CN108856725A - A kind of preparation method and application of dispersion-strengthened Cu in situ composites - Google Patents
A kind of preparation method and application of dispersion-strengthened Cu in situ composites Download PDFInfo
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- CN108856725A CN108856725A CN201810604910.9A CN201810604910A CN108856725A CN 108856725 A CN108856725 A CN 108856725A CN 201810604910 A CN201810604910 A CN 201810604910A CN 108856725 A CN108856725 A CN 108856725A
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1089—Alloys containing non-metals by partial reduction or decomposition of a solid metal compound
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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
Abstract
The invention discloses a kind of preparation methods of dispersion-strengthened Cu in situ composites, belong to technical field of composite materials, include the following steps:Step 1 weighs Cu-Al alloy powder and CuO powder, obtains mixed-powder;Mixed-powder is put into ball milling in ball mill by step 2, obtains the good powder of ball milling;The good powder of ball milling is placed in reductive heat treatment atmosphere by step 3, obtains pure alumina dispersion-strenghtened copper powder;Pure alumina dispersion-strenghtened copper powder is carried out plasma spheroidization processing, obtains spherical dispersion-strengtherning copper powder, as dispersion-strengthened Cu in situ composites by step 4.A kind of application of dispersion-strengthened Cu in situ composites the are also disclosed manufacture in complicated shape part of the invention.The present invention realizes the preparation of the aluminium oxide enhancing dispersion-strengthened Cu spherical powder of in-situ authigenic;Also, related thinking can be extended to other kinds difficult-to-machine material, have apparent practical value.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of system of dispersion-strengthened Cu in situ composites
Preparation Method and application.
Background technique
Copper has excellent conduction and heating conduction, but the intensity of fine copper is low, poor heat resistance, easily-deformable soft under high temperature
Change, causes it in the application in certain fields by biggish limitation;And aluminium oxide enhancing dispersion-strengthened Cu not only has copper itself
Good conductive and heating conduction, and mechanical property also increases substantially.
But since dispersion-strengthened Cu intensity is big, strain-hardening rate is high, non-reusable liquid forming manufactures complicated shape
The features such as part, make dispersion-strengthened Cu poor in processability, manufacture complicated shape part is extremely difficult.
Summary of the invention
Goal of the invention:Of the existing technology in order to solve the problems, such as, the present invention provides a kind of dispersion-strengthened Cu in-situ authigenic
The preparation method of composite material realizes the preparation of the aluminium oxide enhancing dispersion-strengthened Cu spherical powder of in-situ authigenic;Of the invention
Another object is that disclosing a kind of application of the manufacture of dispersion-strengthened Cu in situ composites in complicated shape part.
Technical solution:In order to achieve the above-mentioned object of the invention, the present invention adopts the following technical scheme that:
A kind of preparation method of dispersion-strengthened Cu in situ composites, includes the following steps:
Step 1 weighs Cu-Al alloy powder and CuO powder, obtains mixed-powder;
Mixed-powder is put into ball milling in ball mill by step 2, obtains the good powder of ball milling;
The good powder of ball milling is placed in reductive heat treatment atmosphere, obtains pure alumina dispersion-strenghtened copper by step 3
Powder;
Pure alumina dispersion-strenghtened copper powder is carried out plasma spheroidization processing, it is strong to obtain spherical disperse by step 4
Change copper powder, as dispersion-strengthened Cu in situ composites.
In step 1, the weight ratio of CuO powder is calculated according to the weight of Al in Cu-Al alloy powder, if using Cu-
Al mass percent is x% in Al alloy powder, then the use of the ratio of the quality of CuO powder and Cu-Al alloyed powder quality is x/
Between 31.75~x/22.22, wherein x% range is 0.25%~1%.
In step 1, the purity of Cu-Al alloy powder is 99.9%, and partial size is 40-150 μm;The purity of CuO powder is
99.5%, partial size<50μm.
In step 2, ball material mass ratio is 20~50 when ball milling:1;250~400 revs/min of drum's speed of rotation;Ball-milling Time
It is 15~40 hours;Every ball milling 30~50 minutes shuts down one minute and changes positive and negative rotation direction;The good powder shape of ball milling is in thin
Strip, about 5-20 μm of partial size.
