizer need, by suitably being adjusted to disperse copper component, can be used as electric welding machine
Electrode, low-voltage electrical apparatus touch the various contact materials such as bridge, short-circuited conducting sleeve.
Internal oxidation is to be used to prepare Al2O3The main method of dispersion strengthening copper alloy, due to Al2O3Particle and copper melts
It is almost nonwetting, therefore Al made from internal oxidation2O3Particle size is tiny and is evenly distributed, what profit was prepared in this way
Cu-Al2O3Disperse copper alloy has excellent combination property.Its specific preparation process is as follows：Cu-Al (0.1~
1.2wt%) melting → water atomization or nitrogen atomization powder → with oxidant mix → closed container internal oxidition → hydrogen in dry
And reduce → jacket processing → compacting (high temperature insostatic pressing (HIP) or hot pressing etc.) → hot extrusion molding → follow-up finishing → product inspection →
Product packaging.
The correlated performance of oxidant will influence Al2O3The generation of particle, (intensity, hardness, led so as to influence the performance of material
Electric rate etc.).Such as cuprous as oxidant by the use of pure zirconia, the oxidant is become after being reduced as without the weak fine copper phase for strengthening particle.
The oxidant of salic particle mainly has following preparation method：SCM Corporation of the U.S. (US3779714) uses micron order Cu2O and
Al(NO3)3Solution mixes, and then dries and calcines, finally sieves, and prepares the micron order Cu of the salic particle of -325 purposes2O
Oxidant, but its raw material is Cu2O and Al (NO3)3, and be not directed to accurately control the particle mean size of final oxidant
System.Zhonglu Luoyang Copper Industry Co., Ltd. (CN2004100298136.0) uses the Cu-Al powder after water atomization as raw material, in sky
Toast in gas, and heated in a nitrogen atmosphere, prepare oxidant, but the granularity of oxidant is not controlled, also can not
Ensure the oxygen content of oxidant.No.China Shipbuilding Industry Group Co.ltd. 725 Institute (CN200610128421.8) uses
Cu-Al powder all aoxidizes, by controlling degree of oxidation, then direct internal oxidition, the processing compound can not accurately controlling oxygen content,
And then influence the formation of alumina particle in Copper substrate.
The content of the invention
The main object of the present invention is to provide a kind of internal oxidation production alumina dispersion-strenghtened copper alloy oxidant, holds
Easily accomplish scale production, and production efficiency is high, effect is good.
To reach above-mentioned purpose, the present invention uses following technical scheme：
A kind of internal oxidation produces alumina dispersion-strenghtened copper alloy oxidant, has following characteristic：
(1) composition：Al content：0.1~1.2% (percentage by weight)；
(2) hydrogen loss value is：8~11%；
(3) oxidizing agent pellets：Molybdenum mean particle size D is less than 8 μm；Average grain diameter is preferably 1~3 μm；
Another object of the present invention is to provide a kind of internal oxidation production alumina dispersion-strenghtened copper alloy oxidant
Preparation method, comprise the following steps：
(1) raw material prepares：Water atomization or nitrogen atomization produce Cu-Al alloyed powders；
(2) once oxidation：The Cu-Al alloyed powders are heated in air atmosphere using oxidation furnaces；
(3) once calcine：Step (2) resulting material is placed in closed container under protective atmosphere and calcined；
(4) primary fragmentation：Material after the once calcining is crushed；
(5) secondary oxidation：By it is described it is broken after material reheating in air atmosphere；
(6) secondary clacining：Material after the reheating is placed in closed container under protective atmosphere and calcined；
(7) second-time breakage：Material after the secondary clacining is crushed；
(8) Oxidizer Particle Size regulates and controls：Material after told second-time breakage is subjected to broken classification, obtains internal oxidation production
Alumina dispersion-strenghtened copper alloy oxidant.
Further, in step (1), the aluminium contents of the Cu-Al alloyed powders is 0.1~1.2wt%, granularity requirements 80
Mesh.
Further, in step (2), described raw material Cu-Al alloyed powders, set in kiln, resistance furnace or other oxidations
Aoxidized under standby middle air atmosphere, 400~650 DEG C of oxidizing temperature, oxidization time 0.5-1 hours；Or oxidizing temperature be 400~
650 DEG C, oxidization time 4-6 hours, then directly carry out step (6), (7), (8).When temperature is less than 400 DEG C, Cu-Al alloyed powders
Oxygenation effect is too slow, is unfavorable for large quantities of production.When temperature is higher than 650 DEG C, the oxidation of Cu-Al alloyed powders is too fast, is easily formed big
The alumina particle of size, while the caking phenomenon of Cu-Al alloyed powders is serious, is unfavorable for follow-up crush.
