CN107299319A - A kind of preparation method of the core shell structure CuO/Al nanometers thin-film materials containing energy - Google Patents

A kind of preparation method of the core shell structure CuO/Al nanometers thin-film materials containing energy Download PDF

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CN107299319A
CN107299319A CN201710475915.1A CN201710475915A CN107299319A CN 107299319 A CN107299319 A CN 107299319A CN 201710475915 A CN201710475915 A CN 201710475915A CN 107299319 A CN107299319 A CN 107299319A
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thin
cuo
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core shell
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CN107299319B (en
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周翔
姜炜
柯香
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Nanjing University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment

Abstract

The invention discloses the preparation method of a kind of core shell structure CuO/Al nanometers thin-film materials containing energy.Methods described prepares Cr transition zones and Cu films first with vacuum PVD technology in substrate, then substrate is placed in containing NaOH and (NH at room temperature4)2S2O8Mixed liquor in obtain the Cu (OH) with one-dimensional nano structure2Thin-film material, then the thermally treated CuO thin-film materials obtained with one-dimensional nano structure, finally using physical gas phase deposition technology, nanometer Al are coated to CuO one-dimensional nano structures and obtains CuO/Al nanometers of thin-film materials containing energy of core shell structure.Temperature limiting is below 200 DEG C in preparation process of the present invention, compare existing use >=450 DEG C of high-temperature process, energy consumption is significantly reduced, and CuO/Al nanometers of thin-film materials containing energy of obtained core shell structure can be mutually compatible with back-end CMOS process, and preparation process is reproducible.