In step 3, alumina dispersion-strenghtened copper powder is by Cu and Al after reduction treatment2O3Two kinds at being grouped as, powder
Impurity oxygen content is less than 200ppm.
In step 3, reductive heat treatment atmosphere is CO gas, and CO gas flow is 1~3 liter/min, reduction temperature 400
~500 DEG C, the recovery time is 30~50 minutes.
In step 4, spherical dispersion-strengtherning copper powder is by Cu and Al2O3Two kinds at being grouped as, Al wherein included2O3Enhance grain
Sub- 5~20nm of size, mass percent 0.47%~1.89%.
A kind of spherical dispersion-strengtherning copper powder of the preparation method preparation of the dispersion-strengthened Cu in situ composites
In the application of the complex parts using increasing material manufacturing method manufacture dispersion-strengthened Cu.
Inventive principle:The Al for generally also thering is internal oxidation to prepare2O3Dispersion-strengthened Cu composite material powder, then uses powder
It is metallurgy sintered at blocky sample, squeeze, forging, machining carry out part manufacture.Due to being limited by bulk material manufacturing process, manufacture
Complicated and heavy parts have larger difficulty.Therefore powder preparation → spheroidising → increasing material manufacturing complexity, heavy parts is proposed
Manufacturing technology scheme.Wherein, the powder of high-energy ball milling internal oxidation preparation belongs to similar principle with internal oxidation, is to utilize
CuAl+CuO reaction in-situ generates aluminium oxide, but we realize reaction using ball grinding method.Either high-energy ball milling internal oxidation
Or powder made from common internal oxidation is the powder of aspherical particle, they are not directly used for increasing material manufacturing, because
After this needs to carry out the spheroidising of powder granule, increasing material manufacturing just can be carried out.
Beneficial effect:Compared with prior art, the preparation of a kind of dispersion-strengthened Cu in situ composites of the invention
Method passes through the Al of in-situ authigenic2O3The high-energy ball milling internal oxidation of dispersion-strengthened Cu composite material powder prepares and its powder ball
Change, spheroidising is then carried out to composite material powder by plasma method, realizes the aluminium oxide enhancing disperse of in-situ authigenic
Strengthen the preparation of copper spherical powder;It is another object of the present invention to disclose a kind of dispersion-strengthened Cu in situ composites multiple
The application of the manufacture of miscellaneous Shape Parts;Also, related thinking can be extended to other kinds difficult-to-machine material, therefore, present invention tool
There is apparent practical value.
Detailed description of the invention
Fig. 1 is the process flow for preparing alumina dispersion-strenghtened copper spherical powder;
Fig. 2 is the scanning electron microscope (SEM) photograph of Cu-Al alloy powder;
Fig. 3 is the scanning electron microscope (SEM) photograph of CuO powder;
Fig. 4 is the scanning electron microscope (SEM) photograph of powder after high-energy ball milling;
Fig. 5 is the scanning electron microscope (SEM) photograph of powder after plasma spheroidization;
Fig. 6 is the X ray diffracting spectrum of carbon monoxide air-flow reduction front and back powder;Fig. 7 is before carbon monoxide air-flow restores
The transmission electron microscope picture of powder;
Fig. 8 is the transmission electron microscope picture of powder after the reduction of carbon monoxide air-flow;
Fig. 9 is the metallograph of the product manufactured in actual use of alumina dispersion-strenghtened copper spherical powder.
Specific embodiment
The present invention is further described with specific implementation example with reference to the accompanying drawing.
A kind of preparation method of dispersion-strengthened Cu in situ composites, includes the following steps:
Step 1 quantitatively weighs Cu-Al alloy powder and CuO powder, obtains mixed-powder, wherein the weight of CuO powder
It is calculated by the weight of Al in Cu-Al alloy powder;Calculating principle is so that Al in oxygen atomicity and Cu-Al alloy in CuO
Atomicity keeps ratio appropriate, and method is as follows:If the use of Al mass percent in Cu-Al alloy powder being x%, then use
The quality of CuO powder and the ratio of Cu-Al alloyed powder quality are between x/31.75~x/22.22.
