CN105598470A - Preparation method of carbon reinforced metal/metal oxide composite powder - Google Patents
Preparation method of carbon reinforced metal/metal oxide composite powder Download PDFInfo
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- CN105598470A CN105598470A CN201610103335.5A CN201610103335A CN105598470A CN 105598470 A CN105598470 A CN 105598470A CN 201610103335 A CN201610103335 A CN 201610103335A CN 105598470 A CN105598470 A CN 105598470A
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- 239000000843 powder Substances 0.000 title claims abstract description 68
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 48
- 239000002184 metal Substances 0.000 title claims abstract description 48
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 30
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 32
- 229910052799 carbon Inorganic materials 0.000 title abstract 7
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 239000000428 dust Substances 0.000 claims abstract description 20
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 239000012266 salt solution Substances 0.000 claims abstract description 12
- 238000006722 reduction reaction Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 5
- 238000000197 pyrolysis Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 52
- 239000002243 precursor Substances 0.000 claims description 25
- 238000000889 atomisation Methods 0.000 claims description 14
- 230000002708 enhancing effect Effects 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 20
- 239000000203 mixture Substances 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 238000010923 batch production Methods 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 239000002041 carbon nanotube Substances 0.000 description 17
- 229910021393 carbon nanotube Inorganic materials 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 229910021389 graphene Inorganic materials 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 230000008676 import Effects 0.000 description 8
- 238000003860 storage Methods 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 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 5
- 229910003472 fullerene Inorganic materials 0.000 description 5
- 229960004643 cupric oxide Drugs 0.000 description 4
- 238000009938 salting Methods 0.000 description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 3
- 229940116318 copper carbonate Drugs 0.000 description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 3
- 235000019850 ferrous citrate Nutrition 0.000 description 3
- 239000011640 ferrous citrate Substances 0.000 description 3
- APVZWAOKZPNDNR-UHFFFAOYSA-L iron(ii) citrate Chemical compound [Fe+2].OC(=O)CC(O)(C([O-])=O)CC([O-])=O APVZWAOKZPNDNR-UHFFFAOYSA-L 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 238000007306 functionalization reaction Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000005118 spray pyrolysis Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical group OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of carbon reinforced metal/metal oxide composite powder and belongs to the field of composite material preparation. The preparation method comprises the steps that a cavity is heated to reach metal salt decomposition temperature, then a metal salt solution and carbon dispersion liquid are mixed, the mixture is atomized into small liquid drops (generally nanoscale) by using a spraying device, the small liquid drops are led into the cavity, pyrolytic reaction instantly occurs under the high-temperature effect of the cavity to generate metal oxide and carbon composite powder, or the small liquid drops are led into the reduction atmosphere, while pyrolysis and reduction reactions occur to generate the metal oxide and carbon composite powder, and then the powder is collected through a dust collection device. The preparation method does not destroy original morphology of carbon, the prepared composite powder particles are smaller in size (can reach the nanoscale), size distribution is more controllable, the dispersity of the carbon in a matrix is more excellent, and the preparation method further has the advantages that the method is simple and convenient to operate, and large-scale batch production is easy to achieve.
Description
Technical field
The invention discloses the preparation method that a kind of carbonaceous strengthens metal/metal oxide composite powder, belong to technical field prepared by composite powder.
Background technology
Carbonaceous strengthens metal/metal oxide powder, especially Ultra-fine Grained and manocrystalline powders, due to its unique mechanics and physicochemical characteristics, such as good heat conduction, electric conductivity, huge specific area etc., have broad application prospects in fields such as electronic applications, field of functional materials, chemical field and Aero-Space.
But, because Ultra-fine Grained and nanocrystalline metal/metal oxide powder have very large specific area, make it be easy to reunite, thereby affect homogeneity and the stability of properties of product. In addition, between carbonaceous and metal/metal oxide powder, there is larger difference of specific gravity and size difference, and the reasons such as interface binding power is weak, if preparation method and technique are incorrect, be easy to cause component segregation, strengthen giving full play to of metal/metal oxide powder excellent properties thereby affected carbonaceous.
Existing prepare method that carbonaceous strengthens metal/metal oxide composite powder be mainly by ball grinding method,
Coprecipitation and molecule rank mixing method, but there is inevitable defect in these methods. in " Microstructuresandtensilebehaviorofcarbonnanotubesreinfo rcedCumatrixcompositeswithmolecular-leveldispersion " paper of delivering as people such as Xue, mention a kind of molecule rank mixing method and prepared carbonaceous and strengthen the method for burning composite powder, concrete steps are that the carbonaceous of functionalization is put into alcohol sonic oscillation 30min by the concentration of 1g/L, metal salt solution is dissolved in ammoniacal liquor by the concentration of 2g/ml, these two kinds of mixed solutions are mixed and ultrasonic vibration 30min, at 100 DEG C, carry out magnetic agitation, at 300 DEG C, calcining obtains dry carbonaceous enhancing burning composite powder again. obviously, in calcination process, powder can occur to reunite and recrystallization phenomenon again, and temperature is higher, and reunion and recrystallization phenomenon are more serious.
