CN106077608A - A kind of graphene-supported metallic composite and preparation method thereof - Google Patents
A kind of graphene-supported metallic composite and preparation method thereof Download PDFInfo
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- CN106077608A CN106077608A CN201610423597.XA CN201610423597A CN106077608A CN 106077608 A CN106077608 A CN 106077608A CN 201610423597 A CN201610423597 A CN 201610423597A CN 106077608 A CN106077608 A CN 106077608A
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- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 54
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 20
- 239000010439 graphite Substances 0.000 claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 19
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 19
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000003647 oxidation Effects 0.000 claims abstract description 19
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 19
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 19
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 19
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims abstract description 19
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004411 aluminium Substances 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229960001471 sodium selenite Drugs 0.000 claims abstract description 18
- 235000015921 sodium selenite Nutrition 0.000 claims abstract description 18
- 239000011781 sodium selenite Substances 0.000 claims abstract description 18
- WUUHFRRPHJEEKV-UHFFFAOYSA-N tripotassium borate Chemical compound [K+].[K+].[K+].[O-]B([O-])[O-] WUUHFRRPHJEEKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 17
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 17
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 16
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 16
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 16
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 16
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 16
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 claims abstract description 16
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 15
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000003398 denaturant Substances 0.000 claims abstract description 9
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 32
- 238000005245 sintering Methods 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- 239000011268 mixed slurry Substances 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 10
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 10
- 239000008187 granular material Substances 0.000 claims description 8
- -1 hydroxybenzene amine Chemical class 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000012778 molding material Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 238000001694 spray drying Methods 0.000 claims description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000460 chlorine Substances 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 claims description 6
- 150000005690 diesters Chemical class 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Natural products OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 5
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 5
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 5
- 229960003742 phenol Drugs 0.000 claims description 5
- HGQSXVKHVMGQRG-UHFFFAOYSA-N dioctyltin Chemical compound CCCCCCCC[Sn]CCCCCCCC HGQSXVKHVMGQRG-UHFFFAOYSA-N 0.000 claims description 4
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims 1
- 238000003682 fluorination reaction Methods 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 229910021389 graphene Inorganic materials 0.000 description 6
- 238000011056 performance test Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 1
- RZBBHEJLECUBJT-UHFFFAOYSA-N 6-methylheptyl 2-sulfanylacetate Chemical compound CC(C)CCCCCOC(=O)CS RZBBHEJLECUBJT-UHFFFAOYSA-N 0.000 description 1
- 241001614291 Anoplistes Species 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- GTTYPHLDORACJW-UHFFFAOYSA-N nitric acid;sodium Chemical compound [Na].O[N+]([O-])=O GTTYPHLDORACJW-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229960001881 sodium selenate Drugs 0.000 description 1
- 235000018716 sodium selenate Nutrition 0.000 description 1
- 239000011655 sodium selenate Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B22F1/0003—
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
-
- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention discloses a kind of graphene-supported metallic composite, it is prepared by the raw materials in: natural flake graphite 25 35 parts, sodium nitrate 5 10 parts, 35 parts of potassium permanganate, sodium borohydride 48 parts, hydrazine hydrate 25 parts, Polyethylene Glycol 9 15 parts, three oxidation four ferrum 26 parts, Nickel dichloride. 13 parts, stannic chloride 13 parts, potassium borate 59 parts, tungsten powder 15 25 parts, nikel powder 5 15 parts, copper powder 39 parts, magnesium powder 48 parts, aluminium powder 35 parts, sodium selenite 27 parts, curing receives 26 parts, Firebrake ZB 57 parts, Zirconium tetrafluoride. 38 parts, polyvinyl alcohol 6 10 parts, denaturant 35 parts, heat stabilizer 5 10 parts.The graphene-supported metallic composite being prepared from, its mechanical strength height, good heat conductivity, electron mobility are big.Meanwhile, corresponding preparation method is also disclosed.
Description
Technical field
The present invention relates to technical field of metal, particularly to a kind of graphene-supported metallic composite and system thereof
Preparation Method.
Background technology
Along with the development of modern science and technology, this year, carbon nanomaterial has caused the concern of every subjects.Since 2004
University of Manchester utilizes mechanical stripping method to obtain Graphene one first, and it is always in carbon nanomaterial the focus of research.
