CN106745237A - A kind of layer type casting moulding Graphene non-metallic metal composite and preparation method - Google Patents
A kind of layer type casting moulding Graphene non-metallic metal composite and preparation method Download PDFInfo
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- CN106745237A CN106745237A CN201611256383.4A CN201611256383A CN106745237A CN 106745237 A CN106745237 A CN 106745237A CN 201611256383 A CN201611256383 A CN 201611256383A CN 106745237 A CN106745237 A CN 106745237A
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- Prior art keywords
- oxide
- graphene
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- type casting
- casting moulding
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 238000005266 casting Methods 0.000 title claims abstract description 32
- 238000000465 moulding Methods 0.000 title claims abstract description 32
- 239000002905 metal composite material Substances 0.000 title abstract 4
- 239000000463 material Substances 0.000 claims abstract description 79
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 238000010791 quenching Methods 0.000 claims abstract description 9
- 230000000171 quenching effect Effects 0.000 claims abstract description 9
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- 239000002096 quantum dot Substances 0.000 claims abstract description 8
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- 238000002525 ultrasonication Methods 0.000 claims abstract description 8
- 238000013532 laser treatment Methods 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims description 78
- 238000000034 method Methods 0.000 claims description 25
- 229910052744 lithium Inorganic materials 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 23
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- ZVKRVGZVXQYLPZ-UHFFFAOYSA-N [Li].[V].P(O)(O)(O)=O Chemical compound [Li].[V].P(O)(O)(O)=O ZVKRVGZVXQYLPZ-UHFFFAOYSA-N 0.000 claims description 4
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- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052789 astatine Inorganic materials 0.000 claims description 4
- RYXHOMYVWAEKHL-UHFFFAOYSA-N astatine atom Chemical compound [At] RYXHOMYVWAEKHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052794 bromium Inorganic materials 0.000 claims description 4
- PLLZRTNVEXYBNA-UHFFFAOYSA-L cadmium hydroxide Chemical compound [OH-].[OH-].[Cd+2] PLLZRTNVEXYBNA-UHFFFAOYSA-L 0.000 claims description 4
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- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 4
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 claims description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 4
- 229960004643 cupric oxide Drugs 0.000 claims description 4
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 4
- ASTZLJPZXLHCSM-UHFFFAOYSA-N dioxido(oxo)silane;manganese(2+) Chemical compound [Mn+2].[O-][Si]([O-])=O ASTZLJPZXLHCSM-UHFFFAOYSA-N 0.000 claims description 4
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- CPSYWNLKRDURMG-UHFFFAOYSA-L hydron;manganese(2+);phosphate Chemical compound [Mn+2].OP([O-])([O-])=O CPSYWNLKRDURMG-UHFFFAOYSA-L 0.000 claims description 4
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- 239000000395 magnesium oxide Substances 0.000 claims description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 4
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- 229910052759 nickel Inorganic materials 0.000 claims description 4
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 4
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- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000123 polythiophene Polymers 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical group CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 241000500881 Lepisma Species 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 description 1
- WYPNXPVMAIXNNH-UHFFFAOYSA-N [Mn].[Co]=S Chemical compound [Mn].[Co]=S WYPNXPVMAIXNNH-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 229910052635 ferrosilite Inorganic materials 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000001999 grid alloy Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000013096 zirconium-based metal-organic framework Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to a kind of layer type casting moulding Graphene non-metallic metal composite and preparation method thereof.The preparation method of layer type casting moulding Graphene non-metallic metal composite, graphene quantum dot and/or microplate are carried out into mixed grinding, shearing with non-metallic metal material under ultrasonication, quenching carried out through laser treatment, refined, promote molecular rearrangement, grafting fusion after drying.Layer type casting moulding Graphene non-metallic metal composite prepared by the invention, it is low with high rigidity, high intensity, resistivity, the superior function for using easily is processed, can be widely applied to the material processing fields such as dental implant, super electric drill；Battery, ultracapacitor energy storage Material Field；Catalyst material field；Heat sink material field；Medical domain；Coating material field；Electrically conductive ink；Photoelectricity, sensor material field；Biological association area etc..
Description
Technical field
The present invention relates to Graphene applied technical field, more particularly to a kind of layer type casting moulding Graphene-nonmetallic-metal is multiple
Condensation material and preparation method.