Summary of the invention
The technical problem to be solved in the present invention is that extensive mass is dispersed in even carbon nanotube in metal/metal oxide powder matrix, and by extremely ultra-fine and nanoscale of composite powder grain refine, preparing metal/metal oxide composite for powder metallurgic method provides important reliable raw material sources.
The object of the present invention is to provide a kind of spray pyrolysis to prepare the method for carbonaceous enhancing metal/metal oxide composite powder, adopt the process route of configuration precursor solution → atomization → pyrolytic → collection powder to obtain carbonaceous enhancing metal/metal oxide composite powder, specifically comprise the following steps:
Metal salt solution and carbonaceous dispersion liquid are configured to precursor solution, it is fully mixed, then this precursor solution is carried out to atomization by atomising device, enter in the cavity that is heated in advance slaine decomposition temperature with the form of drop (being generally nanoscale), and keep temperature constant, issue raw pyrolytic reaction at aerobic environment, then open dust collecting system and collect, obtain burning composite powder; Or in pyrolytic reaction process, pass into reducing atmosphere, carry out pyrolysis and reduction reaction simultaneously, carbonaceous strengthens metal-based compound powder.
Preferably, slaine of the present invention is inorganic metal salt (such as chlorate, sulfate, nitrate) or organic metal salt (salting liquid that such as organic salt such as acetate, citrate forms in water or organic solvent), described metal salt solution is a kind of metal salt solution, or the mixed solution of two or more metal salt solutions.
Cavity of the present invention is the cavity that can heat, and can be both traditional heat conduction mode of heating, as Resistant heating, heated by natural gas etc.; Also can be a mode of heating, as heating using microwave, eddy-current heating, electric spark heating etc.
The material of cavity of the present invention can be metal material, can be also non-metal stupalith, and the shape of cavity can be cylinder, four directions and six sides etc., and can keep temperature constant state in the temperature of setting.
Precursor solution of the present invention is pyrolytic reaction can at high temperature occur or the metal salt solution of pyrolysis and reduction reaction and the mixed liquor that contains carbonaceous dispersion liquid can occur simultaneously, and wherein the concentration of each composition can design and determine according to the requirement of producing or test.
Precursor solution of the present invention need to mix, can be by fully stirring and realize, and agitating mode can be mechanical agitation, electromagnetic agitation etc., mixing time is determined according to the concentration of slaine in precursor solution and carbonaceous dispersion liquid.
Carbonaceous of the present invention can be Graphene, CNT, amorphous carbon, carbon fiber, fullerene etc., can be also to process above carbonaceous through functionalization or other; Carbonaceous dispersion liquid can be the solution of carbonaceous in the organic solvents such as water, dimethyl formamide, methyl pyrrolidone.
Atomising device of the present invention can be mechanical atomization, as direct-injection type, centrifugal and rotary-atomizing mode etc., can be also the forms such as ultrasonic atomization.
To be precursor solution there is decomposition reaction having to have in the high temperature of oxygen atmosphere cavity to pyrolytic reaction of the present invention, or in the high temperature cavity with reducing atmosphere, occur to decompose and reduction reaction simultaneously.
Reducing atmosphere of the present invention can be the atmosphere that hydrogen, carbon monoxide, decomposition ammonia, natural gas etc. have reduction;
Dust arrester installation described in step of the present invention can be that bag collection, electrostatic dust collection, magnetic force gather dust and the device of powder is collected in whirlwind harvest etc.
Compared with the method that the present invention prepares composite powder with tradition, it is better that its beneficial effect is that prepared carbonaceous strengthens the dispersiveness of the carbonaceous in metal/metal oxide composite powder, the particle size of metal is less, size distribution is more controlled, sphericity is higher, the uniformity of composite powder and mobility are all better than existing preparation method, this is because prepare in the process of carbonaceous enhancing metal/metal oxide composite powder at spray pyrolysis, the mixed solution of metal salt solution and carbonaceous diffusion liquid is atomized into drop and passes in cavity and react, under the effect and cavity high temperature action of Surface Tension of Liquid Drops, in a drop, decompose, or occur to decompose and a powder particle of reduction reaction generation simultaneously, the size of drop can be by atomising device control very tiny, the time that powder particle stops in high temperature cavity the inside is very short, thereby can effectively avoid occurring secondary agglomeration.
