CN107299319B - A kind of preparation method of the core-shell structure CuO/Al nanometers of thin-film materials containing energy - Google Patents

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

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CN107299319B
CN107299319B CN201710475915.1A CN201710475915A CN107299319B CN 107299319 B CN107299319 B CN 107299319B CN 201710475915 A CN201710475915 A CN 201710475915A CN 107299319 B CN107299319 B CN 107299319B
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周翔
姜炜
柯香
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Nanjing University of Science and Technology
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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

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Abstract

The invention discloses the preparation methods of a kind of core-shell structure CuO/Al nanometers thin-film materials containing energy.The method prepares Cr transition zone and Cu film 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, the then thermally treated CuO thin-film material for obtaining having one-dimensional nano structure finally utilize physical gas phase deposition technology, and nanometer Al is coated to obtaining CuO/Al nanometer of the core-shell structure thin-film materials containing energy on CuO one-dimensional nano structure.Temperature is limited in 200 DEG C or less in preparation process of the present invention, compare existing use >=450 DEG C of high-temperature process, energy consumption significantly reduces, and the core-shell structure CuO/Al nanometers of thin-film material containing energy is made 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 of thin-film materials containing energy
Technical field
The invention belongs to nanocomposite technical fields, and it is thin containing energy to be related to a kind of CuO/Al nanometer with core-shell structure The preparation method of membrane material.
Background technique
Nanometer thermite is made of the oxidant of nanoscale with reducing agent, also referred to as metastable state intermolecular complex.Group After dividing nanosizing, specific surface area is dramatically increased, and oxidant and reducing agent contact area increase, and diffusion mass transfer distance reduces, chemical Reaction rate increases sharply.In addition, surface can dramatically increase so that the reactivity of nanometer thermite enhances, reaction activity It reduces, reduces the energy consumption in reaction elicitation procedure.The high volume energy density of nanometer thermite, high chemical reaction rate Etc. excellent characteristics make it containing can the fields such as Ignition chip, micro-nano satellite gesture stability and propulsion, micro fluid dynamcis, minimally invasive sterilizing It has 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 tightness of oxidant and reducing agent, therefore has more excellent Energy Release more.
Kaili Zhang etc. has 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, is deposited on 1 μ m-thick Cu film to silicon base, then substrate is placed in tube furnace, in air atmosphere by electro-plating method 450 DEG C are heated to, cooled to room temperature after 5h is kept the temperature, obtains CuO nano wire, is received finally by vacuum thermal evaporation methods deposition Rice Al wrap up CuO nano wire, thus obtain CuO/Al nanometer of core-shell structure containing energy films (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).The core-shell structure of this method preparation CuO/Al nanometers containing can films have many advantages, such as to contact close, purity is high, size adjustable and thermal discharge between component high, but its preparation 450 DEG C of high-temperature process used by the process bring following two main problem: first is that due in Cu film thermal oxidation process Stress problem causes CuO nano wire film to be easy to fall off, and yield rate is low；Second is that high-temperature process energy consumption is very big, and and rear end CMOS technology is incompatible.Wenchao Zhang etc. has studied the nuclear shell structure nano based on three-dimensional ordered macroporous oxide containing energy Thin-film material forms A Polystyrene Spheres Template by colloidal crystal template method, then impregnating metal salt precursor on the glass substrate Body, then remove removing template through 500 DEG C of high-temperature calcinations while metal salt being made to be decomposed into respective metal oxide, finally by physical vacuum Vapor deposition method coats nanometer Al, 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 easy to collapse in preparation process, preparation weight Renaturation is difficult to ensure, and high-temperature process is still needed in preparation process.
Summary of the invention
The purpose of the present invention is to provide high-temperature process (≤200 DEG C) are not necessarily in a kind of preparation process, there is core-shell structure And the preparation method of the CuO/Al nanometer of excellent response characteristic thin-film material containing energy.