Graphene is with sp by carbon atom2The monoatomic layer that hydridization connects is constituted, and is also called " mono-layer graphite sheet ", and its theoretic throat is only
0.35nm, be at present seen by the thinnest two-dimensional material.And Graphene is the elementary cell constituting other carbon nanomaterials.Stone
The theoretical specific area of ink alkene is high, and mechanical strength is high, good heat conductivity, and electron transport ability is strong, and it is excellent that electron mobility is big etc.
Point.So Graphene is excellent carrier or the ingredient of many materials.
Graphene and metal material are combined the Metal/grapheme composite that obtains can in conjunction with both advantages, one
Aspect Graphene can make metal material be uniformly dispersed, stable；On the other hand electric transmission rate can be strengthened, it is provided that composite
Overall performance.Just because of the good characteristic of Metal/grapheme composite, this material modified electrode, electrochmical power source,
Solaode, catalyst and the aspect such as pharmaceutical carrier and gas sensor have a wide range of applications.So this grinds
Study carefully and be intended to research a kind of novel graphene-supported metallic composite of discovery, to expect to have in various new technology fields
Significant progress and application prospect.
Summary of the invention
For solving above-mentioned technical problem, the present invention provides a kind of graphene-supported metallic composite and preparation side thereof
Method, by using specified raw material to be combined, coordinates corresponding production technology, has obtained a kind of graphene-supported metal composite
Material, its mechanical strength height, good heat conductivity, electron mobility are big, it is possible to meet the requirement of industry, before having preferably application
Scape.
The purpose of the present invention can be achieved through the following technical solutions:
Graphene-supported metallic composite, is prepared by the raw materials in: natural flake graphite 25-35 part, nitric acid
Sodium 5-10 part, potassium permanganate 3-5 part, sodium borohydride 4-8 part, hydrazine hydrate 2-5 part, Polyethylene Glycol 9-15 part, three oxidation four ferrum 2-6
Part, Nickel dichloride. 1-3 part, stannic chloride 1-3 part, potassium borate 5-9 part, tungsten powder 15-25 part, nikel powder 5-15 part, copper powder 3-9 part, magnesium powder
4-8 part, aluminium powder 3-5 part, sodium selenite 2-7 part, curing receive 2-6 part, Firebrake ZB 5-7 part, Zirconium tetrafluoride. 3-8 part, polyvinyl alcohol
6-10 part, denaturant 3-5 part, heat stabilizer 5-10 part.
Preferably, described denaturant is selected from para hydroxybenzene amine, paranitrophenol, aminopropyl triethoxysilane, six Asias
One or more in tetramine.
Preferably, described heat stabilizer is selected from dioctyl adipate, propylene glycol methyl ether acetate, double isooctyl mercaptoacetate
One or more in dioctyltin, double acrylic acid fourth diester.
The preparation method of described graphene-supported metallic composite, comprises the following steps:
(1) each raw material is weighed according to weight portion；
(2) by tungsten powder, nikel powder, copper powder, magnesium powder, aluminium powder, sodium selenite, curing are received, Firebrake ZB, Zirconium tetrafluoride., polyvinyl alcohol add
Entering blending tank, stir 3-5 hour with the speed of 1000-1500 rev/min, send into high temperature furnace pre-burning, calcined temperature is 300-450
DEG C, burn-in time is 2-3 hour；
(3) again the mixture after preheating is added in ball mill, adds the isopropanol of mixture weight 20%, carry out ball
Mill processes, and obtains powder mixture；
(4) by natural flake graphite, sodium nitrate, potassium permanganate, sodium borohydride, hydrazine hydrate, Polyethylene Glycol, three oxidation four ferrum, chlorine
Changing in nickel, stannic chloride, potassium borate, denaturant, heat stabilizer addition ultrasonator, under conditions of 50kHz, 220W, dispersion is all
Even, obtain mixed slurry；
(5) powder mixture that step (3) obtains is added in the mixed slurry that step (4) obtains, is stirring evenly and then adding into
Spray drying tower, inlet temperature is 250-300 DEG C, and outlet temperature is 150-180 DEG C, obtains granular material, then crosses 20 mesh
Sieve；
(6) it is compressing that mould put into by the material after sieving, and is directly placed in the cryostat of-30 DEG C cold by the material after molding
But 20-30 minute；
(7) molding materials after sub-cooled is sintered, is cooled to room temperature after having sintered, obtains finished product.
