CN107557602A - A kind of preparation method of graphene enhancing ODS copper - Google Patents
A kind of preparation method of graphene enhancing ODS copper Download PDFInfo
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- CN107557602A CN107557602A CN201710968906.6A CN201710968906A CN107557602A CN 107557602 A CN107557602 A CN 107557602A CN 201710968906 A CN201710968906 A CN 201710968906A CN 107557602 A CN107557602 A CN 107557602A
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Abstract
The present invention relates to a kind of preparation method of graphene enhancing ODS copper, belong to Cu-base composites preparing technical field.Copper source is used as using mantoquita, silicon source is used as using aluminum nitrate, precipitating reagent is used as using sodium hydroxide or ammoniacal liquor, make copper ion, aluminium ion generation Kocide SD, aluminium hydroxide, and the graphene with disperseing in solution is co-precipitated, graphene enhancing ODS copper base bodies are obtained through drying, reduction, shaping, sintering, full densification is made up to by the hot-working means such as hot extrusion, hot forging, hot rolling.It is uniformly dispersed in Copper substrate that the present invention improves graphene, improve the interface fine structure between graphene and Copper substrate, reach dual reinforcing effect by the nano alumina particles that graphene and Dispersed precipitate are introduced in Copper substrate, its conductive performance will not be reduced again while improving matrix strength.
Description
Technical field
The present invention relates to a kind of preparation method of graphene enhancing ODS copper, belong to Cu-base composites preparing technical field.
Background technology
Aluminum oxide (Al2O3) dispersion-strengtherning (ODS) copper not only have with fine copper similar in highly conductive, thermal conductivity, and also have
Anti electric arc corrosion, antiwear property and excellent mechanical behavior under high temperature, thus be used widely.But in fact, ODS copper
Prominent contradiction, excessive (＞ 1wt.%) Al between conductive and heat-conductive and mechanical property be present2O3The addition of dispersed granules can make material
Conductive performance be greatly reduced compared with fine copper, processing characteristics can also be deteriorated.Graphene is because of its special two-dimensional structure and electricity, light
The excellent properties such as, mechanics and receive much attention.Graphene has the conductive performance of superelevation, and thermal conductivity factor can reach 5000W/
(mK), specific surface area 2630m2/ g, Young's modulus reaches 1.02TPa, and intensity is up to 130GPa, while it has very well again
Elasticity, stretch range can reach the 20% of own dimensions.Therefore, excessive Al in ODS copper is made up by doped graphene2O3
Caused conductibility loss of energy, it is a kind of preparation method of the high-strength highly-conductive Cu-base composites with bright prospects.
But because graphene has very high specific surface area, thus there is higher surface energy, agglomeration is more serious.
To solve this outstanding problem, it is copper-based compound that Chinese invention patent application CN 104451227A disclose a kind of graphene enhancing
Material and preparation method thereof, this method are to carry out ball milling with metal dust after graphene oxide powder surface chemistry method copper facing to mix
Powder, using process in warm compaction in powder metallurgy, warm compaction molding, sintering are carried out to copper-plated graphite alkene/metal mixed powder, using extruding,
The technique such as forging and stamping and rolling carries out composite processing, is made that interface cohesion is good, graphene of high-compactness enhancing Metal Substrate is answered
Condensation material.In graphene enhancing Cu-base composites prepared by this method, graphene is more uniformly dispersed in metallic matrix,
But copper-plated graphite alkene mealy structure is easily destroyed in mechanical milling process, copper coating is also easily fallen off, and this will influence
The mechanical property and thermal conductivity of material.
The content of the invention
And can keeps its conductive performance while it is an object of the invention to improve Copper substrate intensity, solves graphene enhancing
In ODS copper between graphene dispersion difference and graphene and Copper substrate the problem of interface cohesion.
The present invention technical principle be：The present invention makes copper using the method for co-precipitation by adding sodium hydroxide or ammoniacal liquor
Metal ion generation hydroxide precipitation in salt, aluminium salt mixed solution, while by dispersed graphene bag in the solution
Wrap and together precipitate, obtain graphene/ODS copper composite powders after drying, reduction, realize graphene in composite powder
It is dispersed.Then composite powder is strengthened into ODS copper base bodies by obtaining graphene after being molded, sintering, then through hot extrusion, heat
Roll, the hot-working means such as hot forging make composite further be densified, obtain that interface cohesion is good, fully dense graphene enhancing
ODS carbon/carbon-copper composite materials.
