CN102263243B - Preparation methods for arrayed nickel silicon nanowire and nickel silicon-silicon core-shell nanowire - Google Patents
Preparation methods for arrayed nickel silicon nanowire and nickel silicon-silicon core-shell nanowire Download PDFInfo
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- 239000002070 nanowire Substances 0.000 title claims abstract description 60
- 239000011258 core-shell material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- PEUPIGGLJVUNEU-UHFFFAOYSA-N nickel silicon Chemical compound [Si].[Ni] PEUPIGGLJVUNEU-UHFFFAOYSA-N 0.000 title abstract 5
- MGTLYUZSHHQPEY-UHFFFAOYSA-N [Si][Ni][Si] Chemical compound [Si][Ni][Si] MGTLYUZSHHQPEY-UHFFFAOYSA-N 0.000 title abstract 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 47
- 239000010703 silicon Substances 0.000 claims abstract description 47
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000758 substrate Substances 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 238000004544 sputter deposition Methods 0.000 claims abstract description 22
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 78
- 229910052759 nickel Inorganic materials 0.000 claims description 29
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 21
- 239000006260 foam Substances 0.000 claims description 20
- 230000008021 deposition Effects 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000007747 plating Methods 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- 229910000077 silane Inorganic materials 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000011889 copper foil Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 6
- 238000004050 hot filament vapor deposition Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 229910005883 NiSi Inorganic materials 0.000 description 5
- 229910005881 NiSi 2 Inorganic materials 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses preparation methods for an arrayed nickel silicon nanowire and a nickel silicon-silicon core-shell nanowire. The preparation method for the nickel silicon-silicon core-shell nanowire comprises the following steps of: washing a metal substrate for a lithium ion battery anode basal body by using a hydrochloric acid and ethanol, and drying the washed metal substrate for later use; growing the arrayed nickel silicon nanowire on the surface of the washed metal substrate by using a hot wire chemical vapor deposition device; and further depositing a layer of thickness-controllable silicon on the surface of the obtained arrayed nickel silicon nanowire by using a radio frequency sputtering method to obtain the arrayed nickel silicon-silicon core-shell nanowire. The metal substrate and the arrayed nickel silicon nanowire grown on the metal substrate form a lithium ion battery anode. The preparation methods provided by the invention are simple and controllable; and the prepared nanowire materials can be used for the lithium ion battery anode and high performance can be obtained.
Description
Technical field
The invention belongs to material science, be specifically related to the preparation method for array nisiloy nano wire and the nisiloy-silicon core-shell nano line of lithium ion battery negative.
Background technology
Owing to having higher theoretical capacity, silicon is considered to the substitute of desirable lithium ion battery negative graphite-like material with carbon element, thereby satisfies the demand of lithium ion battery with high energy density.Yet due to change in volume huge in charge and discharge process, can cause the efflorescence of silicon electrode material, its capacity can sharply descend; In addition, the silicon electrode material is unstable properties under large charging and discharging currents, and these have all limited its commercial applications as lithium ion battery negative material.
Increasing work at present is devoted to improve silicon as the performance of lithium ion battery negative material, and wherein the electrode structure of array has unique advantage.The first, with electrically contacting of matrix, greatly improved the conductivity of electrode material, the second, the huge volumetric expansion in cyclic process of silicon electrode material can be effectively alleviated in the gap between the array structure, thereby significantly improves its cycle performance.Up to the present, the nickel of the carbon nano-tube-silicon heterostructure of the silicon nanowires of the nano-tube of array, array, array and array-silicon nucleocapsid structure all is used in the negative pole of lithium ion battery and has obtained the raising on the performance.Yet these methods also face some problems, and, reaction condition loaded down with trivial details such as the growth that can not realize highdensity array structure on large matrix, the course of reaction comparatively conductivity of harshness and electrode is relatively poor etc.Therefore, thus also need electrode structure is carried out the lithium electrical property that careful design further improves the silicium cathode material.
Summary of the invention
The invention provides the preparation method of a kind of array nisiloy nano wire for lithium ion battery negative and nisiloy-silicon core-shell nano line, realize the high-density growth of array nisiloy nano wire on large stretch of metal substrate by easy method, wherein nisiloy is mutually controlled, realize subsequently the preparation of high-quality array nisiloy-silicon core-shell nano line by easy method, wherein the ratio of nisiloy and silicon is controlled.