Preferably, being sintered to vacuum-sintering in step (7), vacuum is 1.5 × 10-1Pa, sintering temperature is 950-
1000 DEG C, sintering time is 2-3 hour.
Compared with prior art, it has the beneficial effect that the present invention
(1) the graphene-supported metallic composite of the present invention is with natural flake graphite, tungsten powder, nikel powder, copper powder, magnesium powder, aluminum
Powder is main component, by adding sodium selenite, curing and receiving, Firebrake ZB, Zirconium tetrafluoride., polyvinyl alcohol, sodium nitrate, permanganic acid
Potassium, sodium borohydride, hydrazine hydrate, Polyethylene Glycol, three oxidation four ferrum, Nickel dichloride., stannic chloride, potassium borate, denaturant, heat stabilizers,
It is aided with the techniques such as high-temperature calcination, stirring ball-milling, ultrasonic disperse, drying and screening, pressing mold cooling, sintering, machine-shaping so that preparation
Graphene-supported metallic composite, its mechanical strength height, good heat conductivity, electron mobility are big, it is possible to meet
The requirement of industry, has preferable application prospect.
(2) the graphene-supported metallic composite cheaper starting materials of the present invention, technique simply, are suitable to heavy industrialization
Use, practical.
Detailed description of the invention
Below in conjunction with specific embodiment, the technical scheme of invention is described in detail.
Embodiment 1
(1) natural flake graphite 25 parts, sodium nitrate 5 parts, 3 parts of potassium permanganate, sodium borohydride 4 parts, hydrazine hydrate 2 parts, poly-second are weighed
Glycol 9 parts, three oxidation four ferrum 2 parts, Nickel dichloride. 1 part, stannic chloride 1 part, potassium borate 5 parts, tungsten powder 15 parts, nikel powder 5 parts, copper powder 3 parts,
Magnesium powder 4 parts, aluminium powder 3 parts, sodium selenite 2 parts, curing receive 2 parts, Firebrake ZB 5 parts, Zirconium tetrafluoride. 3 parts, polyvinyl alcohol 6 parts, to hydroxyl
Base aniline 3 parts, dioctyl adipate 5 parts；
(2) by tungsten powder, nikel powder, copper powder, magnesium powder, aluminium powder, sodium selenite, curing are received, Firebrake ZB, Zirconium tetrafluoride., polyvinyl alcohol add
Entering blending tank, stir 3 hours with the speed of 1000 revs/min, send into high temperature furnace pre-burning, calcined temperature is 300 DEG C, and burn-in time is
2 hours；
(3) again the mixture after preheating is added in ball mill, adds the isopropanol of mixture weight 20%, carry out ball
Mill processes, and obtains powder mixture；
(4) by natural flake graphite, sodium nitrate, potassium permanganate, sodium borohydride, hydrazine hydrate, Polyethylene Glycol, three oxidation four ferrum, chlorine
Change in nickel, stannic chloride, potassium borate, para hydroxybenzene amine, dioctyl adipate addition ultrasonator, in the condition of 50kHz, 220W
Under be uniformly dispersed, obtain mixed slurry；
(5) powder mixture that step (3) obtains is added in the mixed slurry that step (4) obtains, is stirring evenly and then adding into
Spray drying tower, inlet temperature is 250 DEG C, and outlet temperature is 150 DEG C, obtains granular material, then crosses 20 mesh sieves；
(6) it is compressing that mould put into by the material after sieving, and is directly placed in the cryostat of-30 DEG C cold by the material after molding
But 20 minutes；
(7) molding materials after sub-cooled is sintered, is cooled to room temperature after having sintered, obtains finished product, be sintered to true
Empty sintering, vacuum is 1.5 × 10-1Pa, sintering temperature is 950 DEG C, and sintering time is 2 hours.
The performance test results of the graphene-supported metallic composite prepared is as shown in table 1.