A kind of preparation method of graphene enhancing ODS copper provided by the invention, is achieved through the following technical solutions：
1st, graphene powder is entered in concentration is 2wt.%~10wt.% sodium hydroxide solutions, dilute hydrochloric acid solution respectively
Row alkali cleaning, pickled surface pretreatment, are made the high graphene powder of surface-active；Graphene powder is scattered in detergent alkylate sulphur
Graphene dispersing solution is obtained in acid sodium aqueous solution.
2nd, mantoquita and aluminum nitrate mixed solution are prepared, and the graphene dispersing solution prepared in advance is mixed with, is passed through
Graphene/copper aluminium salt mixed solution is made in magnetic agitation；
3rd, sodium hydroxide or ammonia spirit are prepared, and at the uniform velocity makes graphene to graphene copper aluminium salt mixed solution and dripping
Together precipitated with Kocide SD, aluminium hydroxide, finally give the mixing of the Kocide SD and aluminium hydroxide mixed with graphene
Sediment；
4th, the mixed sediment of acquisition is washed, dried and reduced, obtain required graphene/ODS copper composite powders
End；
5th, graphene/ODS copper composite powders are molded and sintered, pass through the hot-working hand such as hot extrusion, hot rolling, hot forging
Section makes composite further be densified, and obtains that interface cohesion is good, fully dense graphene enhancing ODS carbon/carbon-copper composite materials, stone
The content of graphene is 0.1wt.%~2wt.% in black alkene enhancing ODS carbon/carbon-copper composite materials.
Further, graphene described in step 1 is reduced graphene, and the length of two-dimensional directional is 2~20 μm, lamellar spacing
Less than 3nm, based on 1~1.5nm.
Further, graphene dispersing solution described in step 1 be by by graphene powder in neopelex water
Solution
What middle 0.5~2h of ultrasonic disperse was obtained, neopelex contains in sodium dodecyl benzene sulfonate aqueous solution
Amount accounts for stone
The mass fraction of black alkene powder is 0.5wt.%~2.5wt.%.
Further, mantoquita described in step 2 is copper acetate, copper chloride, copper sulphate, the one or more in copper nitrate, nitre
The addition of sour aluminium strengthens Al in ODS copper according to graphene2O3Content calculates for 0.2wt.%~2wt.%.
Further, the composite powder described in step 4 reduces 0.5~5h at 400~600 DEG C.
Further, the forming method of the composite powder described in step 5 is cold isostatic compaction or compression molding, cold etc. quiet
Molded pressure is 80~250MPa, and the dwell time is 30~120s；Compression molding pressure is 200~500MPa, the dwell time
For 5~30s, it is sintered under vacuum after shaping, vacuum 10-1~10-3Pa, sintering temperature are 850~1050
DEG C, soaking time is 1~5h.
The beneficial effects of the present invention are：
(1) after graphene is uniformly dispersed in advance in the solution, it is co-precipitated with the hydroxide of copper, aluminium, ensure that graphene
Dispersing uniformity in the composite, avoid in the composite reuniting as formation of crack.
(2) graphene serves both functions, first, the intensity as enhancing phase, further raising ODS copper；Second, as profit
Lubrication prescription, improve the processing characteristics of ODS copper.
Embodiment
Embodiment 1：
(1) preparation of graphene dispersing solution：It is respectively that 10wt.% sodium hydroxides are molten in concentration by 0.25g graphene powders
Alkali cleaning, pickling pretreatment are carried out in liquid, dilute hydrochloric acid solution, the high graphene powder of surface-active is made；Then 0.005g is weighed
Neopelex dissolves in deionized water, and ultrasonic disperse 1h obtains graphene dispersion wherein by graphene powder
Liquid.
(2) preparation of graphene/ODS copper composite powders：Weigh 154g acetic acid copper crystal and 2.4g ANN aluminium nitrate nonahydrates are matched somebody with somebody
Copper acetate and aluminum nitrate mixed solution is made, and the graphene dispersing solution prepared in advance is mixed with, passes through magnetic agitation
Graphene/copper aluminium salt mixed solution is made；Weigh 62.56g sodium hydroxides and be configured to the sodium hydroxide solution that concentration is 10g/ml,
And with the speed of 2~3s/ drops at the uniform velocity to mixed solution and dripping so that graphene together precipitates with Kocide SD, aluminium hydroxide
Get off, finally give the mixed sediment of the Kocide SD and aluminium hydroxide mixed with graphene；The mixed sediment of acquisition is entered
Row washing, dry, and 3h is reduced at 450 DEG C, obtain required graphene/ODS copper composite powders.
