CN106935852A - Si doped gallium nitrides/metal negative electrode battery material and preparation method thereof, lithium battery - Google Patents
Si doped gallium nitrides/metal negative electrode battery material and preparation method thereof, lithium battery Download PDFInfo
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- CN106935852A CN106935852A CN201710248369.8A CN201710248369A CN106935852A CN 106935852 A CN106935852 A CN 106935852A CN 201710248369 A CN201710248369 A CN 201710248369A CN 106935852 A CN106935852 A CN 106935852A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
Abstract
The invention provides a kind of Si doped gallium nitrides/metal negative electrode battery material and preparation method thereof, lithium battery.Above-mentioned Si doped gallium nitrides/metal negative electrode battery material includes：Metal substrate；And the Si doped gallium nitride films above metal substrate are formed at, it is crystalline state and amorphous mixed state with loose and porous structure.The specific surface area of Si doped gallium nitrides/metal negative electrode battery material is larger, and Si3N4Tetrahedral structure and Si3N4The open three-dimensional frame structure of the stabilization of tetrahedron and Ga atomic buildings, the electro-chemical activity reduction problem caused by during Lithium-ion embeding is deviate from because of structure collapses is it also avoid while lithium ion transport efficiency is strengthened, cycle characteristics with lithium storage content higher and stabilization, for development high-performance lithium battery provides new selection.
Description
Technical field
The invention belongs to field of lithium ion battery and inorganic compound semiconductor Material Field, it is related to a kind of Si doping nitridation
Gallium/metal negative electrode battery material and preparation method thereof, lithium battery.
Background technology
At present, the new a collection of electronic product such as electric automobile, to high-energy-density, the requirement day of high power density energy battery
It is beneficial urgent.The negative material for being applied to lithium ion battery at present is essentially all carbon materials, such as electrographite, day
Right graphite, carbon fiber and thermal decomposed resins carbon etc..Carbon material is typically disordered structure, because its crystallinity is low, crystallite dimension is small, crystal face
Spacing is greatly and preferable with the compatibility of electrolyte, therefore is widely used in lithium battery, can not but first charge-discharge is still present
The problems such as capacity is higher, first charge-discharge efficiency is low, cycle performance is poor, at present for other new type lithium ions of exploration stage
Cell negative electrode material there is also first charge-discharge capacity it is low, without obvious charge and discharge platform voltage, cycle performance difference the problems such as.
The content of the invention
(1) technical problem to be solved
The invention provides a kind of Si doped gallium nitrides/metal negative electrode battery material and preparation method thereof, lithium battery, so that
Small part solves technical problem set forth above.
(2) technical scheme
According to an aspect of the invention, there is provided a kind of Si doped gallium nitrides/metal negative electrode battery material, including：Gold
Category substrate；And it is formed at the Si doped gallium nitride films above metal substrate；Wherein, the Si doped gallium nitrides film has
Loose and porous structure, is crystalline state and amorphous mixed state.
In one embodiment of this invention, the material selection Copper Foil of above-mentioned metal substrate, nickel foil, foam copper, nickel foam or
The Copper Foil of pre-deposition graphene buffer layers, nickel foil, foam copper and nickel foam.
In one embodiment of this invention, the thickness of above-mentioned Si doped gallium nitrides film is 10 μm；And/or the Si doping
The doping ratio of Si elements is 10% in gallium nitride film.
According to another aspect of the present invention, there is provided a kind of preparation of Si doped gallium nitrides/metal negative electrode battery material
Method, including：Using radio-frequency sputtering target, Si doped gallium nitride films are deposited on the metallic substrate, obtain Si doped gallium nitrides/
Metal negative electrode battery material.
In one embodiment of this invention, above-mentioned target includes：Gallium nitride disk is bonded at Si plates by conductive silver glue
Centre, wherein, the diameter of Si plates is equal to target rifle size, and the diameter of gallium nitride disk is attached in the corresponding groove bosom of sputter area
It is changed in nearly 1cm~3cm, constitutes the mixing sputtering target material of concentric structure.
In one embodiment of this invention, in above-mentioned preparation method the diameter of gallium nitride disk at 1.5 inches to 2.4 inches
Between, preferably 2 inches.