Embodiment 2
(1) natural flake graphite 28 parts, sodium nitrate 7 parts, 4 parts of potassium permanganate, sodium borohydride 5 parts, hydrazine hydrate 3 parts, poly-second are weighed
Glycol 11 parts, three oxidation four ferrum 3 parts, Nickel dichloride. 2 parts, stannic chloride 2 parts, potassium borate 7 parts, tungsten powder 19 parts, nikel powder 8 parts, copper powders 5
Part, magnesium powder 5 parts, aluminium powder 4 parts, sodium selenite 3 parts, curing receive 3 parts, Firebrake ZB 6 parts, Zirconium tetrafluoride. 4 parts, polyvinyl alcohol 7 parts, right
Nitrophenol 4 parts, propylene glycol methyl ether acetate 7 parts；
(2) by tungsten powder, nikel powder, copper powder, magnesium powder, aluminium powder, sodium selenite, curing are received, Firebrake ZB, Zirconium tetrafluoride., polyvinyl alcohol add
Entering blending tank, stir 3.5 hours with the speed of 1200 revs/min, send into high temperature furnace pre-burning, calcined temperature is 350 DEG C, burn-in time
It it is 2.4 hours；
(3) again the mixture after preheating is added in ball mill, adds the isopropanol of mixture weight 20%, carry out ball
Mill processes, and obtains powder mixture；
(4) by natural flake graphite, sodium nitrate, potassium permanganate, sodium borohydride, hydrazine hydrate, Polyethylene Glycol, three oxidation four ferrum, chlorine
Change in nickel, stannic chloride, potassium borate, paranitrophenol, propylene glycol methyl ether acetate addition ultrasonator, at 50kHz, 220W
Under the conditions of be uniformly dispersed, obtain mixed slurry；
(5) powder mixture that step (3) obtains is added in the mixed slurry that step (4) obtains, is stirring evenly and then adding into
Spray drying tower, inlet temperature is 270 DEG C, and outlet temperature is 160 DEG C, obtains granular material, then crosses 20 mesh sieves；
(6) it is compressing that mould put into by the material after sieving, and is directly placed in the cryostat of-30 DEG C cold by the material after molding
But 23 minutes；
(7) molding materials after sub-cooled is sintered, is cooled to room temperature after having sintered, obtains finished product, be sintered to true
Empty sintering, vacuum is 1.5 × 10-1Pa, sintering temperature is 970 DEG C, and sintering time is 2.3 hours.
The performance test results of the graphene-supported metallic composite prepared is as shown in table 1.
Embodiment 3
(1) natural flake graphite 32 parts, sodium nitrate 8 parts, 4 parts of potassium permanganate, sodium borohydride 7 parts, hydrazine hydrate 4 parts, poly-second are weighed
Glycol 13 parts, three oxidation four ferrum 5 parts, Nickel dichloride. 2 parts, stannic chloride 2 parts, potassium borate 7 parts, tungsten powder 22 parts, nikel powder 12 parts, copper powders 8
Part, magnesium powder 6 parts, aluminium powder 4 parts, sodium selenite 6 parts, curing receive 5 parts, Firebrake ZB 6 parts, Zirconium tetrafluoride. 7 parts, polyvinyl alcohol 9 parts, ammonia
Propyl-triethoxysilicane 4 parts, Imarcaptoacetate dioctyltin 9 parts；
(2) by tungsten powder, nikel powder, copper powder, magnesium powder, aluminium powder, sodium selenite, curing are received, Firebrake ZB, Zirconium tetrafluoride., polyvinyl alcohol add
Entering blending tank, stir 4 hours with the speed of 1400 revs/min, send into high temperature furnace pre-burning, calcined temperature is 400 DEG C, and burn-in time is
2.8 hour；
(3) again the mixture after preheating is added in ball mill, adds the isopropanol of mixture weight 20%, carry out ball
Mill processes, and obtains powder mixture；
(4) by natural flake graphite, sodium nitrate, potassium permanganate, sodium borohydride, hydrazine hydrate, Polyethylene Glycol, three oxidation four ferrum, chlorine
Change nickel, stannic chloride, potassium borate, aminopropyl triethoxysilane, Imarcaptoacetate dioctyltin addition ultrasonic vibration
In device, it is uniformly dispersed under conditions of 50kHz, 220W, obtains mixed slurry；
(5) powder mixture that step (3) obtains is added in the mixed slurry that step (4) obtains, is stirring evenly and then adding into
Spray drying tower, inlet temperature is 290 DEG C, and outlet temperature is 170 DEG C, obtains granular material, then crosses 20 mesh sieves；
(6) it is compressing that mould put into by the material after sieving, and is directly placed in the cryostat of-30 DEG C cold by the material after molding
But 28 minutes；
(7) molding materials after sub-cooled is sintered, is cooled to room temperature after having sintered, obtains finished product, be sintered to true
Empty sintering, vacuum is 1.5 × 10-1Pa, sintering temperature is 980 DEG C, and sintering time is 2.8 hours.