The advantage that the present invention has and good effect
(1) method of preparing carbonaceous enhancing metal/metal oxide composite powder of the present invention, safe and reliable, environmental friendliness, and handling process is short, and technique is simple, and output is high, is easy to accomplish scale production.
(2) the prepared carbonaceous of the inventive method strengthens in metal/metal oxide composite powder, and the size of composite powder particle can reach nanometer and Ultra-fine Grained rank, and size distribution is controlled, and constituent is even.
(3) the process major part of preparation carbonaceous enhancing metal/metal oxide composite powder of the present invention is to carry out in enclosed environment, and the purity of gained powder is high.
Brief description of the drawings
Fig. 1 is the scanning electron microscope image that the carbonaceous prepared of embodiment 1 strengthens burning composite powder.
Fig. 2 is the images of transmissive electron microscope that the carbonaceous prepared of embodiment 1 strengthens burning composite powder.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in further details, but protection scope of the present invention is not limited to described content.
Embodiment1
The present embodiment provides carbonaceous to strengthen the preparation method of metal/metal oxide composite powder:
(1) weigh 50g Schweinfurt green solution and put into the deionized water of 5000ml and obtain Schweinfurt green solution, the carbon nanotube dispersed that weighs 1g obtains carbon nano tube dispersion liquid in the water of 1000ml;
(2) mix after ready step (1) Schweinfurt green solution and carbon nano tube dispersion liquid are fully stirred and obtain precursor solution, precursor solution is poured in the storage bin of ultrasonic atomizing device, connect the outlet of atomising device and high temperature cavity (in advance resistance heated be warmed up to 450 DEG C and keep constant temperature) import, open atomising device, start atomization;
(3) opening dust collecting system collects, and the composite powder that pyrolytic is produced is collected and is obtained CNT enhancing cupric oxide composite powder by cyclone dust collection, as depicted in figs. 1 and 2, as seen from the figure: copper oxide particle disperses better, and better with the combination of CNT, CNT is embedded in copper oxide particle.
Embodiment2
The present embodiment provides carbonaceous to strengthen the preparation method of metal/metal oxide composite powder:
(1) weigh 100g copper nitrate solution and put into the deionized water of 1000ml and obtain copper nitrate solution, the Graphene that weighs 1g is distributed in the water of 800ml and obtains graphene dispersing solution;
(2) mix after the ready copper nitrate solution of step (1) and graphene dispersing solution are fully stirred and obtain precursor solution, precursor solution is poured in the storage bin of ultrasonic atomizing device, connect the outlet of atomising device and high temperature cavity (in advance eddy-current heating be warmed up to 600 DEG C and keep constant temperature) import, open atomising device, start atomization;
(3) open dust collecting system and collect, and the composite powder that pyrolytic is produced is collected and obtained Graphene enhancing cupric oxide composite powder by bag collection.
Embodiment3
The present embodiment provides carbonaceous to strengthen the preparation method of metal/metal oxide composite powder:
(1) weigh 50g cobalt chloride solution and put into the deionized water of 2000ml and obtain cobalt chloride solution, the fullerene that weighs 1g is distributed in the water of 1000ml and obtains fullerene dispersion liquid;
(2) mix after the ready cobalt chloride solution of step (1) and fullerene dispersion liquid are fully stirred and obtain precursor solution, precursor solution is poured in the storage bin of ultrasonic atomizing device, connect the outlet of atomising device and high temperature cavity (in advance heated by microwave be warmed up to 550 DEG C and keep constant temperature) import, open atomising device, start atomization;
(3) open dust collecting system and collect, and the composite powder that pyrolytic is produced is collected and obtained fullerene enhancing cobalt oxide composite powder by electrostatic dust collection.
Embodiment4
The present embodiment provides carbonaceous to strengthen the preparation method of metal/metal oxide composite powder:
(1) weigh 50g copper carbonate solution and put into the deionized water of 1500ml and obtain copper carbonate solution, the carbon nanotube dispersed that weighs 1g obtains carbon nano tube dispersion liquid in the water of 500ml;
(2) mix after ready step (1) copper carbonate solution and carbon nano tube dispersion liquid are fully stirred and obtain precursor solution, precursor solution is poured in the storage bin of two flow atomization devices, connect the outlet of atomising device and high temperature cavity (in advance resistance heated be warmed up to 800 DEG C and keep constant temperature) import, pass into nitrogen and hydrogen volume than the mixed atmosphere of 9:1, open atomising device, start atomization;
(3) open dust collecting system and collect, and the composite powder that pyrolytic is produced is collected and obtained carbon nanotube reinforced copper composite powder by bag collection.