A kind of preparation method of array nisiloy nano wire comprises the following steps:
(1) will clean respectively with hydrochloric acid and ethanol for the metal substrate of lithium ion battery negative matrix, subsequent drying is standby; Described drying is that vacuumize or nitrogen dry up; Described hydrochloric acid and ethanol adopt general commercially available watery hydrochloric acid and alcohol product to get final product, and usually mass fraction are called watery hydrochloric acid lower than 37% hydrochloric acid;
(2) the metal substrate superficial growth array nisiloy nano wire that was cleaning through step (1) by the hot-wire chemical gas-phase deposition device, it is 10～1000sccm that silane flow rate is set, hydrogen flowing quantity is 10～1000sccm, cavity air pressure is 10～1000Pa, temperature is 200～1000 ℃, reaction time is 1～300min, obtains array nisiloy nano wire.
Described metal substrate and the array nano-material that is grown on metal substrate consist of lithium ion battery negative.
Described metal substrate is the foam copper of nickel foam, nickel foil, plating nickel on surface, the Copper Foil of plating nickel on surface or the titanium foil of plating nickel on surface.
In said method, by process parameter control, can obtain different crystalline phase (Ni
3Si
2, NiSi, Ni
2Si, NiSi
2Or Ni
31Si
12) the nisiloy nano wire, therefore, described array nisiloy nano wire is Ni
3Si
2Nano wire, NiSi nano wire, Ni
2Si nano wire, NiSi
2Nano wire or Ni
31Si
12Nano wire.
The preparation method of a kind of nisiloy-silicon core-shell nano line comprises the following steps:
(1) will clean respectively with hydrochloric acid and ethanol for the metal substrate of lithium ion battery negative matrix, subsequent drying is standby; Described drying is that vacuumize or nitrogen dry up; Described hydrochloric acid and ethanol adopt general commercially available watery hydrochloric acid and alcohol product to get final product, and usually mass fraction are called watery hydrochloric acid lower than 37% hydrochloric acid;
(2) the metal substrate superficial growth array nisiloy nano wire that was cleaning through step (1) by the hot-wire chemical gas-phase deposition device, it is 10～1000sccm that silane flow rate is set, hydrogen flowing quantity is 10～1000sccm, cavity air pressure is 10～1000Pa, temperature is 200～1000 ℃, reaction time is 1～300min, obtains array nisiloy nano wire;
(3) the controlled silicon of surface deposition a layer thickness of the array nisiloy nano wire that obtains in step (2) of the method by radio frequency sputtering, it is 20～500 ℃ that the silicon substrate temperature is set, argon flow amount is 10～1000sccm, cavity air pressure is 1～100Pa, sputtering power is 10～1000W, sputtering time is 1～300min, obtains array nisiloy-silicon core-shell nano line.
Described metal substrate and the array nano-material that is grown on metal substrate consist of lithium ion battery negative.
Described metal substrate is the foam copper of nickel foam, nickel foil, plating nickel on surface, the Copper Foil of plating nickel on surface or the titanium foil of plating nickel on surface.
In said method, by process parameter control, can obtain different crystalline phase (Ni
3Si
2, NiSi, Ni
2Si, NiSi
2Or Ni
31Si
12) the nisiloy nano wire, therefore, described array nisiloy nano wire is Ni
3Si
2Nano wire, NiSi nano wire, Ni
2Si nano wire, NiSi
2Nano wire or Ni
31Si
12Nano wire.
With respect to prior art, the present invention has following useful technique effect:
(1) the present invention has realized the high-density growth of array nisiloy nano wire on large stretch of metal substrate by easy method;
(2) the inventive method can be controlled obtains not homophase (Ni
3Si
2, NiSi, Ni
2Si, NiSi
2Or Ni
31Si
12) array nisiloy nano wire;
(3) the inventive method obtains array nisiloy-silicon core-shell nano line by easy method, and wherein the ratio of nisiloy and silicon is controlled;
(4) due to the electrode structural designs of uniqueness, the nisiloy nano wire that obtains in the present invention and nisiloy-silicon core-shell nano line all can be used for lithium ion battery negative and expects to obtain excellent performance.
Description of drawings
Fig. 1 is the stereoscan photograph of the array nisiloy nano wire that makes of embodiment 1.
Fig. 2 is the transmission electron microscope photo of the array nisiloy nano wire that makes of embodiment 1.
Fig. 3 is the X ray diffracting spectrum of the array nisiloy nano wire that makes of embodiment 1.
Fig. 4 is the transmission electron microscope photo of the array nisiloy that makes of embodiment 1-silicon core-shell nano line.
Fig. 5 is the cycle performance of lithium ion battery curve chart of the array nisiloy nano wire that makes of embodiment 1.
Fig. 6 is the cycle performance of lithium ion battery curve chart of the array nisiloy that makes of embodiment 1-silicon core-shell nano line.
Embodiment
Describe the present invention in detail below in conjunction with embodiment and accompanying drawing, but the present invention is not limited to this.