The technical solution for realizing the aim of the invention is as follows:
A kind of preparation method of the core-shell structure CuO/Al nanometers of thin-film materials containing energy, first with vacuum PVD Technology prepares Cr transition zone and Cu film in substrate, then substrate is placed in containing NaOH and (NH at room temperature4)2S2O8It is mixed It closes in liquid and obtains 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 material, finally nanometer Al is coated to obtaining nucleocapsid on CuO one-dimensional nano structure using physical gas phase deposition technology UO/Al nanometers of the structure C thin-film materials containing energy, the specific steps are as follows:
The first step prepares Cr transition zone and Cu film using vacuum PVD technology in substrate；
Second step, the substrate for being coated with Cr transition zone and Cu film that the first step is obtained are placed in NaOH concentration as 3~4mol/ L and (NH4)2S2O8Concentration is to react 5~10min in the mixed liquor of 0.15~0.2mol/L, had through surface oxidation treatment There is the Cu (OH) of one-dimensional nano structure2Thin-film material；
Third step, the Cu (OH) with one-dimensional nano structure that second step is obtained2Thin-film material passes through in air atmosphere 180~200 DEG C of heat treatments, obtain the CuO thin-film material with one-dimensional nano structure；
4th step, using vacuum PVD technology, nanometer Al, which is coated to what third step obtained, has a wiener The CuO thin-film material of rice structure obtains CuO/Al nanometers of the core-shell structure thin-film materials containing energy.
In the first step, the substrate is silicon base, substrate of glass or ceramic bases, the vacuum PVD Technology is magnetron sputtering technique or electron beam evaporation technique.
In the first step, the Cr transition region thickness is 20~30nm, and the Cu film thickness is 500~1000nm.
In third step, heating rate is 3~5 DEG C/min, 4~6h of soaking time.
In 4th step, the vacuum PVD technology is thermal evaporation techniques or magnetron sputtering technique, Al film With a thickness of 1~2 μm.
Compared with prior art, the present invention the advantage is that:
CuO/Al nanometers of core-shell structure of the invention containing can in the preparation process of thin-film materials temperature be limited in 200 DEG C with Under, mutually use in method than before >=450 DEG C of high-temperature process, energy consumption substantially reduces, and with back-end CMOS process phase Compatible, preparation process is reproducible.
Detailed description of the invention
Fig. 1 is the preparation process schematic diagram of CuO/Al nanometer thin-film material containing energy of core-shell structure.
Fig. 2 is the SEM figure of CuO one-dimensional nano structure made from embodiment 1.
Fig. 3 is the SEM figure of the CuO/Al obtained with core-shell structure of embodiment 1.
Fig. 4 is the TEM figure of the CuO/Al obtained with core-shell structure of embodiment 1
Fig. 5 is the XRD spectra of the CuO/Al obtained with core-shell structure of embodiment 1.
Fig. 6 is the DSC figure of the CuO/Al obtained with core-shell structure of embodiment 1.
Fig. 7 is the comparative example Cu (OH) obtained for not having one-dimensional nano structure2SEM figure.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
In conjunction with Fig. 1, the preparation method of the of the invention a kind of core-shell structure CuO/Al nanometers thin-film materials containing energy, specific steps It is as follows:
The first step prepares Cr transition zone and Cu film using vacuum PVD technology in substrate；
Second step, the substrate for being coated with Cr transition zone and Cu film that the first step is obtained are 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；
Third step, the Cu (OH) with one-dimensional nano structure that second step is obtained2Thin-film material is placed in Muffle furnace, It is heat-treated in air atmosphere through 180~200 DEG C, obtains the CuO thin-film material with one-dimensional nano structure；
4th step, using magnetron sputtered deposition technology, nanometer Al, which is coated to what third step obtained, has 1-dimention nano knot The CuO thin-film material of structure obtains CuO/Al nanometers of the core-shell structure thin-film materials containing energy.