Background technology
Single-layer graphene film is made up of one layer of intensive carbon hexatomic ring, does not have any fault of construction, and its thickness is
0.35nm or so, is two-dimensional nano-carbon material most thin so far.Meanwhile, it be also constitute other carbon group materials it is substantially single
Unit, can obtain that the fullerene of zero dimension, curling obtain one-dimensional CNT and stacking obtains the graphite of three-dimensional by warpage.Stone
Repetition period unit most basic in black alkene is the most stable phenyl ring knot ditch in organic chemistry, it be it is current untill best two
Dimension nano material.The Graphene prepared in reality does not only exist individual layer, also there is multilayer.Due to its unique structure, Graphene
Various types of properties it is also very excellent.It is most thin most light material in the world, and thickness is most thin up to 0.34nm, and specific surface area is
2630m2/g, carrier mobility at room temperature is about 200,000 (cm2/ vs), oneself knows one of intensity highest material, compares diamond
It is also hard, taller upper 100 times of strength ratio steel best in the world.It possesses good toughness again simultaneously, and can bend,
The theoretical Young's modulus of ideal graphite alkene reaches 1.0TPa, and fracture strength is 130GPa.Thermal conductivity factor is up to 5000W/mK, is current
Untill highest.
At present, domestic and international researcher being combined in grapheme material, modification application aspect has carried out more research, as in
State's number of patent application：CN201610528611.2, disclose a kind of porous carbon-Graphene-metal oxide composite material and its
Preparation method and application.The method has the material of porous material in nature by finding, then with graphene oxide by height
Temperature is thermally treated resulting in porous carbon-graphene composite material, then metal oxide is compound on above-mentioned composite, obtains one kind
Porous carbon-Graphene-metal oxide composite material.The material can solve manually to prepare porous material specific surface area with structure not
Continuously, the larger contradictory problems of internal resistance, and porous material specific surface area and electrical conductivity are further improved using grapheme material, make
Obtain high-specific surface area and high conductivity is unified on same composite.Chinese Patent Application No.：
CN201610481436.6, invents a kind of organic metal framework/nano-stannic oxide/Graphene composite photocatalyst material and its system
Preparation Method and purposes, composite are that, for carrier, nano-stannic oxide is scattered in organic metal framework (Zr-MOFs, UiO66)
The organic metal framework surface, Graphene is then wrapped in the organic metal framework with nano-stannic oxide, shows higher
Catalysis activity.Chinese Patent Application No.：CN201610452943.7, discloses a kind of lead comprising slicker solder-rare earth-Graphene
The preparation method of accumulator plate grid alloy, by adding rare earth element, significantly improves crystal grain, the grain boundary features of alloy, crystal grain chi
Very little to be substantially reduced, grain boundary area increase under same current density, can substantially reduce etching extent.Chinese Patent Application No.：
CN201610825355.3 discloses a kind of preparation method of nickel oxide/graphene oxide composite material, and it is existing in order to solve
Prepare that metal oxide particle in metal oxide/graphene composite material is big and particle diameter is uneven and specific capacitance is relatively low
Problem.Chinese Patent Application No.：CN201610821003.0, discloses a kind of iron oxyhydroxide/graphenoxide oxide composite material
Preparation method and applications.Iron oxyhydroxide/graphenoxide oxide composite material is by the suspension and hydroxyl of graphene oxide
The suspension of iron oxide is according to volume ratio 1:It is composited by hydro-thermal method after 1~2 mixing, dispersion.Chinese Patent Application No.：
CN201610804294.2, discloses a kind of preparation method of LiFePO4/graphene composite material.The method mainly includes will
Waste lithium iron phosphate battery positive plate is mixed by organic solvent immersion, ultrasonication, ball milling, roasting, quenching and conductive black
Close roasting and obtain LiFePO 4 material；Then natural flake graphite and sodium nitrate are added in sulfuric acid solution, by permanganic acid
The oxidation such as potassium obtains graphene oxide；LiFePO 4 material and the graphene oxide mixing that will finally obtain, with N- methyl -2- pyrroles
Pyrrolidone is dispersant, and ball milling obtains final product LiFePO4/graphene composite material.Chinese Patent Application No.：
CN201610768001.X, discloses a kind of preparation method of stannic disulfide/graphene nanocomposite material, lithium ion battery and bears
