CN108202145A - A kind of preparation method of nano aluminium oxide/copper composite strengthening phase - Google Patents
A kind of preparation method of nano aluminium oxide/copper composite strengthening phase Download PDFInfo
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- CN108202145A CN108202145A CN201810020952.8A CN201810020952A CN108202145A CN 108202145 A CN108202145 A CN 108202145A CN 201810020952 A CN201810020952 A CN 201810020952A CN 108202145 A CN108202145 A CN 108202145A
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- Prior art keywords
- copper
- aluminium
- mantoquita
- aluminium oxide
- mixed solution
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Links
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 202
- 239000002131 composite material Substances 0.000 title claims abstract description 75
- 239000010949 copper Substances 0.000 title claims abstract description 56
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 55
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000005728 strengthening Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 42
- 159000000013 aluminium salts Chemical class 0.000 claims abstract description 37
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 19
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 19
- 229940112669 cuprous oxide Drugs 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 238000000197 pyrolysis Methods 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical group [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 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 5
- 230000003993 interaction Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000003595 mist Substances 0.000 claims description 2
- 238000009938 salting Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- -1 Copper Salt Chemical class 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 10
- 238000005118 spray pyrolysis Methods 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 239000005022 packaging material Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 229910052593 corundum Inorganic materials 0.000 description 18
- 239000010431 corundum Substances 0.000 description 15
- 238000010586 diagram Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000013019 agitation Methods 0.000 description 6
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000005979 thermal decomposition reaction Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical class [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005406 washing Methods 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
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1089—Alloys containing non-metals by partial reduction or decomposition of a solid metal compound
Abstract
The present invention relates to a kind of preparation methods of nano aluminium oxide/copper composite strengthening phase, belong to PM technique and technical field of composite preparation.The method of the invention is to prepare mantoquita and the mixed solution of aluminium salt, it is tightly combined using the method for spray pyrolysis and reduction calcining, uniformly tiny nano-level sphere aluminium oxide/copper composite strengthening phase, the composite strengthening powder can be effective for enhancing metal-base composites.The method of the invention has the characteristics that process is simple and convenient to operate, production process is continuous, production capacity is big, production efficiency is high, the aluminium oxide of preparation/copper composite strengthening is mutually nano level size, and copper and alumina dispersion are uniform, and wherein the molar ratio of aluminium oxide and copper can be regulated and controled by adjusting the concentration of solution.
Description
Technical field
The present invention relates to a kind of preparation methods of nano aluminium oxide/copper composite strengthening phase, belong to PM technique and answer
Condensation material preparing technical field.
Background technology
Copper and Cu-base composites because with good electric conductivity, thermal conductivity, corrosion resistance and excellent craftsmanship and
It easily recycles and is used widely as functional material.But copper-based conductive, heat-conductive composite material is in general, conductance
Then intensity is low for rate height, and electricity, hot property can then be lost by improving its intensity.To improve under the premise of the electricity of guarantee material, hot property
Its mechanical property, especially thermal stability, a kind of effective method are using disperse reinforcement（Such as alumina particle）Come to copper
Matrix is strengthened.
Al is prepared at present2O3Dispersed particle-strengthened Cu-base composites are mainly using conventional powder metallurgical method, mechanical alloying
Method, sol-gel method and internal oxidation.Conventional powder metallurgical method technical maturity, but due to being difficult to that nanometer is made according to a conventional method
The Al of grade2O3Powder, it is impossible to while realize Al2O3The refinement of particle and distribution uniformity.And coarse Al2O3Particle can limit
Al2O3The raising of/Cu composite properties.The crystallite dimension that mechanical alloying method obtains is larger and production control is difficult, molten
Glue-gel method technical process is easy to control, and material property obtained is preferable, at present still in experimental stage, internal oxidation technique
Process is complicated, and technical parameter difficulty is big, and manufacture is of high cost.
It is molten that various metal salts are made into presoma by spray-wall interaction according to the stoichiometric ratio prepared needed for compound powder
Liquid after atomizer is atomized, is brought by carrier gas in high temperature reaction stove, and moment completes evaporation of the solvent in reacting furnace, solute precipitates
The a series of physical and chemical processes such as solid particle, particle drying, particle thermal decomposition, sinter molding are formed, are eventually formed ultra-fine
Powder.Raw material mixes under solution state, it is ensured that uniform component distribution, and also technical process is simple, and component loss is few, can essence
Really control stoichiometric ratio, is especially suitable for preparing multicomponent composite powder.Micro mist by the aerial droplet drying of suspending,
Particle, without subsequent washing grinding, ensure that the high-purity of product, high activity generally in the spherical shape of rule, and reunite less.