(3) preparation of graphene enhancing ODS carbon/carbon-copper composite materials：By obtained graphene/ODS copper composite powders in 200MPa
Then lower carry out compression molding, dwell time 10s carry out vacuum-sintering, soaking time 2h at 1000 DEG C, vacuum is protected
Hold 10-2Pa.Finally composite progress hot extrusion is allowed to further be densified, it is good, fully dense to obtain interface cohesion
Graphene strengthens ODS carbon/carbon-copper composite materials.
Embodiment 2：
(1) preparation of graphene dispersing solution：It is respectively 5wt.% sodium hydroxide solutions, dilute in concentration by 1g graphene powders
Alkali cleaning, pickling pretreatment are carried out in hydrochloric acid solution, the high graphene powder of surface-active is made；Then 0.005g dodecanes are weighed
Base benzene sulfonic acid sodium salt dissolves in deionized water, and ultrasonic disperse 2h obtains graphene dispersing solution wherein by graphene powder.
(2) preparation of graphene/ODS copper composite powders：Weigh 197g cupric sulfate pentahydrates crystal and the nitric hydrates of 0.74g nine
Aluminium is configured to copper acetate and aluminum nitrate mixed solution, and the graphene dispersing solution prepared in advance is mixed with, and passes through magnetic force
Graphene/copper aluminium salt mixed solution is made in stirring；Weigh 63.2g sodium hydroxides be configured to concentration be 10g/ml sodium hydroxide it is molten
Liquid, and with the speed of 2~3s/ drops at the uniform velocity to mixed solution and dripping so that graphene together sinks with Kocide SD, aluminium hydroxide
Shallow lake is got off, and finally gives the mixed sediment of the Kocide SD and aluminium hydroxide mixed with graphene；By the mixed sediment of acquisition
Washed, dried, and 5h is reduced at 400 DEG C, obtain required graphene/ODS copper composite powders.
(3) preparation of graphene enhancing ODS carbon/carbon-copper composite materials：By obtained graphene/ODS copper composite powders in 250MPa
Lower carry out cold isostatic compaction, dwell time 30s, then carries out vacuum-sintering, soaking time 5h, vacuum at 850 DEG C
Degree is maintained at 10-1Pa.Finally composite progress hot forging is allowed to further be densified, it is good, complete fine and close to obtain interface cohesion
Graphene enhancing ODS carbon/carbon-copper composite materials.
Embodiment 3：
(1) preparation of graphene dispersing solution：By 0.1g graphene powders respectively concentration be 2wt.% sodium hydroxide solutions,
Alkali cleaning, pickling pretreatment are carried out in dilute hydrochloric acid solution, the high graphene powder of surface-active is made；Then 0.025g 12 is weighed
Sodium alkyl benzene sulfonate dissolves in deionized water, and ultrasonic disperse 0.5h obtains graphene dispersion wherein by graphene powder
Liquid.
(2) preparation of graphene/ODS copper composite powders：Weigh 268.26g copper chloride dihydrates crystal and 7.36g nine is hydrated
Aluminum nitrate is configured to copper acetate and aluminum nitrate mixed solution, and the graphene dispersing solution prepared in advance is mixed with, and passes through
Graphene/copper aluminium salt mixed solution is made in magnetic agitation；Measure 175ml ammoniacal liquor (ammonia concn 25wt.%) and with 1~2s/
The speed of drop is at the uniform velocity to mixed solution and dripping so that and graphene together precipitates with Kocide SD, aluminium hydroxide, final
To the Kocide SD and the mixed sediment of aluminium hydroxide mixed with graphene；The mixed sediment of acquisition is washed, dried,
And 0.5h is reduced at 600 DEG C, obtain required graphene/ODS copper composite powders.
(3) preparation of graphene enhancing ODS carbon/carbon-copper composite materials：By obtained graphene/ODS copper composite powders in 500MPa
Then lower carry out compression molding, dwell time 5s carry out vacuum-sintering, soaking time 1h at 1050 DEG C, vacuum is protected
Hold 10-3Pa.Finally composite progress hot rolling is allowed to further be densified, obtains that interface cohesion is good, fully dense stone
Black alkene strengthens ODS carbon/carbon-copper composite materials.