Pole, lithium ion battery, preparation method step include hydro-thermal operation, compound working procedure, and preparation method of the present invention causes that stannic disulfide exists
Graphenic surface directly carries out growth in situ, by washing, dries and obtains sheet stannic disulfide/graphene composite material, the material
Material is applied to lithium ion battery negative material, effectively improves the stability and electric conductivity of material, lifts battery performance, has
Good cycling stability, the advantages of specific energy density is high.Chinese Patent Application No.：CN201610763257.1, discloses a kind of three
Preparation method, lithium ion battery negative, the lithium ion battery of two iron/graphene composite material are aoxidized, preparation method step includes
Hydro-thermal operation, compound working procedure, preparation method of the present invention cause di-iron trioxide nano particle uniform load in three-dimensional grapheme
In surface and pore passage structure, by washing, dry obtain sesquioxide/graphene composite material, the materials application in lithium from
Sub- battery, with high power capacity, have extended cycle life, low cost and easily large-scale production etc. excellent properties.Chinese Patent Application No.：
CN201610764913.X, discloses a kind of preparation method of manganese sulfide/graphene nanocomposite material, lithium ion battery and bears
Pole, lithium ion battery, preparation method step include hydro-thermal operation, compound working procedure, and preparation method of the present invention causes manganese sulfide in stone
Black alkene surface directly carries out growth in situ, by washing, dries and obtains manganese sulfide/graphene composite material, and the present invention passes through sulphur
Change manganese and three-dimensional redox graphene is combined the shortcomings of to overcome stability difference caused by its Volume Changes, strengthen its conductive
Property, so as to improve the performance of lithium ion battery, the materials application has good cycling stability in lithium ion battery negative material,
The advantages of specific energy density is high.Chinese Patent Application No.：CN201610748848.1, is related to a kind of with level porous hollow
Molybdenum bisuphide/the graphene composite material and its synthetic method of microspheroidal structure, belong to Micron-nano composites and prepare and synthesis
Technical field.Filled with big specific capacitance and excellent circulation when the composite is used as electrode material for super capacitor
Discharge stability, illustrates wide application prospect.Chinese Patent Application No.：CN201610594377.3, discloses one kind
The preparation method of the fluorinated graphene composite of Nano Silver is loaded with, the composite for obtaining has premium properties.It is Chinese special
Sharp application number：A kind of manganese cobalt sulfide/graphene composite material preparation technology of electrochemical performance, electricity in the preparation technology
Chemical deposition uses three-electrode system, and working electrode is three-dimensional graphene foam, is platinized platinum to electrode, and reference electrode is Ag/
AgCl normal electrodes.This technological operation is easy, the structure of matter stabilization of preparation, and changing parameter can change the pattern of material, enter
And the chemical property of material is lifted, can be used for large area and prepare electrode material.
In sum, although Graphene and its composite and technology are applied to more multi-field, and performance improvement is obtained
And lifting, but the Graphene with hard high-strength due to interfacial energy it is high, intermolecular active force and chemical bond are made
With by force and be necessarily susceptible to reunite.Therefore, due to there is lamination and reunion when graphene composite material is prepared into, no
The performance advantage of high rigidity, high intensity and the high heat conduction of grapheme material can be fully demonstrated, this problem limits it bigger
Scope, the application in broader field.
The content of the invention
Present invention aim to address the deficiencies in the prior art, there is provided a kind of layer type casting moulding Graphene-nonmetallic-metal is multiple
The preparation method of condensation material.The present invention is opened between graphene sheet layer under ultrasonication, the Graphene material under laser action
Material is merged with nonmetallic-metallics, and the material for obtaining has high rigidity, high intensity, resistivity low, is easily processed and is used
Superior function, can be widely applied to the material processing fields such as dental implant, super electric drill；Battery, ultracapacitor energy storage material
Material field；Catalyst material field；Heat sink material field；Medical domain；Coating material field；Electrically conductive ink；Photoelectricity, sensor
Material Field；Biological association area etc..