Description

A kind of preparation method of the core shell structure CuO/Al nanometers thin-film materials containing energy
Technical field
The invention belongs to nano composite material technical field, it is related to a kind of CuO/Al nanometers with core shell structure thin containing energy The preparation method of membrane material.
Background technology
Nanometer thermite is made up of the oxidant of nanoscale with reducing agent, also referred to as metastable state intermolecular complex.Group Divide after nanosizing, specific surface area is dramatically increased, oxidant increases with reducing agent contact area, diffusion mass transfer distance reduces, chemical Reaction rate increases sharply.In addition, dramatically increasing for surface energy causes the reactivity of nanometer thermite to strengthen, reaction activity Reduction, reduces the energy expenditure in reaction elicitation procedure.The high volume energy density of nanometer thermite, high chemical reaction rate Make it containing can the field such as Ignition chip, micro-nano satellite gesture stability and propulsion, micro fluid dynamcis, minimally invasive sterilizing etc. excellent specific property Have broad application prospects.Compared to ultrasonic random mixing gained nanometer thermite, the nanometer aluminothermy designed through specific structure Agent has larger improvement on the uniform spatial distribution and interface cohesion tight ness rating of oxidant and reducing agent, therefore with more excellent Energy Release more.
Kaili Zhang etc. have carried out the initiative work in part in CuO/Al nanometers of fields of the thin film study containing energy of core shell structure Make, deposited in 1 μ m-thick Cu films to silicon base, then substrate is placed in tube furnace, in air atmosphere by electro-plating method Room temperature is naturally cooled to after being heated to 450 DEG C, insulation 5h, CuO nano wires are obtained, received finally by vacuum thermal evaporation methods deposition Rice Al parcel CuO nano wires, thus obtain CuO/Al nanometer of the core shell structure films containing energy (Applied Physics Letters, 2007,91 (11)：113117；Journal of Microelectromechanical Systems, 2008,17 (4)：832- 836；Journal of Materials Science, 2012,47 (3)：1296-1305).Core shell structure prepared by this method The CuO/Al nanometers of films containing energy have the advantages that contact is close, purity is high, size adjustable and thermal discharge are high between component, but it is prepared 450 DEG C of high-temperature process employed in process bring following two subject matter：During one is due to Cu film thermal oxidation process Stress problem, causes CuO nano wire films easily to come off, yield rate is low；Two be that high-temperature process energy consumption is very big, and and rear end CMOS technology is incompatible.Wenchao Zhang etc. have studied the nuclear shell structure nano based on three-dimensional ordered macroporous oxide containing energy Thin-film material, forms A Polystyrene Spheres Template, then impregnating metal salt precursor on the glass substrate by colloidal crystal template method Body, then removing template is removed while making metal salt be decomposed into respective metal oxide, finally by physical vacuum through 500 DEG C of high-temperature calcinations CVD method coats nanometer Al, so as to obtain nuclear shell structure nano thin-film material containing energy (ACS Applied Materials＆Interfaces, 2013,5 (2)：239-242；Scientific Reports, 2016,6：22588).The party Method can be used for preparing a variety of nanometers film thermite containing energy, but oxide framework structure is easily caved in preparation process, prepares weight Renaturation is difficult to ensure that, and high-temperature process is still needed in preparation process.
The content of the invention
It is an object of the invention to provide in a kind of preparation process without high-temperature process (≤200 DEG C), with core shell structure And the preparation method of the CuO/Al nanometers of excellent response characteristic thin-film material containing energy.
The technical solution for realizing the object of the invention is：
The preparation method of a kind of core shell structure CuO/Al nanometers thin-film materials containing energy, first with vacuum PVD Technology prepares Cr transition zones and Cu films in substrate, then substrate is placed in containing NaOH and (NH at room temperature4)2S2O8It is mixed Close in liquid and obtain the Cu (OH) with one-dimensional nano structure2Thin-film material, it is then thermally treated to obtain with one-dimensional nano structure CuO thin-film materials, finally nanometer Al is coated using physical gas phase deposition technology and obtains nucleocapsid to CuO one-dimensional nano structures UO/Al nanometers of thin-film materials containing energy of structure C, are comprised the following steps that：
The first step, Cr transition zones and Cu films are prepared using vacuum PVD technology in substrate；
Second step, NaOH concentration is placed in for 3~4mol/ by the substrate for being coated with Cr transition zones and Cu films that the first step is obtained L and (NH4)2S2O8Concentration is in 0.15~0.2mol/L mixed liquor, 5~10min of reaction is had through surface oxidation treatment There is the Cu (OH) of one-dimensional nano structure2Thin-film material；
3rd step, the Cu (OH) with one-dimensional nano structure that second step is obtained2Thin-film material is passed through in air atmosphere 180~200 DEG C of heat treatments, obtain the CuO thin-film materials with one-dimensional nano structure；
4th step, using vacuum PVD technology, nanometer Al, which is coated to what the 3rd step was obtained, has a wiener The CuO thin-film materials of rice structure, obtain CuO/Al nanometers of thin-film materials containing energy of core shell structure.
In the first step, described substrate is silicon base, substrate of glass or ceramic bases, described vacuum PVD Technology is magnetron sputtering technique or electron beam evaporation technique.
In the first step, described Cr transition region thicknesses are 20~30nm, and described Cu film thicknesses are 500~1000nm.
In 3rd step, heating rate is 3~5 DEG C/min, 4~6h of soaking time.