Whole process was quickly completed at short several seconds, therefore drop has little time that solute segregation occurs during the reaction, further
Ensure the homogeneity of component distribution.
Therefore, the present invention prepares aluminium oxide/copper composite strengthening phase using the method that spray pyrolysis and reduction calcining are combined.
Invention content
The purpose of the present invention in view of the problems of the existing technology, provide a kind of spray-wall interaction prepare it is nano oxidized
The method of aluminium/copper composite strengthening phase using mantoquita and aluminium salt mixed solution as precursor liquid, is obtained equal using the method for spray-wall interaction
The composite powder of even and fine small aluminium oxide/cuprous oxide under the high temperature conditions, fine uniform is obtained using the mode of reduction calcining
Alumina in Nano level/copper composite strengthening phase.
A kind of preparation method of nano aluminium oxide/copper composite strengthening phase, is as follows：
（1）The configuration of mantoquita and aluminium salt mixed solution：The mantoquita of weighing and aluminium salt are added in the container equipped with deionized water, room
Under the conditions of temperature, mantoquita and the mixed solution of aluminium salt are configured to by stirring, the molar concentration of mantoquita is in mixed solution
0.001mol/L ~ saturated concentration, the molar concentration of aluminium salt is 0.001mol/L ~ saturated concentration；
（2）Mantoquita/aluminium salt mixed solution spraying pyrolysis：Diamond heating is warming up to certain temperature, by step（1）Gained mixes
It closes salting liquid to be poured into atomizer, the droplet for being atomized generation is passed into progress spray-wall interaction reaction in tube furnace, so
It collects afterwards and obtains aluminium oxide/cuprous oxide composite powder；
（3）Aluminium oxide/cuprous oxide reduction calcining：By step（2）Gained composite powder is fitted into boat, is then placed in tube furnace
In, reduction calcining acquisition aluminium oxide/copper composite strengthening phase in weak reducing atmosphere.
Step of the present invention（1）Middle mantoquita is one or more of copper acetate, copper nitrate, copper sulphate, copper chloride by arbitrary
Than mixing, aluminium salt is aluminum nitrate, one or more of aluminum sulfate, aluminium chloride is mixed by any ratio.
Preferably, step of the present invention（1）Mixing time is 30 ~ 120 min, the concentration of mantoquita and aluminium salt is respectively 0.01 ~
1.0 mol/L。
Step of the present invention（2）Mantoquita/aluminium salt mixed solution spraying pyrolytic reaction detailed process is：Mantoquita/aluminium salt is mixed
Solution is poured into atomizer, and wherein the power of atomizer is 25 ~ 100 W/L, will when tubular type furnace temperature rises to 600 ~ 750 DEG C
Atomizer opens spray patterns, and mantoquita/aluminium salt mixed solution experienced evaporation, drying, subsequent mantoquita/aluminium salt jointly in low-temperature space
Solution is undergone in high-temperature region to be thermally decomposed, and generates nano cuprous oxide and aluminium oxide,（Wherein, high-temperature region is exactly heating zone, low-temperature space
It is exactly the region of heat transfer）.
Step of the present invention（3）Middle weakly reducing atmosphere is：Inert atmosphere and hydrogen or nitric oxide production mixed gas, reduction
Calcination temperature is 950 ~ 1250 DEG C, and the time is 0.5 ~ 4.0 h.
The beneficial effects of the invention are as follows：
（1）Aluminium oxide/copper composite strengthening prepared by the method for the present invention is mutually nano level size, and copper and alumina dispersion are equal
Even, wherein the molar ratio of aluminium oxide and copper can be regulated and controled by adjusting the concentration of solution.
（2）The characteristics of aluminium oxide/copper composite strengthening prepared by the method for the present invention mutually makes full use of spray pyrolysis, mantoquita/aluminium
Mixed salt solution experienced evaporation, drying jointly in low-temperature space, and subsequent mantoquita/aluminium salt mixed solution is undergone in high-temperature region to be thermally decomposed
It generates nano aluminium oxide/cuprous oxide and the two interface is combined closely, aluminium oxide/cuprous oxide restores acquisition under hydrogen atmosphere
Nano level aluminium oxide/copper composite strengthening phase, is conducive to dispersed and strengthened copper-based composite material, obtains relatively good enhancing effect.
（3）The method of the present invention prepares the simple for process of aluminium oxide/copper composite strengthening phase, is calcined by spray pyrolysis+reduction
Two steps just obtain composite strengthening phase, and production efficiency is high.
Description of the drawings
Fig. 1 is the XRD diagram of 1 aluminium oxide of embodiment/copper.