The present invention is achieved by the following technical solutions：
The preparation method of layer type casting moulding Graphene-nonmetallic-metallic composite, it is characterised in that comprise the following steps：
(1) by graphene quantum dot and/or graphene microchip and non-metal simple-substance/compound-metal under ultrasonication
Simple substance/compound carries out mixed grinding, shearing, and composite slurry material or composite powder material is obtained；
(2) obtained composite slurry material or powder body material are dried, obtain anhydrous composite powder material；
(3) obtained anhydrous composite powder material carried out into quenching through laser treatment, refined, promote molecular rearrangement, grafting
Fusion, obtains a layer type casting moulding Graphene-nonmetallic-metallic composite.
Further, the metal simple-substance be zirconium, titanium, lead, nickel, copper, silver, molybdenum, gold, palladium, zinc, aluminium, iron, cobalt, chromium, manganese,
One or more in tin, iridium, ruthenium, indium, lanthanide series metal simple substance.
Further, the non-metal simple-substance is in sulphur, nitrogen, silicon, phosphorus, boron, fluorine, chlorine, arsenic, selenium, bromine, tellurium, iodine, astatine
Plant or several.
Further, the metallic compound is zirconium oxide, molybdenum bisuphide, tungsten disulfide, lead oxide, vulcanized lead, hydrogen-oxygen
Change nickel, nickel oxide, nickel phosphide, cupric oxide, silver oxide, palladium bichloride, zinc oxide, aluminum oxide, iron oxide, iron phosphide, cobalt sulfide, sulphur
Lead plumbate, LiFePO4, lithium manganese phosphate, phosphoric acid vanadium lithium, vanadium phosphate sodium, lithium ferric manganese phosphate, manganese silicate of lithium, ferric metasilicate lithium, lithium titanate,
Cobalt acid lithium, LiMn2O4, nickel ion doped, nickle cobalt lithium manganate, cobalt oxide, titanium oxide, titanium boride, vanadium oxide, cadmium hydroxide, vulcanization
Cadmium, chromium oxide, manganese oxide, tin oxide, antimony oxide, tungsten oxide, bismuth oxide, yittrium oxide, zirconium oxide, zirconium silicate, yttrium oxide, chlorination
Iridium, iridium complex, silver oxide, ruthenium-oxide, ruthenic acid are secret, one or more in ruthenic acid lead, scandium oxide, indium oxide, magnesia.
Further, the nonmetallic compound is boron nitride, CNT, carbon fiber, polyaniline, rare earth, rubber, modeling
One or more of material, polypyrrole, polythiophene, resin cation, resin anion (R.A.).
Further, the ultrasonication is produced by ultrasonic head, ultrasonic device or Vltrasonic device.
Preferably, the mixed grinding of step (1) is carried out under elevated pressure conditions, and pressure is 10-250MPa, and the time is 10-
60min.Solid phase mixing grinding shearing under condition of high voltage, not only causes mixture dispersion, mixing evenly, improves its dispersion mixed
The uniformity of conjunction, more effectively reaches the stacking and reunion for preventing graphene quantum dot and/or graphene microchip, beneficial to Graphene
With the compound action and enhancing adhesion of metallics.
Further, the mixed grinding of step (1) uses the one kind or two in high pressure liquid stream method or physical grinding method
Plant combination.Wherein, the high pressure liquid stream method, refers to mixture to be ground through high-pressure fluid, is sheared, and is crushed, mixed
Method, wherein fluid is water, ethanol, acetone, formamide, 1-METHYLPYRROLIDONE, acetonitrile, methyl alcohol, propyl alcohol, acetone, dioxy
Six rings, tetrahydrofuran, MEK, n-butanol, ethyl acetate, ether, isopropyl ether, dichloromethane, chloroform, bromoethane, benzene, tetrachloro
Change carbon, carbon disulfide, hexamethylene, hexane, one or more in kerosene.Temperature during high pressure liquid stream method mixed grinding is 2-18
DEG C, it is preferable that temperature is 4-6 DEG C.Brownian movement violent when can prevent high temperature is produced reunites again.
The physical grinding method, refers to mixture to be ground through high pressure solid, is sheared, the side for crushed, mixing
Method.
Further, the drying means of step (2) is atmosphere pressure desiccation, low pressure seasoning, boulton process, supercritical drying
Dry method or spray drying process.