Wherein, the purity of Cu-Al alloy powder is 99.9%, and Al content is mass percent 0.25%~1%, and partial size is
40-150 μm, shape is in irregular subsphaeroidal, and microscopic appearance is as shown in the SEM image of Fig. 2;The purity of CuO powder is
99.5%, partial size<50 μm, microscopic appearance is as shown in the SEM image of Fig. 3;
Mixed-powder is put into ball milling in ball mill by step 2, obtains the good powder of ball milling, such as the SEM image institute of Fig. 4
Show, after ball milling powder shape be in tiny sheet, about 5-20 μm of partial size;
The good powder of ball milling is placed in reductive heat treatment atmosphere, obtains pure alumina dispersion-strenghtened copper by step 3
Powder, powder restored before and after composition as shown in the X ray diffracting spectrum of Fig. 6, Cu is represented after reduction2The diffraction maximum of O is complete
It totally disappeared mistake, but it is observed that representing Al2O3Three characteristic diffraction peaks, illustrate to carry out after reduction treatment remaining Cu in powder2O
It is almost completely converted to Cu, and Al2O3Retained, this point is from the lattice analysis in transmission electron microscope picture shown in Fig. 7,8
Also available confirmation;
Pure alumina dispersion-strenghtened copper powder is carried out plasma spheroidization processing, it is strong to obtain spherical disperse by step 4
Change copper powder, as dispersion-strengthened Cu in situ composites, the morphology microstructure after nodularization as shown in the SEM image of Fig. 5, for compared with
For the spheric granules of rule.
Composite material powder by the preparation of high-energy ball milling internal oxidation includes Cu, Cu2O、Al2O3Three kinds of ingredients;Step 3
In, alumina dispersion-strenghtened copper powder only includes Cu and Al after reduction treatment2O3, the impurity oxygen content of powder is less than 200ppm.Through
Cross the Al that the composite material powder of high-energy ball milling internal oxidation preparation includes2O3Enhance 5~20nm of particle size, mass percent
0.47%~1.89%.
In step 2, ball material mass ratio is 20~50 when ball milling:1;250~400 revs/min of drum's speed of rotation;Ball-milling Time
It is 15~40 hours;Every ball milling 30~50 minutes shuts down one minute and changes positive and negative rotation direction.
In step 3, reductive heat treatment atmosphere is CO gas, and CO gas flow is 1~3 liter/min, reduction temperature 400
~500 DEG C, the recovery time is 30~50 minutes.
A kind of spherical dispersion-strengtherning copper powder use increasing of the preparation method preparation of dispersion-strengthened Cu in situ composites
Material manufacturing method manufactures the application of the complex parts of dispersion-strengthened Cu, and the tissue of the product manufactured in actual use of the powder is such as
Shown in Fig. 9, the tiny Al of nanoscale is uniform-distribution on Copper substrate2O3Disperse phase, it is clear that this metallographic structure is beneficial to mention
The intensity of high metal, especially elevated temperature strength, while also there is excellent thermally conductive/electric conductivity.
Method fabricated in situ using high-energy ball-milling alloying includes the dispersion-strengtherning copper powder of alumina in Nano level, then through also
Original removal residual oxygen, using the dispersion-strengthened Cu part that increases material manufacturing technology manufacture is complicated after spheroidising.Invention master
Dispersion-strengthened Cu is overcome to be unable to remelting and carry out liquid forming, elevated temperature strength to be not easy to carry out solid plastics forming, direct powder greatly
Last metallurgy cannot manufacture the problem of forming and poor in processability of large-scale part and the more low aspects of mechanical performance.Due to increasing material
The characteristics of manufacture is because of its discrete manufacture, stack shaping allows it to overcome the defect of material forming and poor processability itself, from
And become the especially difficult forming of metal material, rapidoprint for manufacturing one of most effectual way of complicated metal parts, still
It transports performance to powder and there are certain requirements, mainly the requirement to powder sphericity.In terms of powder processed, existing spherical powder
Body, which manufactures, mainly the main stream approach of the atomizing principles such as VIGA, EIGA, they be required to make the melting of metal material experience, atomization and
The process of solidification, such methods cannot achieve the result that disperse on each copper powder particle generates aluminium oxide.And the preparation of mainstream
The powder granule of the internal oxidation series methods preparation of dispersion-strengthened Cu is also the microscopic appearances such as polygon and sheet, transport property
Energy official post not can be used directly in increasing material manufacturing.The present invention is dexterously by dispersion-strengthened Cu made from high-energy ball milling internal oxidation
After powder undergoes plasma spheroidization processing, it is successfully applied to DED increasing material manufacturing, produces dispersion-strengthened Cu part.This technology energy
The excellent high intensity and softening resistant performance of dispersion-strengthened Cu are enough given full play to, and has both the structure of excellent heat conductivity and electric conductivity
With the performance advantage of functional material, it is allowed to be more widely used the various occasions needed for defence and military and industrial production.