Further, in step (3), the material that step (2) obtains is placed in closed container, in resistance furnace under protective atmosphere
Interior calcining, 700~900 DEG C of calcining heat, it is incubated 1-3 hours.When temperature is less than 700 DEG C, oxygen expands in Cu-Al alloyed powders after oxidation
Dissipate too slowly, cupric oxide conversion is incomplete.When temperature is higher than 900 DEG C, Cu-Al alloyed powders caking phenomenon is serious after oxidation, block
Hardness is high, easily wears crushing mechanism, reduces production efficiency.
Further, in step (4), the material that step (3) obtains is crushed, improves the oxygenation efficiency of secondary oxidation,
Oxidation material after broken is 100 mesh powders, and hydrogen loss value is 4~6%.
Further, in step (5), by step (4) obtain material, in kiln, resistance furnace or other oxidation furnaces
Aoxidized under middle air atmosphere, 400~650 DEG C of oxidizing temperature, oxidization time 30-120 minutes.
Further, in step (6), the material that step (5) obtains is placed in closed container, in resistance furnace under protective atmosphere
Interior calcining, 700~900 DEG C of calcining heat, it is incubated 1-3 hours.
Further, in step (7), the material that step (6) obtains is crushed, the material after crushing is the powder of -100 mesh
End.
In step (8), the second-time breakage oxidation that step (7) is obtained carries out the separation wheel of broken classification, wherein equipment
Rotating speed is 2500~7000 revs/min, and grinding cavity pressure is 0.1~1MPa, and powder feeding rate is 0.1~20kg/ hours, is obtained interior
Oxidizing process produces alumina dispersion-strenghtened copper alloy oxidant.
The preparation method of the present invention, using water atomization or the Cu-Al alloy powder raw materials of nitrogen atomization, pass through tradition or modern
Powder metallurgical technique obtains well dispersed, ultra-fine internal oxidation production alumina dispersion-strenghtened copper alloy oxidant, should
Method can be implemented in existing powder metallurgy production line, easily accomplish scale production, and production efficiency is high.
Good dispersion, ultra-fine internal oxidation production alumina dispersion-strenghtened copper alloy oxidant in the present invention, it is
Internal oxidition production alumina dispersion-strenghtened copper alloy provides raw material guarantee, and then improves prepared alumina dispersion-strenghtened with it
The combination property of copper alloy, promote the development of Domestic Automotive Industry, electronics industry middle and high end parts.
Brief description of the drawings
Fig. 1 is the preparation method technological process that internal oxidation of the present invention produces alumina dispersion-strenghtened copper alloy oxidant
Figure.
Embodiment
, will not changing right of the present invention the following detailed description of embodiments of the invention, but the invention is not limited in this
Suitably it is adjusted in the range of asking, can equally implements the present invention.
The preparation method technological process of the internal oxidation production alumina dispersion-strenghtened copper alloy oxidant of the present invention is such as
Shown in Fig. 1, in figure：1 raw material prepares；2 once oxidations；3 once calcine；4 primary fragmentations；5 once oxidations；6 secondary clacinings；7 two
It is secondary broken；8 Oxidizer Particle Sizes regulate and control.
Embodiment 1
A kind of internal oxidation produces alumina dispersion-strenghtened copper alloy oxidant, and the oxidant includes following components and contained
Measure (weight)：Al：0.6wt%, hydrogen loss value：10.2wt%.Its preparation technology comprises the following steps：
(1) raw material prepares：The Cu-Al alloyed powders produced using water atomization or nitrogen atomization, screen the powder below 80 mesh
End is used as raw material, Al content 0.6wt%, and granular size is -80 mesh；
(2) once oxidation：20 kilograms of material powder in step (1) is taken, is placed in kiln, it is in air atmosphere, right
Material powder is warming up to 600 DEG C, and insulation is come out of the stove after 1 hour.
(3) once calcine：The once oxidation material is placed in closed container, forvacuum is carried out to closed container, is filled
Enter argon gas, keep argon gas in closed container to be in slight positive pressure state；Then closed container is placed in resistance furnace and is warming up to 800
DEG C, 2 hours are incubated, is come out of the stove after temperature decline.
(4) primary fragmentation：Once calcining material takes out by described in, carries out Mechanical Crushing to it using disintegrating machine, then sieves,
The calcined oxide agent of -100 purpose is obtained, measures its hydrogen loss value as 5.2%；
(5) secondary oxidation：Powder after the primary fragmentation is placed in kiln, in air atmosphere, to raw material
Powder is warming up to 600 DEG C, and insulation is come out of the stove after 1 hour；
(6) secondary clacining：The secondary oxidation material is placed in closed container, forvacuum is carried out to closed container, is filled
Enter argon gas, keep argon gas in closed container to be in slight positive pressure state；Then closed container is placed in resistance furnace and is warming up to 800
DEG C, 2 hours are incubated, is come out of the stove after temperature decline.