The present invention also provides a kind of layer type casting moulding Graphene-nonmetallic-metallic composite, it is characterised in that by above-mentioned
Preparation method obtain.
The beneficial effects of the invention are as follows：
By preparation method of the invention so that avoid lamination and reunion during Graphene application, and prepared by the present invention
Layer type casting moulding Graphene answers-nonmetallic-metallic compound composite, is beaten between graphene sheet layer under ultrasonication
Open, grapheme material is merged with nonmetallic-metallic compound under laser action, the material for obtaining has high rigidity, height
Intensity, resistivity are low, are easily processed the superior function for using, and can be widely applied to the processing of the materials such as dental implant, super electric drill
Field；Battery, ultracapacitor energy storage Material Field；Catalyst material field；Heat sink material field；Medical domain；Coating material
Material field；Electrically conductive ink；Photoelectricity, sensor material field；Biological association area etc..
Specific embodiment
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
The layer type casting moulding Graphene-nonmetallic-metallic composite of the present embodiment, its preparation method comprises the following steps：
(1) graphene quantum dot, Zirconium oxide powder, rare earth are mixed under ultrasonic probe effect, it is high using pure water
Pressure liquid flow method high pressure abrasive, shearing, pressure are 220MPa, and the time is 35min, and temperature is 2 DEG C, and composite slurry material is obtained；
(2) obtained composite slurry material is vacuum dried, pressure is 200Pa, drying time is 60min, is obtained
Anhydrous composite powder material；
(3) by drying after anhydrous composite powder material through laser treatment carry out quenching, refine, promote molecular rearrangement, connect
Branch fusion, obtains a layer type casting moulding Graphene-nonmetallic-metallic composite.
In other embodiments, graphene quantum dot can also use graphene microchip or graphene quantum dot and Graphene
The mixture of microplate replaces；Vacuum drying pressure can be in 50-200Pa scopes, and drying time is 20-60min.
Embodiment 2
The layer type casting moulding Graphene-nonmetallic-metallic composite of the present embodiment, its preparation method comprises the following steps：
(1) graphene microchip is mixed with titania powder, polyaniline under ultrasound reactor effect, is used
Ethanol high pressure liquid stream method high pressure abrasive, shearing, pressure are 180MPa, and the time is 45min, and temperature is 18 DEG C, and composite slurry is obtained
Material；
(2) obtained composite slurry material is vacuum dried, pressure is 50Pa, drying time is 20min, obtains nothing
Water composite powder material；
(3) by drying after anhydrous composite powder material carry out quenching of laser, refine, promote molecular rearrangement, grafting fusion,
Obtain a layer type casting moulding Graphene-nonmetallic-metallic composite.
In other embodiments, titania powder can also use zirconium oxide, molybdenum bisuphide, tungsten disulfide, lead oxide, sulphur
Change lead, nickel hydroxide, nickel oxide, nickel phosphide, cupric oxide, silver oxide, palladium bichloride, zinc oxide, aluminum oxide, iron oxide, iron phosphide,
Cobalt sulfide, lead sulfate, LiFePO4, lithium manganese phosphate, phosphoric acid vanadium lithium, vanadium phosphate sodium, lithium ferric manganese phosphate, manganese silicate of lithium, ferrosilite
Lithium, lithium titanate, cobalt acid lithium, LiMn2O4, nickel ion doped, nickle cobalt lithium manganate, cobalt oxide, titanium boride, vanadium oxide, cadmium hydroxide, sulphur
Cadmium, chromium oxide, manganese oxide, tin oxide, antimony oxide, tungsten oxide, bismuth oxide, yittrium oxide, zirconium oxide, zirconium silicate, yttrium oxide, chlorine
Change iridium, iridium complex, silver oxide, ruthenium-oxide, secret ruthenic acid, ruthenic acid lead, scandium oxide, indium oxide, one or more in magnesia
Instead of；Polyaniline can also use boron nitride, CNT, carbon fiber, rare earth, rubber, plastics, polypyrrole, polythiophene, cation
One or more replacements of resin, resin anion (R.A.).