Fig. 2 is 1 aluminium oxide of embodiment/copper composite strengthening phase SEM figures.
Fig. 3 is 1 aluminium oxide of embodiment/copper composite strengthening phase EDX spot scan figures.
Fig. 4 is 1 aluminium oxide of embodiment/copper composite strengthening phase energy spectrum diagram 1.
Fig. 5 is 1 aluminium oxide of embodiment/copper composite strengthening phase energy spectrum diagram 2.
Fig. 6 is 1 aluminium oxide of embodiment/copper composite strengthening phase energy spectrum diagram 3.
Fig. 7 is 1 aluminium oxide of embodiment/copper composite strengthening phase energy spectrum diagram 4.
Fig. 8 is 1 aluminium oxide of embodiment/copper composite strengthening phase energy spectrum diagram 5.
Fig. 9 is 1 aluminium oxide of embodiment/copper composite strengthening phase energy spectrum diagram 6.
Specific embodiment
The present invention is described in further detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
Embodiment 1
A kind of preparation method of aluminium oxide/copper composite strengthening phase, is as follows：
（1）The configuration of copper acetate and aluminum nitrate mixed solution：It first weighs 6.0 g copper acetates and adds in the burning equipped with 3 L deionized waters
In cup, 11.3g aluminum nitrates are then weighed again and are added in the beaker for the 3 L deionized waters that front adds in mantoquita, under room temperature, lead to
Crossing 30 min of magnetic agitation makes it fully dissolve the mixed solution for being configured to mantoquita and aluminium salt；Obtained mantoquita and the concentration of aluminium salt
It is 0.01mol/L；
（2）Mixed solution spraying pyrolysis：By step（1）The mixed solution of middle configuration is poured into atomizer, when diamond heating liter
Atomizer when temperature rise is to 600 DEG C, is opened spray patterns by temperature（Atomizer is located at one end of tube furnace）, power is set
For 75W, the mixed solution of mantoquita and aluminium salt undergoes evaporation, drying jointly by the drop that ultrasonic atomizatio generates in low-temperature space, with
Mixed solution obtains aluminium oxide/cuprous oxide composite powder after the experience thermal decomposition of high-temperature region afterwards.
（3）Aluminium oxide/cuprous oxide composite powder reduction；First by step（2）The composite powder of acquisition is encased in corundum boat
In, then the corundum boat equipped with composite powder is put into corundum tube furnace, by tubular type stove evacuation, when vacuum degree in tube furnace
When reaching 0.01 Pa, vacuum pump is closed, is passed through the high-purity argon gas containing 5.0 wt% hydrogen, heated Tube-furnace increases temperature
Aluminium oxide/copper composite strengthening phase is obtained to 950 DEG C of reduction 4.0h.
The microstructure of composite granule manufactured in the present embodiment can be seen that powder as shown in figs 1-9, by SEM figures
For size in nanometer scale, spherical characteristic is presented in morphology microstructure, from XRD results can be seen that its mainly form as aluminium oxide and
Copper, there is no other impurities, and from EDX it can be seen that aluminium oxide disperse in Copper substrate it is visibly homogeneous.
Embodiment 2
A kind of preparation method of aluminium oxide/copper composite strengthening phase, is as follows：
（1）The configuration of copper nitrate and aluminum nitrate mixed solution：Under agitation, the copper nitrate for first weighing 56 g addition is equipped with
It in 3L deionized water beakers, then weighs 113 g aluminum nitrates and adds in the 3L deionized water beakers of front addition mantoquita, at room temperature
It is made fully to dissolve using 40 min of magnetic agitation, be configured to mantoquita and the mixed solution of aluminium salt.Obtained mantoquita and aluminium salt is molten
The concentration of liquid is 0.1mol/L.
（2）Mixed solution spraying pyrolysis：By step（1）The mixed solution of middle configuration is poured into atomizer, when tube furnace plus
Atomizer when temperature rise is to 650 DEG C, is opened spray patterns by heat heating, and setting power is 150W, and mantoquita and aluminium salt are mixed
It closes solution and evaporation, drying is undergone by the drop that ultrasonic atomizatio generates jointly in low-temperature space, subsequent mixed solution is passed through in high-temperature region
Aluminium oxide/cuprous oxide composite powder is obtained after going through thermal decomposition.
（3）Aluminium oxide/cuprous oxide composite powder reduction；First by step（2）The composite powder of acquisition is encased in corundum boat
In, then the corundum boat equipped with composite powder is put into corundum tube furnace, by tubular type stove evacuation, when vacuum degree in tube furnace
When reaching 0.01 Pa, vacuum pump is closed, is passed through the high pure nitrogen containing 5.0 wt% hydrogen, heated Tube-furnace increases temperature
Aluminium oxide/copper composite strengthening phase is obtained to 1050 DEG C of 1.0 h of reduction.