Embodiment 1
Step 1: using magnetron sputtering technique in silicon substrate bottom sediments 20nm thickness Cr transition zone and 500nm thickness Cu film；
Second step, the silicon base for being coated with 20nm thickness Cr transition zone and 500nm thickness Cu film that the first step is obtained be placed in by 3mol/L NaOH solution and 0.15mol/L (NH4)2S2O8In the mixed liquor of solution composition, through 5min surface oxidation treatment, obtain Cu (OH) with one-dimensional nano structure2Thin-film material；
Third 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 rate is warming up to 180 DEG C, keeps the temperature 4h, obtains the CuO thin-film material with one-dimensional nano structure, pass through SEM table 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 nominal thickness of Al film coated to third step is obtained There is the CuO thin-film material of one-dimensional nano structure, obtains CuO/Al nanometers of the core-shell structure thin-film materials containing energy, it is characterized by SEM Surface microstructure, as a result as shown in Figure 3；CuO/Al core-shell structure is characterized by TEM, as a result as shown in Figure 4；Pass through XRD table 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, There is an exothermic peak after 520 DEG C~Al fusing and Al fusing respectively, total thermal discharge about 2000J/g shows that material prepared has There is excellent response characteristic.
Embodiment 2
Step 1: thin in substrate of glass deposition 30nm thickness Cr transition zone and 1000nm thickness Cu using electron beam evaporation technique Film；
Second step, the silicon base for being coated with 30nm thickness Cr transition zone and 1000nm thickness Cu film that the first step is obtained be placed in by 4mol/L NaOH solution and 0.2mol/L (NH4)2S2O8In the mixed liquor of solution composition, through 10min surface oxidation treatment, obtain Cu (OH) with one-dimensional nano structure2Thin-film material；
Third 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 rate is warming up to 200 DEG C, keeps the temperature 6h, obtains the CuO thin-film material with one-dimensional nano structure；
4th step, it is using thermal evaporation techniques, having of obtaining of 2 μm of nominal thickness of Al film coated to third step is one-dimensional The CuO thin-film material of nanostructure obtains CuO/Al nanometers of the core-shell structure thin-film materials containing energy.
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 composition and exothermicity are similar to Example 1.
Comparative example
Step 1: thin in substrate of glass deposition 30nm thickness Cr transition zone and 1000nm thickness Cu using electron beam evaporation technique Film；
Second step, the silicon base for being coated with 30nm thickness Cr transition zone and 1000nm thickness Cu film that the first step is obtained be placed in by 4mol/L NaOH solution and 0.2mol/L (NH4)2S2O8In the mixed liquor of solution composition, through 15min surface oxidation treatment, obtain Cu (OH)2Without one-dimensional nano structure, SEM schemes as shown in fig. 7, illustrating the reaction time to Cu (OH)2One-dimensional nano structure Preparation so that subsequent CuO/Al core-shell structure 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, which is characterized in that specific step is as follows:
The first step prepares Cr transition zone and Cu film using vacuum PVD technology in substrate；
Second step, the substrate for being coated with Cr transition zone and Cu film that the first step is obtained be placed in NaOH concentration be 3~4mol/L and (NH4)2S2O8Concentration is to react 5~10min in the mixed liquor of 0.15~0.2mol/L, obtains having one through surface oxidation treatment The Cu (OH) of dimension nanometer construction2Thin-film material；
Third 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 material with one-dimensional nano structure；
4th step, using vacuum PVD technology, nanometer Al, which is coated to what third step obtained, has 1-dimention nano knot The CuO thin-film material of structure obtains CuO/Al nanometers of the core-shell structure thin-film materials containing energy.
2. preparation method according to claim 1, which is characterized in that in the first step, the substrate is silicon base, glass Substrate or ceramic bases, the vacuum PVD technology are magnetron sputtering technique or electron beam evaporation technique.
3. preparation method according to claim 1, which is characterized in that in the first step, the Cr transition region thickness is 20 ~30nm, the Cu film thickness are 500~1000nm.
4. preparation method according to claim 1, which is characterized in that in third step, heating rate is 3~5 DEG C/min, is protected Warm 4~6h of time.
5. preparation method according to claim 1, which is characterized in that in the 4th step, the vacuum PVD Technology is thermal evaporation techniques or magnetron sputtering technique.
6. preparation method according to claim 1, which is characterized in that in the 4th step, Al film thickness is 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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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
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