Embodiment 3
The layer type casting moulding Graphene-nonmetallic-metallic composite of the present embodiment, its preparation method comprises the following steps：
(1) graphene microchip, titania powder, rare earth are mixed under ultrasonic probe effect, is ground using physics
Mill method high pressure abrasive, shearing, pressure is 180MPa, and the time is 45min, and composite slurry material is obtained；
(2) obtained composite slurry material is carried out into constant pressure and dry, drying time is 30-300min, obtains anhydrous compound
Powder body material；
(3) by drying after anhydrous composite powder material carry out quenching of laser, refine, promote molecular rearrangement, grafting fusion,
Obtain a layer type casting moulding Graphene-nonmetallic-metallic composite.
Embodiment 4
The layer type casting moulding Graphene-nonmetallic-metallic composite of the present embodiment, its preparation method comprises the following steps：
(1) graphene microchip is mixed with zirconium, sulphur under ultrasonic probe effect, is ground using physical grinding method high pressure
Mill, shearing, pressure is 10MPa, and the time is 60min, and composite slurry material is obtained；
(2) obtained composite slurry material is spray-dried, drying time is 30-200min, is obtained anhydrous compound
Powder body material；
(3) by drying after anhydrous composite powder material carry out quenching of laser, refine, promote molecular rearrangement, grafting fusion,
Obtain a layer type casting moulding Graphene-nonmetallic-metallic composite.
In other embodiments, zirconium can also by titanium, lead, nickel, copper, silver, molybdenum, gold, palladium, zinc, aluminium, iron, cobalt, chromium, manganese,
One or more replacements in tin, iridium, ruthenium, indium, lanthanide series metal simple substance；Sulphur can also by nitrogen, silicon, phosphorus, boron, fluorine, chlorine, arsenic, selenium,
One or more replacements in bromine, tellurium, iodine, astatine.
Embodiment 5
The layer type casting moulding Graphene-nonmetallic-metallic composite of the present embodiment, its preparation method comprises the following steps：
(1) graphene quantum dot is mixed with silicon, Zinc oxide powder under ultrasonic probe effect, using physical grinding
Method high pressure abrasive, shearing, pressure is 250MPa, and the time is 10min, and composite powder material is obtained；
(2) obtained composite slurry material is carried out into supercritical drying, pressure is 500Pa, and drying time is 100min, is obtained
To anhydrous composite powder material；
(3) by drying after anhydrous composite powder material carry out quenching of laser, refine, promote molecular rearrangement, grafting fusion,
Obtain a layer type casting moulding Graphene-nonmetallic-metallic composite.
In other embodiments, silicon can also be by the one kind in sulphur, nitrogen, phosphorus, boron, fluorine, chlorine, arsenic, selenium, bromine, tellurium, iodine, astatine
Or several replacements；Zinc oxide powder can also by zirconium oxide, molybdenum bisuphide, tungsten disulfide, lead oxide, vulcanized lead, nickel hydroxide,
Nickel oxide, nickel phosphide, cupric oxide, silver oxide, palladium bichloride, zinc oxide, aluminum oxide, iron oxide, iron phosphide, cobalt sulfide, lead sulfate,
LiFePO4, lithium manganese phosphate, phosphoric acid vanadium lithium, vanadium phosphate sodium, lithium ferric manganese phosphate, manganese silicate of lithium, ferric metasilicate lithium, lithium titanate, cobalt acid
Lithium, LiMn2O4, nickel ion doped, nickle cobalt lithium manganate, cobalt oxide, titanium oxide, titanium boride, vanadium oxide, cadmium hydroxide, cadmium sulfide, oxygen
Change chromium, manganese oxide, tin oxide, antimony oxide, tungsten oxide, bismuth oxide, yittrium oxide, zirconium oxide, zirconium silicate, yttrium oxide, iridium chloride, iridium
Complex compound, silver oxide, ruthenium-oxide, ruthenic acid are secret, one or more replacements in ruthenic acid lead, scandium oxide, indium oxide, magnesia；It is super
Critical dry pressure can be in the range of 10-1000Pa, and drying time is 15-200min.
The invention is not limited in above-mentioned implementation method, if not departing from the present invention to various changes of the invention or deformation
Spirit and scope, if these are changed and within the scope of deformation belongs to claim of the invention and equivalent technologies, then this hair
It is bright to be also intended to comprising these changes and deform.