In 4th step, described vacuum PVD technology is thermal evaporation techniques or magnetron sputtering technique, Al films Thickness is 1~2 μm.
The present invention compared with prior art, the advantage is that：
In the preparation process of CuO/Al nanometer of the core shell structure of present invention thin-film materials containing energy temperature limiting 200 DEG C with Under, mutually use than before in method >=450 DEG C of high-temperature process, energy consumption substantially reduces, and with back-end CMOS process phase Compatibility, preparation process is reproducible.
Brief description of the drawings
Fig. 1 is the preparation process schematic diagram of CuO/Al nanometers thin-film material containing energy of core shell structure.
Fig. 2 is the SEM figures of CuO one-dimensional nano structures made from embodiment 1.
Fig. 3 is the obtained CuO/Al with core shell structure of embodiment 1 SEM figures.
Fig. 4 is the obtained CuO/Al with core shell structure of embodiment 1 TEM figures
Fig. 5 is the obtained CuO/Al with core shell structure of embodiment 1 XRD spectra.
Fig. 6 is the obtained CuO/Al with core shell structure of embodiment 1 DSC figures.
Fig. 7 is the obtained Cu (OH) for not having one-dimensional nano structure of comparative example2SEM figure.
Embodiment
With reference to embodiment and accompanying drawing, the invention will be further described.
With reference to Fig. 1, a kind of core shell structure CuO/Al nanometers of the invention containing can thin-film materials preparation method, specific steps It is as follows：
The first step, Cr transition zones and Cu films are prepared using vacuum PVD technology in substrate；
Second step, the substrate for being coated with Cr transition zones and Cu films that the first step is obtained is placed in by NaOH solution and (NH4)2S2O8In the mixed liquor of solution composition, the Cu (OH) with one-dimensional nano structure is obtained through surface oxidation treatment2Thin-film material；
3rd step, the Cu (OH) with one-dimensional nano structure that second step is obtained2Thin-film material is placed in Muffle furnace, Through 180~200 DEG C of heat treatments in air atmosphere, the CuO thin-film materials with one-dimensional nano structure are obtained；
4th step, using magnetron sputtered deposition technology, nanometer Al, which is coated to what the 3rd step was obtained, has 1-dimention nano knot The CuO thin-film materials of structure, obtain CuO/Al nanometers of thin-film materials containing energy of core shell structure.
Embodiment 1
The first step：Using magnetron sputtering technique in silicon substrate bottom sediments 20nm thickness Cr transition zones and 500nm thickness Cu films；
Second step, by the silicon base for being coated with 20nm thickness Cr transition zones and 500nm thickness Cu films that the first step is obtained be placed in by 3mol/L NaOH solutions and 0.15mol/L (NH4)2S2O8In the mixed liquor of solution composition, through 5min surface oxidation treatments, obtain Cu (OH) with one-dimensional nano structure2Thin-film material；
3rd step, the Cu (OH) with one-dimensional nano structure that second step is obtained2Thin-film material is placed in Muffle furnace, warp 3 DEG C/min heating rates are warming up to 180 DEG C, are incubated 4h, obtain the CuO thin-film materials with one-dimensional nano structure, pass through SEM tables Its surface microstructure is levied, as a result as shown in Figure 2；
4th step, using magnetron sputtered deposition technology, the tool that 1 μm of Al film coateds of nominal thickness are obtained to the 3rd step There are the CuO thin-film materials of one-dimensional nano structure, obtain CuO/Al nanometers of thin-film materials containing energy of core shell structure, it is characterized by SEM Surface microstructure, as a result as shown in Figure 3；CuO/Al core shell structures are characterized by TEM, as a result as shown in Figure 4；Pass through XRD tables Its structure composition is levied, as a result as shown in Figure 5；Its exothermicity is characterized by DSC, as a result as shown in fig. 6, at 210~400 DEG C, 520 DEG C~Al melts, and has an exothermic peak after Al fusings respectively, and total thermal discharge about 2000J/g shows prepared material tool There is excellent response characteristic.
Embodiment 2
The first step：30nm thickness Cr transition zones are deposited in substrate of glass and 1000nm thickness Cu is thin using electron beam evaporation technique Film；
Second step, by the silicon base for being coated with 30nm thickness Cr transition zones and 1000nm thickness Cu films that the first step is obtained be placed in by 4mol/L NaOH solutions and 0.2mol/L (NH4)2S2O8In the mixed liquor of solution composition, through 10min surface oxidation treatments, obtain Cu (OH) with one-dimensional nano structure2Thin-film material；
3rd step, the Cu (OH) with one-dimensional nano structure that second step is obtained2Thin-film material is placed in Muffle furnace, warp 5 DEG C/min heating rates are warming up to 200 DEG C, are incubated 6h, obtain the CuO thin-film materials with one-dimensional nano structure；
4th step, it is using thermal evaporation techniques, having of obtaining of 2 μm of Al film coateds to the 3rd step of nominal thickness is one-dimensional The CuO thin-film materials of nanostructured, obtain CuO/Al nanometers of thin-film materials containing energy of core shell structure.
The core shell structure CuO/Al nanometers of microstructure of the thin-film material surface containing energy, core shell structure, knot made from the present embodiment Structure is constituted and exothermicity is similar to Example 1.
Comparative example
The first step：30nm thickness Cr transition zones are deposited in substrate of glass and 1000nm thickness Cu is thin using electron beam evaporation technique Film；
Second step, by the silicon base for being coated with 30nm thickness Cr transition zones and 1000nm thickness Cu films that the first step is obtained be placed in by 4mol/L NaOH solutions and 0.2mol/L (NH4)2S2O8In the mixed liquor of solution composition, through 15min surface oxidation treatments, obtain Cu (OH)2Without one-dimensional nano structure, its SEM figures as shown in fig. 7, the explanation reaction time is to Cu (OH)2One-dimensional nano structure Preparation so that follow-up CuO/Al core shell structures formation it is most important.