Embodiment 4：
(1) preparation of graphene dispersing solution：It is respectively 7wt.% sodium hydroxide solutions, dilute in concentration by 1g graphene powders
Alkali cleaning, pickling pretreatment are carried out in hydrochloric acid solution, the high graphene powder of surface-active is made；Then 0.01g dodecanes are weighed
Base benzene sulfonic acid sodium salt dissolves in deionized water, and ultrasonic disperse 1.5h obtains graphene dispersing solution wherein by graphene powder.
(2) preparation of graphene/ODS copper composite powders：Weigh 295.14g nitric acid copper crystal and the nitric hydrates of 14.72g nine
Aluminium is configured to copper acetate and aluminum nitrate mixed solution, and the graphene dispersing solution prepared in advance is mixed with, and passes through magnetic force
Graphene/copper aluminium salt mixed solution is made in stirring；Weigh 130.6g sodium hydroxides and be configured to the sodium hydroxide that concentration is 20g/ml
Solution, and with the speed of 3~4s/ drops at the uniform velocity to mixed solution and dripping so that graphene and Kocide SD, aluminium hydroxide are together
Precipitate, finally give the mixed sediment of the Kocide SD and aluminium hydroxide mixed with graphene；By the mixed precipitation of acquisition
Thing is washed, dried, and reduces 1h at 500 DEG C, obtains required graphene/ODS copper composite powders.
(3) preparation of graphene enhancing ODS carbon/carbon-copper composite materials：By obtained graphene/ODS copper composite powders in 80MPa
Lower carry out cold isostatic compaction, dwell time 120s, then carries out vacuum-sintering, soaking time 3h, vacuum at 900 DEG C
Degree is maintained at 10-2Pa.Finally composite progress hot extrusion is allowed to further be densified, obtains interface cohesion and cause well, entirely
Close graphene enhancing ODS carbon/carbon-copper composite materials.
Claims (6)
1. a kind of preparation method of graphene enhancing ODS copper, it is characterised in that comprise the following steps：
(1) graphene powder is subjected to alkali in concentration is 2wt.%~10wt.% sodium hydroxide solutions, dilute hydrochloric acid solution respectively
Wash, pickled surface pretreatment, the high graphene powder of surface-active is made, graphene powder is scattered in DBSA
Graphene dispersing solution is obtained in sodium water solution；
(2) mantoquita and aluminum nitrate mixed solution are prepared, and the graphene dispersing solution prepared in advance is mixed with, passes through magnetic force
Graphene/copper aluminium salt mixed solution is made in stirring；
(3) sodium hydroxide or ammonia spirit are prepared, and at the uniform velocity makes graphene and hydrogen to graphene copper aluminium salt mixed solution and dripping
Cupric oxide, aluminium hydroxide together precipitate, and finally give the mixed precipitation of the Kocide SD and aluminium hydroxide mixed with graphene
Thing；
(4) mixed sediment of acquisition is washed, dried and reduced, obtain required graphene/ODS copper composite powders；
(5) graphene/ODS copper composite powders are molded and sintered, made by hot extrusion, hot rolling, hot forging hot-working means
Composite is further densified, and obtains that interface cohesion is good, fully dense graphene enhancing ODS carbon/carbon-copper composite materials, graphene
The content for strengthening graphene in ODS carbon/carbon-copper composite materials is 0.1wt.%~2wt.%.
2. the preparation method of a kind of graphene enhancing ODS copper according to claim 1, it is characterised in that step (1) is described
Graphene is reduced graphene, and the length of two-dimensional directional is 2~20 μm, and lamellar spacing is less than 3nm, based on 1~1.5nm.
3. the preparation method of a kind of graphene enhancing ODS copper according to claim 1, it is characterised in that step (1) is described
Graphene dispersing solution is by the way that by graphene powder, 0.5~2h of ultrasonic disperse is obtained in sodium dodecyl benzene sulfonate aqueous solution
, the mass fraction that the content of neopelex accounts for graphene powder in sodium dodecyl benzene sulfonate aqueous solution is
0.5wt.%~2.5wt.%.