By sem analysis it can be seen that the size of powder is in nanometer scale, spherical characteristic, Er Qietong is presented in morphology microstructure
Cross EDX analysis it can be seen that aluminium oxide disperse in Copper substrate it is visibly homogeneous.
Embodiment 3
A kind of preparation method of aluminium oxide/copper composite strengthening phase, is as follows：
（1）The configuration of copper chloride and aluminium chloride mixed solution：Under agitation, will first weigh copper chloride add in equipped with 3L go from
It in sub- water beaker, then weighs aluminium chloride and adds in the 3L deionized water beakers of front addition mantoquita, stirred at room temperature using magnetic force
Mixing 40 min makes it fully dissolve, and is configured to mantoquita and the mixed solution of aluminium salt.Obtained mantoquita and the solution of aluminium salt it is dense
Degree is 1.0 mol/L.
（2）Mixed solution spraying pyrolysis：By step（1）The mixed solution of middle configuration is poured into atomizer, when tube furnace plus
Atomizer when temperature rise is to 650 DEG C, is opened spray patterns by heat heating, and setting power is 300W, and mantoquita and aluminium salt are mixed
It closes solution and evaporation, drying is undergone by the drop that ultrasonic atomizatio generates jointly in low-temperature space, subsequent mixed solution is passed through in high-temperature region
Aluminium oxide/cuprous oxide composite powder is obtained after going through thermal decomposition.
（3）Aluminium oxide/cuprous oxide composite powder reduction；First by step（2）The composite powder of acquisition is encased in corundum boat
In, then the corundum boat equipped with composite powder is put into corundum tube furnace, by tubular type stove evacuation, when vacuum degree in tube furnace
When reaching 0.01 Pa, vacuum pump is closed, is passed through the nitrogen containing 5.0 wt% carbon monoxide, heated Tube-furnace increases temperature
Aluminium oxide/copper composite strengthening phase is obtained to 1250 DEG C of reduction 0.5h.
By sem analysis it can be seen that the size of powder is in nanometer scale, spherical characteristic, Er Qietong is presented in morphology microstructure
Cross EDX analysis it can be seen that aluminium oxide disperse in Copper substrate it is visibly homogeneous.
Embodiment 4
A kind of preparation method of aluminium oxide/copper composite strengthening phase, is as follows：
（1）The configuration of copper sulphate and aluminum sulfate mixture solution：Under agitation, will first weigh copper sulphate add in equipped with 3L go from
It in sub- water beaker, then weighs 113 g aluminum sulfate and adds in the 3L deionized water beakers of front addition mantoquita, at room temperature using magnetic
Power, which stirs 60 min, makes it fully dissolve, and is configured to mantoquita and the mixed solution of aluminium salt, obtained mantoquita and aluminum salt solution it is dense
Degree is 0.5 mol/L.
（2）Mixed solution spraying pyrolysis：By step（1）The mixed solution of middle configuration is poured into atomizer, when tube furnace plus
Atomizer when temperature rise is to 650 DEG C, is opened spray patterns by heat heating, and setting power is 150W, and mantoquita and aluminium salt are mixed
It closes solution and evaporation, drying is undergone by the drop that ultrasonic atomizatio generates jointly in low-temperature space, subsequent mixed solution is passed through in high-temperature region
Aluminium oxide/cuprous oxide composite powder is obtained after going through thermal decomposition.
（3）Aluminium oxide/cuprous oxide composite powder reduction；First by step（2）The composite powder of acquisition is encased in corundum boat
In, then the corundum boat equipped with composite powder is put into corundum tube furnace, by tubular type stove evacuation, when vacuum degree in tube furnace
When reaching 0.01 Pa, vacuum pump is closed, is passed through the high pure nitrogen containing 5.0 wt% hydrogen, heated Tube-furnace increases temperature
Aluminium oxide/copper composite strengthening phase is obtained to 1100 DEG C of 3.0 h of reduction.
By sem analysis it can be seen that the size of powder is in nanometer scale, spherical characteristic, Er Qietong is presented in morphology microstructure
Cross EDX analysis it can be seen that aluminium oxide disperse in Copper substrate it is visibly homogeneous.