Claims (10)
1. the preparation method of layer type casting moulding Graphene-nonmetallic-metallic composite, it is characterised in that comprise the following steps：
(1) under ultrasonication by graphene quantum dot and/or graphene microchip and non-metal simple-substance/compound-metal simple-substance/
Compound carries out mixed grinding, shearing, and composite slurry material or composite powder material is obtained；
(2) obtained composite slurry material or powder body material are dried, obtain anhydrous composite powder material；
(3) obtained anhydrous composite powder material carried out into quenching through laser treatment, refined, promote molecular rearrangement, grafting fusion,
Obtain layer type casting moulding Graphene-nonmetallic-metallic composite.
2. the according to claim 1 layer of preparation method of type casting moulding Graphene-nonmetallic-metallic composite, its feature
It is：The metal simple-substance be zirconium, titanium, lead, nickel, copper, silver, molybdenum, gold, palladium, zinc, aluminium, iron, cobalt, chromium, manganese, tin, iridium, ruthenium, indium,
One or more in lanthanide series metal simple substance.
3. the according to claim 1 layer of preparation method of type casting moulding Graphene-nonmetallic-metallic composite, its feature
It is：The non-metal simple-substance is one or more in sulphur, nitrogen, silicon, phosphorus, boron, fluorine, chlorine, arsenic, selenium, bromine, tellurium, iodine, astatine.
4. the according to claim 1 layer of preparation method of type casting moulding Graphene-nonmetallic-metallic composite, its feature
It is：The metallic compound be zirconium oxide, molybdenum bisuphide, tungsten disulfide, lead oxide, vulcanized lead, nickel hydroxide, nickel oxide,
Nickel phosphide, cupric oxide, silver oxide, palladium bichloride, zinc oxide, aluminum oxide, iron oxide, iron phosphide, cobalt sulfide, lead sulfate, ferric phosphate
Lithium, lithium manganese phosphate, phosphoric acid vanadium lithium, vanadium phosphate sodium, lithium ferric manganese phosphate, manganese silicate of lithium, ferric metasilicate lithium, lithium titanate, cobalt acid lithium, mangaic acid
Lithium, nickel ion doped, nickle cobalt lithium manganate, cobalt oxide, titanium oxide, titanium boride, vanadium oxide, cadmium hydroxide, cadmium sulfide, chromium oxide, oxygen
Change manganese, tin oxide, antimony oxide, tungsten oxide, bismuth oxide, yittrium oxide, zirconium oxide, zirconium silicate, yttrium oxide, iridium chloride, iridium complex,
Silver oxide, ruthenium-oxide, ruthenic acid are secret, one or more in ruthenic acid lead, scandium oxide, indium oxide, magnesia.
5. the according to claim 1 layer of preparation method of type casting moulding Graphene-nonmetallic-metallic composite, its feature
It is：The nonmetallic compound is boron nitride, CNT, carbon fiber, polyaniline, rare earth, rubber, plastics, polypyrrole, poly-
One or more of thiophene, resin cation, resin anion (R.A.).
6. the according to claim 1 layer of preparation method of type casting moulding Graphene-nonmetallic-metallic composite, its feature
It is：The ultrasonication is produced by ultrasonic head, ultrasonic device or Vltrasonic device.
7. the according to claim 1 layer of preparation method of type casting moulding Graphene-nonmetallic-metallic composite, its feature
It is：The mixed grinding of step (1) is carried out under elevated pressure conditions, and pressure is 10-250MPa, and the time is 10-60min.
8. the according to claim 1 layer of preparation method of type casting moulding Graphene-nonmetallic-metallic composite, its feature
It is：The mixed grinding of step (1) uses one or two combinations in high pressure liquid stream method or physical grinding method.
9. the according to claim 1 layer of preparation method of type casting moulding Graphene-nonmetallic-metallic composite, its feature
It is：The drying means of step (2) is that atmosphere pressure desiccation, low pressure seasoning, boulton process, supercritical drying or spraying are dry
Dry method.
10. a kind of layer type casting moulding Graphene-nonmetallic-metallic composite, it is characterised in that by any institute of claim 1~9
The preparation method stated is obtained.
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