4. the preparation method of a kind of graphene enhancing ODS copper according to claim 1, it is characterised in that step (2) is described
Mantoquita is the one or more in copper acetate, copper chloride, copper nitrate, copper sulphate, and the addition of aluminum nitrate strengthens according to graphene
Al in ODS copper2O3Content calculates for 0.2wt.%~2wt.%.
5. the preparation method of a kind of graphene enhancing ODS copper according to claim 1, it is characterised in that step (4) is described
Composite powder 0.5~5h is reduced at 400~600 DEG C.
6. the preparation method of a kind of graphene enhancing ODS copper according to claim 1, it is characterised in that step (5) is described
The forming method of composite powder be cold isostatic compaction or compression molding, cold isostatic compaction pressure is 80~250MPa, is protected
The pressure time is 30~120s；Compression molding pressure is 200~500MPa, and the dwell time is 5~30s, in vacuum condition after shaping
Under be sintered, vacuum 10-1~10-3Pa, sintering temperature are 850~1050 DEG C, and soaking time is 1~5h.
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Cited By (8)
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| CN110227825A (en) * | 2019-05-16 | 2019-09-13 | 湖南华瑞康源科技有限公司 | A kind of low energy ball milling prepares graphene/copper/cuprous oxide composite granule method |
| CN110699617A (en) * | 2019-10-31 | 2020-01-17 | 成都工业学院 | Preparation method of graphene and aluminum oxide whisker co-reinforced copper-based composite material and product thereof |
| CN110828024A (en) * | 2019-11-20 | 2020-02-21 | 北京清大际光科技发展有限公司 | Conducting wire prepared from conductive graphene coated copper and preparation method and application thereof |
| CN111020263A (en) * | 2019-12-19 | 2020-04-17 | 哈尔滨工业大学（威海） | Plastic processing preparation method of high-strength high-conductivity graphene reinforced copper-based composite material |
| CN112139512A (en) * | 2020-08-25 | 2020-12-29 | 湖南大学 | Preparation method of copper-based composite material precursor powder |
| CN112391549A (en) * | 2020-12-07 | 2021-02-23 | 西安稀有金属材料研究院有限公司 | Preparation method of reduced graphene oxide and aluminum oxide co-reinforced copper-based composite material |
| CN113061768A (en) * | 2021-03-22 | 2021-07-02 | 中南大学 | Preparation method of dispersion-strengthened copper-based composite material |
| CN113480875A (en) * | 2021-07-27 | 2021-10-08 | 雷索新材料(苏州)有限公司 | Aluminum oxide modified graphene, graphene heat dissipation coating and preparation method thereof |
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| CN110227825A (en) * | 2019-05-16 | 2019-09-13 | 湖南华瑞康源科技有限公司 | A kind of low energy ball milling prepares graphene/copper/cuprous oxide composite granule method |
| CN110699617A (en) * | 2019-10-31 | 2020-01-17 | 成都工业学院 | Preparation method of graphene and aluminum oxide whisker co-reinforced copper-based composite material and product thereof |
| CN110699617B (en) * | 2019-10-31 | 2020-12-22 | 成都工业学院 | Preparation method of graphene and aluminum oxide whisker co-reinforced copper-based composite material and product thereof |
| CN110828024A (en) * | 2019-11-20 | 2020-02-21 | 北京清大际光科技发展有限公司 | Conducting wire prepared from conductive graphene coated copper and preparation method and application thereof |
| CN111020263A (en) * | 2019-12-19 | 2020-04-17 | 哈尔滨工业大学（威海） | Plastic processing preparation method of high-strength high-conductivity graphene reinforced copper-based composite material |
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| CN112139512B (en) * | 2020-08-25 | 2021-12-21 | 湖南大学 | Preparation method of copper-based composite material precursor powder |
| CN112391549A (en) * | 2020-12-07 | 2021-02-23 | 西安稀有金属材料研究院有限公司 | Preparation method of reduced graphene oxide and aluminum oxide co-reinforced copper-based composite material |
| CN113061768A (en) * | 2021-03-22 | 2021-07-02 | 中南大学 | Preparation method of dispersion-strengthened copper-based composite material |
| CN113061768B (en) * | 2021-03-22 | 2023-08-25 | 中南大学 | Preparation method of dispersion strengthening copper-based composite material |
| CN113480875A (en) * | 2021-07-27 | 2021-10-08 | 雷索新材料(苏州)有限公司 | Aluminum oxide modified graphene, graphene heat dissipation coating and preparation method thereof |
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