Embodiment 1
(1) raw material weighs:The Cu-Al alloy powder of certain mass is weighed, wherein the quality of Al is divided in Cu-Al powder used
Number is 0.31%, calculates CuO powder and Cu-Al alloy powder weight ratio is about 1:100, weigh the CuO powder of the quality;
(2) preparation of dispersion-strengtherning copper powder:The mixed-powder of Cu-Al and CuO is put into ball milling in ball mill, uses steel ball
Diameter 6mm:10mm quantity ratio is 1:1;Ball material mass ratio is 30:1;300 revs/min of drum's speed of rotation;Ball-milling Time is 24 hours;
(3) powder restores:The good powder of ball milling is placed in Carbon monoxide reduction air-flow, restores 40 minutes, obtains at 450 DEG C
To pure alumina dispersion-strenghtened copper powder, oxygen content is less than 200ppm;
(4) powder nodularization:Dispersion-strengtherning copper powders are subjected to plasma spheroidization processing, obtain spherical dispersion-strengtherning copper powder,
It can be used for increasing material manufacturing technique and manufacture complicated dispersion-strengthened Cu part.
Embodiment 2
(1) raw material weighs:The Cu-Al alloy powder of certain mass is weighed, wherein the quality of Al is divided in Cu-Al powder used
Number is 0.25%, calculates CuO powder and Cu-Al alloy powder weight ratio is about 1:90, weigh the CuO powder of the quality;
(2) preparation of dispersion-strengtherning copper powder:The mixed-powder of Cu-Al and CuO is put into ball milling in ball mill, uses steel ball
Diameter 6mm:10mm quantity ratio is 4:3;Ball material mass ratio is 20:1;400 revs/min of drum's speed of rotation;Ball-milling Time is 15 hours;
(3) powder restores:The good powder of ball milling is placed in Carbon monoxide reduction air-flow, restores 50 minutes, obtains at 400 DEG C
To pure alumina dispersion-strenghtened copper powder, oxygen content is less than 200ppm;
(4) powder nodularization:Dispersion-strengtherning copper powders are subjected to plasma spheroidization processing, obtain spherical dispersion-strengtherning copper powder,
It can be used for increasing material manufacturing technique and manufacture complicated dispersion-strengthened Cu part.
Embodiment 3
(1) raw material weighs:The Cu-Al alloy powder of certain mass is weighed, wherein the quality of Al is divided in Cu-Al powder used
Number is 1%, calculates CuO powder and Cu-Al alloy powder weight ratio is about 1:22.5, weigh the CuO powder of the quality;
(2) preparation of dispersion-strengtherning copper powder:The mixed-powder of Cu-Al and CuO is put into ball milling in ball mill, uses steel ball
Diameter 6mm:10mm quantity ratio is 3:4;Ball material mass ratio is 50:1;250 revs/min of drum's speed of rotation;Ball-milling Time is 40 hours;
(3) powder restores:The good powder of ball milling is placed in Carbon monoxide reduction air-flow, restores 30 minutes, obtains at 500 DEG C
To pure alumina dispersion-strenghtened copper powder, oxygen content is less than 200ppm;
(4) powder nodularization:Dispersion-strengtherning copper powders are subjected to plasma spheroidization processing, obtain spherical dispersion-strengtherning copper powder,
It can be used for increasing material manufacturing technique and manufacture complicated dispersion-strengthened Cu part.