Embodiment5
The present embodiment provides carbonaceous to strengthen the preparation method of metal/metal oxide composite powder:
(1) weigh 50g aluminum nitrate solution and put into the deionized water of 2000ml and obtain aluminum nitrate solution, the carbon nanotube dispersed that weighs 1g obtains carbon nano tube dispersion liquid in the water of 2000ml;
(2) mix after the ready aluminum nitrate solution of step (1) and carbon nano tube dispersion liquid are fully stirred and obtain precursor solution, precursor solution is poured in the storage bin of ultrasonic atomizing device, connect the outlet of atomising device and high temperature cavity (in advance heated by natural gas be warmed up to 1150 DEG C and keep constant temperature) import, open atomising device, start atomization;
(3) open dust collecting system and collect, and the composite powder that pyrolytic is produced is collected and obtained CNT enhancing alumina composite powder by cyclone dust collection.
Embodiment6
The present embodiment provides carbonaceous to strengthen the preparation method of metal/metal oxide composite powder:
(1) weigh 20g nickel oxalate solution and put into the deionized water of 1000ml and obtain nickel oxalate solution, the carbon nanotube dispersed that weighs 1g obtains carbon nano tube dispersion liquid in the water of 500ml;
(2) mix after ready step (1) nickel oxalate solution and carbon nano tube dispersion liquid are fully stirred and obtain precursor solution, precursor solution is poured in the storage bin of ultrasonic atomizing device, connect the outlet of atomising device and high temperature cavity (in advance resistance heated be warmed up to 300 DEG C and keep constant temperature) import, open atomising device, start atomization;
(3) open dust collecting system and collect, and the composite powder that pyrolytic is produced is collected and obtained CNT and strengthen Ni-based composite powder by electrostatic dust collection.
Embodiment7
The present embodiment provides carbonaceous to strengthen the preparation method of metal/metal oxide composite powder:
(1) weigh 5g secondary tungsten acid ammonium solution and put into the deionized water of 500ml and obtain secondary tungsten acid ammonium solution, the carbon nanotube dispersed that weighs 1g obtains carbon nano tube dispersion liquid in the water of 100ml;
(2) mix after the ready secondary tungsten acid ammonium solution of step (1) and carbon nano tube dispersion liquid are fully stirred and obtain precursor solution, precursor solution is poured in the storage bin of rotary-atomizing device, connect the outlet of atomising device and high temperature cavity (in advance eddy-current heating be warmed up to 600 DEG C and keep constant temperature) import, open atomising device, start atomization;
(3) open dust collecting system and collect, and the composite powder that pyrolytic is produced is collected and obtained CNT enhancing tungsten oxide composite powder by electrostatic dust collection.
Embodiment 8
The present embodiment provides carbonaceous to strengthen the preparation method of metal/metal oxide composite powder:
(1) weigh 200g ferrous citrate salting liquid and put into the deionized water of 5000ml and obtain ferrous citrate salting liquid, weigh the graphene dispersing solution 20ml that contains 6.0wt% and add solution;
(2) mix after ready step (1) ferrous citrate salting liquid and graphene dispersing solution are fully stirred and obtain precursor solution, precursor solution is poured in the storage bin of ultrasonic atomizing device, connect the outlet of atomising device and high temperature cavity (in advance heated by microwave be warmed up to 250 DEG C and keep constant temperature) import, open atomising device, start atomization;
(3) open dust collecting system and collect, and the composite powder that pyrolytic is produced gathers dust to collect by magnetic force and obtains Graphene and strengthen iron oxide composite powder.
Claims (2)
1. the preparation method of a carbonaceous enhancing metal/metal oxide composite powder, it is characterized in that, specifically comprise the following steps: metal salt solution and carbonaceous dispersion liquid are configured to precursor solution, it is fully mixed, then this precursor solution is carried out to atomization by atomising device, enter with the form of drop in the cavity that is heated in advance slaine decomposition temperature, and keep temperature constant, issue raw pyrolytic reaction at aerobic environment, then open dust collecting system and collect, obtain burning composite powder; Or in pyrolytic reaction process, pass into reducing atmosphere, carry out pyrolysis and reduction reaction simultaneously, carbonaceous strengthens metal-based compound powder.
2. carbonaceous according to claim 1 strengthens the preparation method of metal/metal oxide composite powder, it is characterized in that: described slaine is solubility inorganic metal salt or solubility organic metal salt, described metal salt solution is a kind of metal salt solution, or the mixed solution of two or more metal salt solutions.
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