(7) second-time breakage：Once calcining material takes out by described in, carries out Mechanical Crushing to it using disintegrating machine, then sieves,
Obtain the calcined oxide agent of -100 purpose；
(8) Oxidizer Particle Size regulates and controls：Oxidation material after told second-time breakage is carried out to the sorting of broken classification, wherein equipment
Wheel speed is 5000 revs/min, and grinding cavity pressure is 0.6MPa, and powder feeding rate is 10kg/ hours, obtains internal oxidation production oxygen
Change aluminium dispersion strengthening copper alloy oxidant.
Good dispersion, even particle size distribution, ultra-fine internal oxidation production alumina dispersion-strenghtened copper is made in the present embodiment
Alloy oxidant, its leading indicator are：Al：0.6wt%, hydrogen loss value are 10.2%, and particle mean size is 2.827 μm.
Embodiment 2
A kind of internal oxidation produces alumina dispersion-strenghtened copper alloy oxidant, and the oxidant includes following components and contained
Measure (weight)：Al：0.1wt%, hydrogen loss value：9.6wt%.Its preparation technology comprises the following steps：
(1) raw material prepares：The Cu-Al alloyed powders produced using water atomization or nitrogen atomization, screen the powder below 80 mesh
End is used as raw material, Al content 0.1wt%, and granular size is -80 mesh；
(2) once oxidation：20 kilograms of material powder in step (1) is taken, is placed in kiln, it is in air atmosphere, right
Material powder is warming up to 500 DEG C, and insulation is come out of the stove after 1 hour.
(3) once calcine：The once oxidation material is placed in closed container, forvacuum is carried out to closed container, is filled
Enter argon gas, keep argon gas in closed container to be in slight positive pressure state；Then closed container is placed in resistance furnace and is warming up to 700
DEG C, 2 hours are incubated, is come out of the stove after temperature decline.
(4) primary fragmentation：Once calcining material takes out by described in, carries out Mechanical Crushing to it using disintegrating machine, then sieves,
The calcined oxide agent of -100 purpose is obtained, measures its hydrogen loss value as 4.7%；
(5) secondary oxidation：Powder after the primary fragmentation is placed in kiln, in air atmosphere, to raw material
Powder is warming up to 500 DEG C, and insulation is come out of the stove after 1 hour；
(6) secondary clacining：The secondary oxidation material is placed in closed container, forvacuum is carried out to closed container, is filled
Enter argon gas, keep argon gas in closed container to be in slight positive pressure state；Then closed container is placed in resistance furnace and is warming up to 700
DEG C, 2 hours are incubated, is come out of the stove after temperature decline.
(7) second-time breakage：Once calcining material takes out by described in, carries out Mechanical Crushing to it using disintegrating machine, then sieves,
Obtain the calcined oxide agent of -100 purpose；
(8) Oxidizer Particle Size regulates and controls：Oxidation material after told second-time breakage is carried out to the sorting of broken classification, wherein equipment
Wheel speed is 5000 revs/min, and grinding cavity pressure is 0.8MPa, and powder feeding rate is 6kg/ hours, obtains internal oxidation production oxygen
Change aluminium dispersion strengthening copper alloy oxidant.
Good dispersion, even particle size distribution, ultra-fine internal oxidation production alumina dispersion-strenghtened copper is made in the present embodiment
Alloy oxidant, its leading indicator are：Al：0.1wt%, hydrogen loss value are 9.6%, and particle mean size is 1.741 μm.
Embodiment 3
A kind of internal oxidation produces alumina dispersion-strenghtened copper alloy oxidant, and the oxidant includes following components and contained
Measure (weight)：Al：0.6wt%, hydrogen loss value：8.0wt%.Its preparation technology comprises the following steps：
(1) raw material prepares：The Cu-Al alloyed powders produced using water atomization or nitrogen atomization, screen the powder below 80 mesh
End is used as raw material, Al content 0.6wt%, and granular size is -80 mesh；
(2) aoxidize：30 kilograms of material powder in step (1) is taken, is placed in kiln, in air atmosphere, to raw material
Powder is warming up to 650 DEG C, and insulation is come out of the stove after 10 hours.
(3) calcine：The oxidation material is placed in closed container, forvacuum is carried out to closed container, is filled with argon gas, is protected
Hold argon gas in closed container and be in slight positive pressure state；Then closed container is placed in resistance furnace and is warming up to 850 DEG C, insulation 3 is small
When, come out of the stove after temperature decline.
(4) crush：The calcining material is taken out, Mechanical Crushing is carried out to it using disintegrating machine, then sieving, obtains -100
Calcined oxide agent of purpose；
(5) Oxidizer Particle Size regulates and controls：Oxidation material after told second-time breakage is carried out to the sorting of broken classification, wherein equipment
Wheel speed is 3500 revs/min, and grinding cavity pressure is 0.8MPa, and powder feeding rate is 4kg/ hours, obtains internal oxidation production oxygen
Change aluminium dispersion strengthening copper alloy oxidant.