Embodiment 5
A kind of preparation method of aluminium oxide/copper composite strengthening phase, is as follows：
（1）The configuration of copper sulphate and aluminum nitrate mixed solution：Under agitation, the copper nitrate first weighed is added in equipped with 10L
It in deionized water beaker, then weighs aluminum nitrate and adds in the 10L deionized water beakers of front addition mantoquita, at room temperature using magnetic
Power, which stirs 30 min, makes it fully dissolve, and is configured to mantoquita and the mixed solution of aluminium salt；Obtained mantoquita and aluminum salt solution it is dense
Degree is 0.1 mol/L.
（2）Mixed solution spraying pyrolysis：By step（1）The mixed solution of middle configuration is poured into atomizer, when tube furnace plus
Atomizer when temperature rise is to 650 DEG C, is opened spray patterns by heat heating, and setting power is 500W, and mantoquita and aluminium salt are mixed
It closes solution and evaporation, drying is undergone by the drop that ultrasonic atomizatio generates jointly in low-temperature space, subsequent mixed solution is passed through in high-temperature region
Aluminium oxide/cuprous oxide composite powder is obtained after going through thermal decomposition.
（3）Aluminium oxide/cuprous oxide composite powder reduction；First by step（2）The composite powder of acquisition is encased in corundum boat
In, then the corundum boat equipped with composite powder is put into corundum tube furnace, by tubular type stove evacuation, when vacuum degree in tube furnace
When reaching 0.01 Pa, vacuum pump is closed, is passed through containing pure hydrogen, temperature is increased to 1050 DEG C of reduction 1.0 by heated Tube-furnace
H obtains aluminium oxide/copper composite strengthening phase.
By sem analysis it can be seen that the size of powder is in nanometer scale, spherical characteristic, Er Qietong is presented in morphology microstructure
Cross EDX analysis it can be seen that aluminium oxide disperse in Copper substrate it is visibly homogeneous.
Claims (5)
1. the preparation method of a kind of nano aluminium oxide/copper composite strengthening phase, which is characterized in that be as follows：
（1）The configuration of mantoquita and aluminium salt mixed solution：The mantoquita of weighing and aluminium salt are added in the container equipped with deionized water, room
Under the conditions of temperature, mantoquita and the mixed solution of aluminium salt are configured to by stirring, the molar concentration of mantoquita is in mixed solution
0.001mol/L ~ saturated concentration, the molar concentration of aluminium salt is 0.001mol/L ~ saturated concentration；
（2）Mantoquita/aluminium salt mixed solution spraying pyrolysis：Diamond heating is warming up to certain temperature, by step（1）Gained mixes
It closes salting liquid to be poured into atomizer, the droplet for being atomized generation is passed into progress spray-wall interaction reaction in tube furnace, so
It collects afterwards and obtains aluminium oxide/cuprous oxide composite powder；
（3）Aluminium oxide/cuprous oxide reduction calcining：By step（2）Gained composite powder is fitted into boat, is then placed in tube furnace
In, reduction calcining acquisition aluminium oxide/copper composite strengthening phase in weak reducing atmosphere.
2. the preparation method of nano aluminium oxide/copper composite strengthening phase according to claim 1, it is characterised in that：Step（1）In
Mantoquita is that one or more of copper acetate, copper nitrate, copper sulphate, copper chloride are mixed by any ratio, and aluminium salt is aluminum nitrate, sulfuric acid
One or more of aluminium, aluminium chloride is mixed by any ratio.
3. the preparation method of nano aluminium oxide/copper composite strengthening phase according to claim 1, it is characterised in that：Step（1）It stirs
The time is mixed as 30 ~ 120 min, the concentration of mantoquita and aluminium salt is respectively 0.01 ~ 1.0 mol/L.
4. the preparation method of nano aluminium oxide/copper composite strengthening phase according to claim 1, it is characterised in that：Step（2）Copper
Salt/aluminium salt mixed solution spraying pyrolytic reaction detailed process is：Mantoquita/aluminium salt mixed solution is poured into atomizer, wherein mist
Change the power of device as 25 ~ 100 W/L, when tubular type furnace temperature rises to 600 ~ 750 DEG C, atomizer is opened into spray patterns, mantoquita/
Aluminium salt mixed solution experienced evaporation, drying jointly in low-temperature space, and subsequent mantoquita/aluminum salt solution is undergone in high-temperature region to be thermally decomposed,
Generate nano cuprous oxide and aluminium oxide.
5. the preparation method of nano aluminium oxide/copper composite strengthening phase according to claim 1, it is characterised in that：Step（3）In
Weakly reducing atmosphere is：Inert atmosphere and hydrogen or nitric oxide production mixed gas, reduction calcination temperature are 950 ~ 1250 DEG C, when
Between be 0.5 ~ 4.0 h.
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