In another embodiment of the invention, above-mentioned target includes：Si plates are bonded at into gallium nitride by conductive silver glue to justify
The centre of piece, wherein, the diameter of gallium nitride is equal to target rifle size, and the diameter of Si plates is attached in the corresponding groove bosom of sputter area
It is changed in nearly 1cm~3cm, constitutes the mixing sputtering target material of concentric structure.
In one embodiment of this invention, the parameter of above-mentioned radio-frequency sputtering is：Underlayer temperature is 300 DEG C~500 DEG C；Sputtering
Power is 100W；Vacuum is better than 1.5*10-7Torr；Background gas pressure is 1Pa；Nitrogen flow is 10ppm；Target rotation speed is
30r/min；Sedimentation time is 1hour.
According to a further aspect of the invention, there is provided a kind of lithium battery, including above-mentioned Si doped gallium nitrides/metal negative electrode
Battery material.
In one embodiment of this invention, above-mentioned lithium battery is CR2025 type button cells, and its initial charge capacity is：
290mAh/g, discharge capacity is：350mAh/g, between 0.2V to 0.85V, discharge platform is in 0.65V to 0.02V for charging platform
Between.
(3) beneficial effect
From above-mentioned technical proposal as can be seen that the present invention provide Si doped gallium nitrides/metal negative electrode battery material and its
Preparation method, lithium battery, have the advantages that：The above-mentioned material for preparing has loose and porous structure, be crystalline state with
Amorphous mixed state, its specific surface area is larger, and Si3N4Tetrahedral structure and Si3N4Tetrahedron is steady with Ga atomic buildings
Fixed open three-dimensional frame structure, it also avoid deviating from process in Lithium-ion embeding while lithium ion transport efficiency is strengthened
It is middle because caused by structure collapses electro-chemical activity reduction problem, with lithium storage content higher and stabilization cycle characteristics, be hair
Exhibition high performance lithium ion battery provides new selection.
Brief description of the drawings
Fig. 1 is the space structure schematic diagram of the gallium nitride of hexagonal wurtzite structure.
Fig. 2 is the preparation method flow chart according to embodiment of the present invention Si doped gallium nitrides/metal negative electrode battery material.
Fig. 3 (a) is the signal according to embodiment of the present invention sputtering growth Si doped gallium nitrides/metal negative electrode battery material
Figure；Fig. 3 (b) is the schematic cross-section cut along radius according to embodiment of the present invention self assembly sputtering target material.
Fig. 4 is the EDX figures and corresponding composition row of the Si doped gallium nitride materials prepared according to the embodiment of the present invention
Table.
Fig. 5 (a) and Fig. 5 (b) are respectively the Si doped gallium nitrides/metal negative electrode electricity for characterizing the embodiment of the present invention and preparing
The front SEM figures and section SEM figures of pond material.
Fig. 6 (a) and Fig. 6 (b) are respectively the Si doped gallium nitrides/metal negative electrode electricity for characterizing the embodiment of the present invention and preparing
Transmission electron microscope TEM and high-resolution-ration transmission electric-lens the HRTEM figure of pond material；Fig. 6 (c) and Fig. 6 (d) is SEAD SAED
Figure.
Fig. 7 (a), Fig. 7 (b) and Fig. 7 (c) are respectively Si doped gallium nitrides/metal negative electrode battery according to embodiments of the present invention
The first time of the lithium ion battery of material assembling, second and third time charging and discharging curve figure.
Specific embodiment
Gallium nitride-based material has the chemical property of excellent photoelectric properties and stabilization, is the research heat of current Material Field
One of point.Gallium nitride crystal structure includes buergerite, zincblende and salt mine, and wherein hexagonal wurtzite structure is Stable structure,
Cubic sphalerite structure is metastable structure, and a cube salt mine structure only exists in the case of extreme high pressure, and common is nitrogen
Change the hexagonal wurtzite structure of gallium crystal.
The basic parameter of gallium nitride is given in table 1, Fig. 1 is the space of the gallium nitride of hexagonal wurtzite structure
Structural representation.From table 1 it follows that the gallium nitride of hexagonal wurtzite structure has direct band gap wider,
Its band-gap energy is 3.39eV during 300K, and its lattice parameter is respectivelyCome with reference to Fig. 1
See, wherein Ga atoms are in the summit of hexagonal structure and the upper and lower center of area, make hexagonal closs packing, and N atoms are filled in the four sides of half
In body space, Ga atoms are connected with N atoms with covalent bond, and ligancy is 4, and pairing polyhedron is that a tripartite singly bores, parallel to z
More than the bond distance of other 3 Ga-N keys, singly cone is connected all of tripartite the Ga-N bond distance of axle in three dimensions with corner-sharing top, they
Ga-N keys long parallel to z-axis and point to it is identical, it is overall that layer structure is presented.