Good dispersion, even particle size distribution, ultra-fine internal oxidation production alumina dispersion-strenghtened copper is made in the present embodiment
Alloy oxidant, its leading indicator are：Al：0.6wt%, hydrogen loss value are 8.0%, and particle mean size is 4.088 μm.
Claims (10)
1. a kind of internal oxidation produces alumina dispersion-strenghtened copper alloy oxidant, it is characterised in that
(1) composition：Al content：0.1~1.2% (percentage by weight)；
(2) hydrogen loss value is：8~11%；
(3) oxidizing agent pellets：Alumina particles average grain diameter：1.0~8.0 μm.
A kind of 2. preparation method of internal oxidation production alumina dispersion-strenghtened copper alloy oxidant, it is characterised in that including
Following steps：
(1) raw material prepares：Water atomization or nitrogen atomization produce Cu-Al alloyed powders；
(2) once oxidation：The Cu-Al alloyed powders are heated in air atmosphere using oxidation furnaces；
(3) once calcine：Step (2) resulting material is placed in closed container under protective atmosphere and calcined；
(4) primary fragmentation：Material after the once calcining is crushed；
(5) secondary oxidation：By it is described it is broken after material reheating in air atmosphere；
(6) secondary clacining：Material after the reheating is placed in closed container under protective atmosphere and calcined；
(7) second-time breakage：Material after the secondary clacining is crushed；
(8) Oxidizer Particle Size regulates and controls：Material after told second-time breakage is subjected to broken classification, obtains internal oxidation production oxidation
Aluminium dispersion strengthening copper alloy oxidant.
3. according to the method for claim 2, it is characterised in that：Aluminium content is in Cu-Al alloyed powders described in step (1)
0.1~1.2wt%, granularity requirements are 80 mesh.
4. according to the method for claim 2, it is characterised in that：Oxidation described in step (2) is in kiln or resistance
Aoxidized in stove under air atmosphere, 400~650 DEG C of oxidizing temperature, oxidization time 0.5-1 hours；Or oxidizing temperature be 400~
650 DEG C, oxidization time 4-6 hours, then directly carry out step (6), (7), (8).
5. according to the method for claim 2, it is characterised in that：Once calcine described in step (3) and carried out in resistance furnace,
700~900 DEG C of calcining heat, it is incubated 1-3 hours.
6. according to the method for claim 2, it is characterised in that：Material after being crushed in step (4) is 100 mesh powders,
Hydrogen loss value is 4~6%.
7. according to the method for claim 2, it is characterised in that step carries out oxygen in (5) in kiln or resistance furnace
Change, 400~650 DEG C of oxidizing temperature, oxidization time 30-120 minutes.
8. according to the method for claim 2, it is characterised in that：Secondary clacining is carried out in resistance furnace described in step (6),
700~900 DEG C of calcining heat, it is incubated 1-3 hours.
9. according to the method for claim 2, it is characterised in that：Material in step (7) after second-time breakage is the powder of 100 mesh
End.
10. according to the method for claim 2, it is characterised in that：In step (8), the equipment of the broken classification use
It is 2500~7000 revs/min to sort wheel speed, and grinding cavity pressure is 0.1~1MPa, and powder feeding rate is 0.1~20kg/ hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112342A (en) * | 2018-08-21 | 2019-01-01 | 中山麓科睿材科技有限公司 | A kind of preparation process of ODS copper-base alloys alloy inner oxidation oxidant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3779714A (en) * | 1972-01-13 | 1973-12-18 | Scm Corp | Dispersion strengthening of metals by internal oxidation |
| CN1563447A (en) * | 2004-03-30 | 2005-01-12 | 洛阳铜加工集团有限责任公司 | Dispersion strengthened copper alloy, and preparing technical method |
| CN1940116A (en) * | 2005-09-30 | 2007-04-04 | 中南大学 | Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al2O3 alloy and its production |
-
2017
- 2017-09-15 CN CN201710831296.5A patent/CN107574332A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3779714A (en) * | 1972-01-13 | 1973-12-18 | Scm Corp | Dispersion strengthening of metals by internal oxidation |
| CN1563447A (en) * | 2004-03-30 | 2005-01-12 | 洛阳铜加工集团有限责任公司 | Dispersion strengthened copper alloy, and preparing technical method |
| CN1940116A (en) * | 2005-09-30 | 2007-04-04 | 中南大学 | Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al2O3 alloy and its production |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112342A (en) * | 2018-08-21 | 2019-01-01 | 中山麓科睿材科技有限公司 | A kind of preparation process of ODS copper-base alloys alloy inner oxidation oxidant |
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