The performance test results of the graphene-supported metallic composite prepared is as shown in table 1.
Embodiment 4
(1) natural flake graphite 35 parts, sodium nitrate 10 parts, 5 parts of potassium permanganate, sodium borohydride 8 parts, hydrazine hydrate 5 parts, poly-second are weighed
Glycol 15 parts, three oxidation four ferrum 6 parts, Nickel dichloride. 3 parts, stannic chloride 3 parts, potassium borate 9 parts, tungsten powder 25 parts, nikel powder 15 parts, copper powders 9
Part, magnesium powder 8 parts, aluminium powder 5 parts, sodium selenite 7 parts, curing receive 6 parts, Firebrake ZB 7 parts, Zirconium tetrafluoride. 8 parts, polyvinyl alcohol 10 parts,
Hexamethylenetetramine 5 parts, double acrylic acid fourth diester 10 parts；
(2) by tungsten powder, nikel powder, copper powder, magnesium powder, aluminium powder, sodium selenite, curing are received, Firebrake ZB, Zirconium tetrafluoride., polyvinyl alcohol add
Entering blending tank, stir 5 hours with the speed of 1500 revs/min, send into high temperature furnace pre-burning, calcined temperature is 450 DEG C, and burn-in time is
3 hours；
(3) again the mixture after preheating is added in ball mill, adds the isopropanol of mixture weight 20%, carry out ball
Mill processes, and obtains powder mixture；
(4) by natural flake graphite, sodium nitrate, potassium permanganate, sodium borohydride, hydrazine hydrate, Polyethylene Glycol, three oxidation four ferrum, chlorine
Change in nickel, stannic chloride, potassium borate, hexamethylenetetramine, double acrylic acid fourth diester addition ultrasonator, at 50kHz, 220W
Under the conditions of be uniformly dispersed, obtain mixed slurry；
(5) powder mixture that step (3) obtains is added in the mixed slurry that step (4) obtains, is stirring evenly and then adding into
Spray drying tower, inlet temperature is 300 DEG C, and outlet temperature is 180 DEG C, obtains granular material, then crosses 20 mesh sieves；
(6) it is compressing that mould put into by the material after sieving, and is directly placed in the cryostat of-30 DEG C cold by the material after molding
But 30 minutes；
(7) molding materials after sub-cooled is sintered, is cooled to room temperature after having sintered, obtains finished product, be sintered to true
Empty sintering, vacuum is 1.5 × 10-1Pa, sintering temperature is 1000 DEG C, and sintering time is 3 hours.
The performance test results of the graphene-supported metallic composite prepared is as shown in table 1.
Comparative example 1
(1) natural flake graphite 25 parts, sodium nitrate 5 parts, hydrazine hydrate 2 parts, Polyethylene Glycol 9 parts, three oxidation four ferrum 2 parts, chlorine are weighed
Change 1 part of nickel, stannic chloride 1 part, potassium borate 5 parts, tungsten powder 15 parts, magnesium powder 4 parts, aluminium powder 3 parts, sodium selenite 2 parts, curing receive 2 parts,
Firebrake ZB 5 parts, Zirconium tetrafluoride. 3 parts, polyvinyl alcohol 6 parts, para hydroxybenzene amine 3 parts, dioctyl adipate 5 parts；
(2) by tungsten powder, magnesium powder, aluminium powder, sodium selenite, curing are received, Firebrake ZB, Zirconium tetrafluoride., polyvinyl alcohol add blending tank, with
The speed of 1000 revs/min stirs 3 hours, sends into high temperature furnace pre-burning, and calcined temperature is 300 DEG C, and burn-in time is 2 hours；
(3) again the mixture after preheating is added in ball mill, adds the isopropanol of mixture weight 20%, carry out ball
Mill processes, and obtains powder mixture；
(4) by natural flake graphite, sodium nitrate, hydrazine hydrate, Polyethylene Glycol, three oxidation four ferrum, Nickel dichloride., stannic chloride, potassium borate,
Para hydroxybenzene amine, dioctyl adipate add in ultrasonator, be uniformly dispersed, mixed under conditions of 50kHz, 220W
Slip；
(5) powder mixture that step (3) obtains is added in the mixed slurry that step (4) obtains, is stirring evenly and then adding into
Spray drying tower, inlet temperature is 250 DEG C, and outlet temperature is 150 DEG C, obtains granular material, then crosses 20 mesh sieves；
(6) it is compressing that mould put into by the material after sieving, and is directly placed in the cryostat of-30 DEG C cold by the material after molding
But 20 minutes；
(7) molding materials after sub-cooled is sintered, is cooled to room temperature after having sintered, obtains finished product, be sintered to true
Empty sintering, vacuum is 1.5 × 10-1Pa, sintering temperature is 950 DEG C, and sintering time is 2 hours.