Embodiment 1:
(1) nickel foam is cleaned respectively with watery hydrochloric acid and alcohol, dry up standby with vacuumize or nitrogen subsequently; The mass percentage concentration of watery hydrochloric acid is 10%, and the concentration expressed in percentage by volume of alcohol is 98%;
(2) nickel foam that will clean is placed in the hot-wire chemical gas-phase deposition device, and it is 80sccm that silane flow rate is set, and hydrogen flowing quantity is 80sccm, cavity air pressure is 600Pa, temperature is 500 ℃, and the reaction time is 15min, obtains array nisiloy nano wire in the nickel foam superficial growth of cleaning;
(3) the controlled silicon of surface deposition a layer thickness of the array nisiloy nano wire that obtains in step (2) of the method by radio frequency sputtering, it is 20 ℃ that the silicon substrate temperature is set, argon flow amount is 30sccm, cavity air pressure is 3Pa, sputtering power is 80W, sputtering time is 60min, obtains array nisiloy-silicon core-shell nano line.
Fig. 1, Fig. 2 and Fig. 3 are respectively stereoscan photograph, transmission electron microscope photo and the X ray diffracting spectrums by the synthetic array nisiloy nano wire of the present embodiment.As seen, what obtain is the nano thread structure of array from Fig. 1～3, and wherein nanowire surface is smooth, and diameter is 30～50 nanometers, and main nisiloy crystalline phase is Ni
3Si
2Phase.
Fig. 4 is the transmission electron microscope photo of the synthetic array nisiloy of the present embodiment-silicon core-shell nano line.As can be seen from Figure 4, the thickness of the silicon layer of nisiloy nanowire surface is 10～20 nanometers.
Fig. 5 is that nickel foam consists of lithium ion battery negative gained cycle performance of battery curve with the array nisiloy nano wire that is grown on metal substrate.As can be seen from Figure 5, the capacity first of array nisiloy nano wire has reached the 800mAh/g left and right, and curve is steady, after 8 circulations, capacity stably maintains 450mAh/g, and efficient maintains more than 95%, has shown the cycle performance of battery more more excellent than commercialization material with carbon element.
Fig. 6 is above-mentioned nickel foam and is grown in array nisiloy on metal substrate-silicon core-shell nano line and consists of lithium ion battery negative gained cycle performance of battery curve, and current density is 4.2A/g.As can be seen from Figure 6, the specific capacity first of array nisiloy-silicon core-shell nano line has reached the 3400mAh/g left and right, and curve is steady, after 5 circulations, capacity stably maintains 1850mAh/g, and efficient maintains more than 95%, has shown very excellent cycle performance.
Embodiment 2:
(1) nickel foil is cleaned respectively with watery hydrochloric acid and alcohol, dry up standby with vacuumize or nitrogen subsequently; The mass percentage concentration of watery hydrochloric acid is 5%, and the concentration expressed in percentage by volume of alcohol is 90%;
(2) nickel foam that will clean is placed in the hot-wire chemical gas-phase deposition device, and it is 10sccm that silane flow rate is set, and hydrogen flowing quantity is 10sccm, cavity air pressure is 10Pa, temperature is 200 ℃, and the reaction time is 1min, obtains array nisiloy nano wire in the nickel foam superficial growth of cleaning;
(3) method by radio frequency sputtering is at the controlled silicon of surface deposition a layer thickness of array nisiloy nano wire, and it is 50 ℃ that the silicon substrate temperature is set, and argon flow amount is 10sccm, cavity air pressure is 1Pa, sputtering power is 10W, and sputtering time is 1min, obtains array nisiloy-silicon core-shell nano line.
Test result and example 1 are similar.
Embodiment 3:
(1) foam copper with plating nickel on surface cleans respectively with watery hydrochloric acid and alcohol, dries up standby with vacuumize or nitrogen subsequently; The mass percentage concentration of watery hydrochloric acid is 20%, and the concentration expressed in percentage by volume of alcohol is 80%;
(2) nickel foam that will clean is placed in the hot-wire chemical gas-phase deposition device, it is 100sccm that silane flow rate is set, hydrogen flowing quantity is 1000sccm, cavity air pressure is 1000Pa, temperature is 400 ℃, reaction time is 30min, obtains array nisiloy nano wire in the nickel foam superficial growth of cleaning;
(3) method by radio frequency sputtering is at the controlled silicon of surface deposition a layer thickness of array nisiloy nano wire, it is 100 ℃ that the silicon substrate temperature is set, argon flow amount is 100sccm, cavity air pressure is 10Pa, sputtering power is 50W, sputtering time is 30min, obtains array nisiloy-silicon core-shell nano line.
Test result and example 1 are similar.