Claims (8)
1. a kind of preparation method of dispersion-strengthened Cu in situ composites, which is characterized in that include the following steps:
Step 1 weighs Cu-Al alloy powder and CuO powder, obtains mixed-powder;
Mixed-powder is put into ball milling in ball mill by step 2, obtains the good powder of ball milling;
The good powder of ball milling is placed in reductive heat treatment atmosphere by step 3, obtains pure alumina dispersion-strenghtened copper powder;
Pure alumina dispersion-strenghtened copper powder is carried out plasma spheroidization processing, obtains spherical dispersion-strengthened Cu by step 4
Powder, as dispersion-strengthened Cu in situ composites.
2. a kind of preparation method of dispersion-strengthened Cu in situ composites according to claim 1, which is characterized in that
In step 1, the weight ratio of CuO powder is calculated according to the weight of Al in Cu-Al alloy powder, if using Cu-Al alloyed powder
Al mass percent is x% in end, then the use of the ratio of the quality of CuO powder and Cu-Al alloyed powder quality is x/31.75~x/
Between 22.22, wherein x% range is 0.25%~1%.
3. a kind of preparation method of dispersion-strengthened Cu in situ composites according to claim 1, which is characterized in that
In step 1, the purity of Cu-Al alloy powder is 99.9%, and partial size is 40-150 μm;The purity of CuO powder is 99.5%, grain
Diameter<50μm.
4. a kind of preparation method of dispersion-strengthened Cu in situ composites according to claim 1, which is characterized in that
In step 2, ball material mass ratio is 20~50 when ball milling:1;250~400 revs/min of drum's speed of rotation;Ball-milling Time is 15~40
Hour;Every ball milling 30~50 minutes shuts down one minute and changes positive and negative rotation direction;The good powder shape of ball milling is in tiny sheet,
About 5-20 μm of partial size.
5. a kind of preparation method of dispersion-strengthened Cu in situ composites according to claim 1, which is characterized in that
In step 3, alumina dispersion-strenghtened copper powder is by Cu and Al after reduction treatment2O3Two kinds at being grouped as, the impurity oxygen of powder contains
Amount is less than 200ppm.
6. a kind of preparation method of dispersion-strengthened Cu in situ composites according to claim 1, which is characterized in that
In step 3, reductive heat treatment atmosphere is CO gas, and CO gas flow is 1~3 liter/min, and reduction temperature is 400~500 DEG C,
Recovery time is 30~50 minutes.
7. a kind of preparation method of dispersion-strengthened Cu in situ composites according to claim 1, which is characterized in that
In step 4, spherical dispersion-strengtherning copper powder is by Cu and Al2O3Two kinds at being grouped as, Al wherein included2O3Enhance particle size 5
~20nm, mass percent 0.47%~1.89%.
8. a kind of preparation method preparation of dispersion-strengthened Cu in situ composites described in any one of claim 1-7
Spherical dispersion-strengtherning copper powder using increasing material manufacturing method manufacture dispersion-strengthened Cu complex parts application.
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Cited By (5)
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CN112322922A (en) * | 2020-11-14 | 2021-02-05 | 中国兵器科学研究院宁波分院 | Powder metallurgy preparation method of dispersion copper-copper laminated composite material |
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CN115505798A (en) * | 2022-06-22 | 2022-12-23 | 安徽工程大学 | Spherical intermetallic compound particle reinforced aluminum matrix composite and preparation method thereof |
CN116240484A (en) * | 2022-12-15 | 2023-06-09 | 江苏鑫华能环保工程股份有限公司 | Preparation method of aluminum-copper composite welding material |
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CN115505798A (en) * | 2022-06-22 | 2022-12-23 | 安徽工程大学 | Spherical intermetallic compound particle reinforced aluminum matrix composite and preparation method thereof |
CN116240484A (en) * | 2022-12-15 | 2023-06-09 | 江苏鑫华能环保工程股份有限公司 | Preparation method of aluminum-copper composite welding material |
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