Claims (6)

1. the preparation method of a kind of core shell structure CuO/Al nanometers thin-film materials containing energy, it is characterised in that comprise the following steps that：
The first step, Cr transition zones and Cu films are prepared using vacuum PVD technology in substrate；
Second step, by the substrate for being coated with Cr transition zones and Cu films that the first step is obtained be placed in NaOH concentration for 3~4mol/L and (NH4)2S2O8Concentration obtains having one through surface oxidation treatment in 0.15~0.2mol/L mixed liquor, to react 5~10min The Cu (OH) of dimension nanometer construction2Thin-film material；
3rd step, the Cu (OH) with one-dimensional nano structure that second step is obtained2Thin-film material in air atmosphere through 180~ 200 DEG C of heat treatments, obtain the CuO thin-film materials with one-dimensional nano structure；
4th step, using vacuum PVD technology, nanometer Al, which is coated to what the 3rd step was obtained, has 1-dimention nano knot The CuO thin-film materials of structure, obtain CuO/Al nanometers of thin-film materials containing energy of core shell structure.
2. preparation method according to claim 1, it is characterised in that in the first step, described substrate is silicon base, glass Substrate or ceramic bases, described vacuum PVD technology are magnetron sputtering technique or electron beam evaporation technique.
3. preparation method according to claim 1, it is characterised in that in the first step, described Cr transition region thicknesses are 20 ~30nm, described Cu film thicknesses are 500~1000nm.
4. preparation method according to claim 1, it is characterised in that in the 3rd step, heating rate is 3~5 DEG C/min, protect Warm 4~6h of time.
5. preparation method according to claim 1, it is characterised in that in the 4th step, described vacuum PVD Technology is thermal evaporation techniques or magnetron sputtering technique.
6. preparation method according to claim 1, it is characterised in that in the 4th step, Al film thicknesses are 1~2 μm.
CN201710475915.1A 2017-06-21 2017-06-21 A kind of preparation method of the core-shell structure CuO/Al nanometers of thin-film materials containing energy Active CN107299319B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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CN109295418A (en) * 2018-10-10 2019-02-01 重庆大学 Highly exothermic amount Al/CuO 3D nucleocapsid array structure thermite with high load capacity
CN109680309A (en) * 2019-03-06 2019-04-26 重庆大学 Super hydrophobic porous Al/CuO nanometers of aluminothermy composite material containing energy

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CN105693442A (en) * 2016-01-21 2016-06-22 电子科技大学 Ignition bridge with lattice-shaped energy-containing thin film
CN106226382A (en) * 2016-08-08 2016-12-14 北京科技大学 Nano porous copper/Cu (OH)2nano-wire array sensor electrode material and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109295418A (en) * 2018-10-10 2019-02-01 重庆大学 Highly exothermic amount Al/CuO 3D nucleocapsid array structure thermite with high load capacity
CN109295418B (en) * 2018-10-10 2020-09-25 重庆大学 High-heat-release Al/CuO 3D core-shell array structure thermite with extremely high load capacity
CN109680309A (en) * 2019-03-06 2019-04-26 重庆大学 Super hydrophobic porous Al/CuO nanometers of aluminothermy composite material containing energy

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