Embodiment 4:
(1) Copper Foil with plating nickel on surface cleans respectively with watery hydrochloric acid and alcohol, dries up standby with vacuumize or nitrogen subsequently; The mass percentage concentration of watery hydrochloric acid is 30%, and the concentration expressed in percentage by volume of alcohol is 70%;
(2) nickel foam that will clean is placed in the hot-wire chemical gas-phase deposition device, it is 1000sccm that silane flow rate is set, hydrogen flowing quantity is 100sccm, cavity air pressure is 1000Pa, temperature is 800 ℃, reaction time is 150min, obtains array nisiloy nano wire in the nickel foam superficial growth of cleaning;
(3) method by radio frequency sputtering is at the controlled silicon of surface deposition a layer thickness of array nisiloy nano wire, it is 200 ℃ that the silicon substrate temperature is set, argon flow amount is 500sccm, cavity air pressure is 50Pa, sputtering power is 500W, sputtering time is 150min, obtains array nisiloy-silicon core-shell nano line.
Test result and example 1 are similar.
Embodiment 5:
(1) titanium foil with plating nickel on surface cleans respectively with watery hydrochloric acid and alcohol, dries up standby with vacuumize or nitrogen subsequently; The mass percentage concentration of watery hydrochloric acid is 37%, and the concentration expressed in percentage by volume of alcohol is 60%;
(2) nickel foam that will clean is placed in the hot-wire chemical gas-phase deposition device, it is 1000sccm that silane flow rate is set, hydrogen flowing quantity is 1000sccm, cavity air pressure is 1000Pa, temperature is 1000 ℃, reaction time is 300min, obtains array nisiloy nano wire in the nickel foam superficial growth of cleaning;
(3) method by radio frequency sputtering is at the controlled silicon of surface deposition a layer thickness of array nisiloy nano wire, it is 500 ℃ that the silicon substrate temperature is set, argon flow amount is 1000sccm, cavity air pressure is 100Pa, sputtering power is 1000W, sputtering time is 100min, obtains array nisiloy-silicon core-shell nano line.
Test result and example 1 are similar.
Claims (2)
1. the preparation method of nisiloy-silicon core-shell nano line, is characterized in that, comprises the following steps:
(1) will clean respectively with hydrochloric acid and ethanol for the metal substrate of lithium ion battery negative matrix, subsequent drying is standby;
(2) the metal substrate superficial growth array nisiloy nano wire that was cleaning through step (1) by the hot-wire chemical gas-phase deposition device, it is 80sccm that silane flow rate is set, hydrogen flowing quantity is 80sccm, cavity air pressure is 600Pa, temperature is 500 ° of C, reaction time is 15min, obtains array nisiloy nano wire;
(3) the controlled silicon of surface deposition a layer thickness of the array nisiloy nano wire that obtains in step (2) of the method by radio frequency sputtering, it is 20～500 ° of C that the silicon substrate temperature is set, argon flow amount is 10～1000sccm, cavity air pressure is 1～100Pa, sputtering power is 10～1000W, sputtering time is 1～300min, obtains array nisiloy-silicon core-shell nano line.
2. the preparation method of nisiloy as claimed in claim 1-silicon core-shell nano line, is characterized in that, described metal substrate is the foam copper of nickel foam, nickel foil, plating nickel on surface, the Copper Foil of plating nickel on surface or the titanium foil of plating nickel on surface.
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| CN103474632B (en) * | 2012-06-07 | 2016-08-03 | 中国科学院物理研究所 | A kind of negative material for lithium battery and its preparation method and application |
| CN105702942A (en) * | 2016-01-22 | 2016-06-22 | 奇瑞汽车股份有限公司 | Silicon-based negative electrode material and preparation method and application thereof |
| CN107799723A (en) * | 2016-08-30 | 2018-03-13 | 华为技术有限公司 | A kind of silicon substrate composite negative plate and preparation method thereof and lithium rechargeable battery |
| CN107482193B (en) * | 2017-08-02 | 2019-11-01 | 合肥国轩高科动力能源有限公司 | The silicon nanowires composite material and preparation method that a kind of nano nickel particles and tantnickel nano-substance are modified jointly |
| CN110010864A (en) * | 2019-03-21 | 2019-07-12 | 中国科学院半导体研究所 | Silicon-graphene battery negative electrode material and preparation method thereof, lithium battery |
| CN110993906A (en) * | 2019-11-21 | 2020-04-10 | 浙江大学 | Silicon-based lithium ion battery cathode material and preparation method thereof |
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| CN101202331A (en) * | 2007-11-19 | 2008-06-18 | 北京理工大学 | Method for preparation of insulating film material for batteries |
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| Title |
|---|
| Sa Zhou,et al.Si/TiSi2 Heteronanostructures as High-Capacity Anode Material for Li Ion Batteries.《NANO LETTERS》.2010,第10卷第860-863页. |
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