The performance test results of the graphene-supported metallic composite prepared is as shown in table 1.
Comparative example 2
(1) natural flake graphite 35 parts, 5 parts of potassium permanganate, sodium borohydride 8 parts, Polyethylene Glycol 15 parts, three oxidation four ferrum 6 are weighed
Part, Nickel dichloride. 3 parts, stannic chloride 3 parts, potassium borate 9 parts, tungsten powder 25 parts, nikel powder 15 parts, copper powder 9 parts, magnesium powder 8 parts, aluminium powder 5 parts, sub-
Sodium selenate 7 parts, curing receive 6 parts, Firebrake ZB 7 parts, polyvinyl alcohol 10 parts, hexamethylenetetramine 5 parts, double acrylic acid fourth diester 10
Part；
(2) by tungsten powder, nikel powder, copper powder, magnesium powder, aluminium powder, sodium selenite, curing are received, Firebrake ZB, polyvinyl alcohol add mixing
Tank, stirs 5 hours with the speed of 1500 revs/min, sends into high temperature furnace pre-burning, and calcined temperature is 450 DEG C, and burn-in time is 3 hours；
(3) again the mixture after preheating is added in ball mill, adds the isopropanol of mixture weight 20%, carry out ball
Mill processes, and obtains powder mixture；
(4) by natural flake graphite, potassium permanganate, sodium borohydride, Polyethylene Glycol, three oxidation four ferrum, Nickel dichloride., stannic chloride, boron
Acid potassium, hexamethylenetetramine, double acrylic acid fourth diester add in ultrasonator, and under conditions of 50kHz, 220W, dispersion is all
Even, obtain mixed slurry；
(5) powder mixture that step (3) obtains is added in the mixed slurry that step (4) obtains, is stirring evenly and then adding into
Spray drying tower, inlet temperature is 300 DEG C, and outlet temperature is 180 DEG C, obtains granular material, then crosses 20 mesh sieves；
(6) it is compressing that mould put into by the material after sieving, and is directly placed in the cryostat of-30 DEG C cold by the material after molding
But 30 minutes；
(7) molding materials after sub-cooled is sintered, is cooled to room temperature after having sintered, obtains finished product, be sintered to true
Empty sintering, vacuum is 1.5 × 10-1Pa, sintering temperature is 1000 DEG C, and sintering time is 3 hours.
The performance test results of the graphene-supported metallic composite prepared is as shown in table 1.
The graphene-supported metallic composite of embodiment 1-4 and comparative example 1-2 is carried out tensile strength, heat conduction respectively
The test of the performance such as coefficient, electron mobility.
Table 1
| Tensile strength (MPa) | Heat conductivity (W.m<sup>-3</sup>.K<sup>-1</sup>) | Electron mobility (cm<sup>2</sup>.v<sup>-1</sup>.s<sup>-1</sup>) | |
| Embodiment 1 | 1260 | 5300 | 14600 |
| Embodiment 2 | 1300 | 5400 | 15000 |
| Embodiment 3 | 1310 | 5200 | 14800 |
| Embodiment 4 | 1320 | 5500 | 15100 |
| Comparative example 1 | 460 | 2700 | 8900 |
| Comparative example 2 | 540 | 2850 | 9200 |
The graphene-supported metallic composite of the present invention with natural flake graphite, tungsten powder, nikel powder, copper powder, magnesium powder, aluminium powder is
Main component, by adding sodium selenite, curing and receiving, Firebrake ZB, Zirconium tetrafluoride., polyvinyl alcohol, sodium nitrate, potassium permanganate, boron
Sodium hydride, hydrazine hydrate, Polyethylene Glycol, three oxidation four ferrum, Nickel dichloride., stannic chloride, potassium borate, denaturant, heat stabilizers, be aided with height
The techniques such as temperature calcining, stirring ball-milling, ultrasonic disperse, drying and screening, pressing mold cooling, sintering, machine-shaping so that be prepared from
Graphene-supported metallic composite, its mechanical strength height, good heat conductivity, electron mobility are big, it is possible to meet industry
Requirement, has preferable application prospect.The graphene-supported metallic composite cheaper starting materials of the present invention, technique are simple, suitable
Use in heavy industrialization, practical.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every utilize this
Equivalent structure or equivalence flow process that bright description is made convert, or are directly or indirectly used in other relevant technology necks
Territory, is the most in like manner included in the scope of patent protection of the present invention.
Claims (5)
1. a graphene-supported metallic composite, it is characterised in that: it is prepared by the raw materials in: natural scale
Graphite 25-35 part, sodium nitrate 5-10 part, potassium permanganate 3-5 part, sodium borohydride 4-8 part, hydrazine hydrate 2-5 part, Polyethylene Glycol 9-15
Part, three oxidation four ferrum 2-6 parts, Nickel dichloride. 1-3 part, stannic chloride 1-3 part, potassium borate 5-9 part, tungsten powder 15-25 part, nikel powder 5-15
Part, copper powder 3-9 part, magnesium powder 4-8 part, aluminium powder 3-5 part, sodium selenite 2-7 part, curing receive 2-6 part, Firebrake ZB 5-7 part, fluorination
Zirconium 3-8 part, polyvinyl alcohol 6-10 part, denaturant 3-5 part, heat stabilizer 5-10 part.
Graphene-supported metallic composite the most according to claim 1, it is characterised in that: described denaturant is selected from
One or more in para hydroxybenzene amine, paranitrophenol, aminopropyl triethoxysilane, hexamethylenetetramine.
Graphene-supported metallic composite the most according to claim 1, it is characterised in that: described heat stabilizer is selected from
In dioctyl adipate, propylene glycol methyl ether acetate, Imarcaptoacetate dioctyltin, double acrylic acid fourth diester one
Plant or several.
4. according to the preparation method of the arbitrary described graphene-supported metallic composite of claim 1-3, it is characterised in that
Comprise the following steps:
(1) each raw material is weighed according to weight portion；
(2) by tungsten powder, nikel powder, copper powder, magnesium powder, aluminium powder, sodium selenite, curing are received, Firebrake ZB, Zirconium tetrafluoride., polyvinyl alcohol add
Entering blending tank, stir 3-5 hour with the speed of 1000-1500 rev/min, send into high temperature furnace pre-burning, calcined temperature is 300-450
DEG C, burn-in time is 2-3 hour；
(3) again the mixture after preheating is added in ball mill, adds the isopropanol of mixture weight 20%, carry out ball
Mill processes, and obtains powder mixture；
(4) by natural flake graphite, sodium nitrate, potassium permanganate, sodium borohydride, hydrazine hydrate, Polyethylene Glycol, three oxidation four ferrum, chlorine
Changing in nickel, stannic chloride, potassium borate, denaturant, heat stabilizer addition ultrasonator, under conditions of 50kHz, 220W, dispersion is all
Even, obtain mixed slurry；
(5) powder mixture that step (3) obtains is added in the mixed slurry that step (4) obtains, is stirring evenly and then adding into
Spray drying tower, inlet temperature is 250-300 DEG C, and outlet temperature is 150-180 DEG C, obtains granular material, then crosses 20 mesh
Sieve；
(6) it is compressing that mould put into by the material after sieving, and is directly placed in the cryostat of-30 DEG C cold by the material after molding
But 20-30 minute；
(7) molding materials after sub-cooled is sintered, is cooled to room temperature after having sintered, obtains finished product.
Preparation method the most according to claim 4, it is characterised in that be sintered to vacuum-sintering, vacuum in step (7)
It is 1.5 × 10-1Pa, sintering temperature is 950-1000 DEG C, and sintering time is 2-3 hour.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108470625A (en) * | 2018-01-29 | 2018-08-31 | 广东明路电力电子有限公司 | Micropore conduction sheet electrodes and its processing technology |
| CN112687873A (en) * | 2020-12-23 | 2021-04-20 | 湖南永盛新材料股份有限公司 | Preparation method of high-specific-energy lithium battery |
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| CN104711443A (en) * | 2015-03-18 | 2015-06-17 | 上海和伍新材料科技有限公司 | Graphene/copper composite and preparation method thereof |
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