Micro Si elements are selectively mixed, the electrochemical properties of gallium nitride material can be effectively improved, it is former using Si
Son combines to form Si with N atoms3N4The covalent bond tetrahedron and Si of structure3N4Tetrahedron is with Ga atoms by corner-sharing or common
While connecting into the structural advantages such as the three-dimensional frame structure of opening, it is innovatively applied to the negative material of lithium ion battery,
In addition, gallium nitride material also has the chemical property of stabilization, strong acid environment can be resisted, comprehensively utilize its space structure and stabilization
Chemical property, as lithium cell cathode material application, as improving the battery capacity that cathode of lithium battery is present at this stage
A new approaches low, the problems such as cycle performance is poor.
The gallium nitride basic parameter of table 1
According to an aspect of the invention, there is provided a kind of Si doped gallium nitrides/metal negative electrode battery material and its preparation
Method, lithium battery, the Li in the numerous alloys formed during one side Si insertion Li4.4Si, its theoretical capacity is up to 4200mAh/g,
The capacity of lithium ion battery can be effectively improved, on the other hand, by building Si3N4Tetrahedral structure and Si3N4Tetrahedron and Ga
The open three-dimensional frame structure of atomic building stabilization, it also avoid in lithium ion while lithium ion transport efficiency is strengthened
Because of electro-chemical activity reduction problem caused by structure collapses, cycle life and cyclicity to improving material during embedded abjection
Can be extremely beneficial.
To make the object, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, and reference
Accompanying drawing, is described in further detail to the present invention.
In one exemplary embodiment of the invention, there is provided a kind of Si doped gallium nitrides/metal negative electrode battery material.
Si doped gallium nitrides/metal negative electrode battery material includes：Metal substrate；And it is formed at the Si doping nitridations above metal substrate
Gallium film, is crystalline state and amorphous mixed state with loose and porous structure.
The part to above-mentioned Si doped gallium nitrides/metal negative electrode battery material is described in detail below：
Wherein, metal substrate includes Copper Foil, the nickel of Copper Foil, nickel foil, foam copper, nickel foam or pre-deposition graphene buffer layers
Paper tinsel, foam copper, nickel foam；
In the present embodiment, the thickness of Si doped gallium nitride films is about 10 μm；Metal substrate selects Copper Foil；Si doping nitridations
The doping ratio of Si elements is about 10% in gallium film.
Fig. 2 is the preparation method flow chart according to embodiment of the present invention Si doped gallium nitrides/metal negative electrode battery material；Figure
3 (a) is the schematic diagram according to embodiment of the present invention sputtering growth Si doped gallium nitrides/metal negative electrode battery material；Fig. 3 (b) is
The schematic cross-section that self assembly sputtering target material according to embodiments of the present invention cuts along radius.
Reference picture 2 and Fig. 3, the method for preparing above-mentioned Si doped gallium nitrides/metal negative electrode battery material, including：
Step S202：Prepare self assembly sputtering target material；
By conductive silver glue be bonded in the middle of Si plates gallium nitride disk with shown in Fig. 3 (b) by reference picture 3 (a), and composition is same
The heart justifies the mixing sputtering target material of structure；
Wherein, the diameter of gallium nitride disk changes between 1.5 inches to 2.4 inches, by gallium nitride and Si targets
The doping ratio of the silicon that the change regulation and control of relative area ratio are sputtered out, the present embodiment is justified from a diameter of 2 inches of gallium nitride
Piece；A diameter of 3 inches of Si plates, cover all target rifle；
As shown in Fig. 3 (b), one shape of sputter area correspondence such as groove checked the number, wherein most deep place is our meat
The visible target as sputter depth of eye, designs less concentric radius of circle as follows：In the corresponding groove of sputter area most
1cm~3cm near depths, design is finely adjusted to the less disk size of area；
It should be noted that the present embodiment hits, the full-size of rifle is 3 inches, therefore silicon plate chooses 3 inches, for other
Magnetron sputtering apparatus, can correspondingly design the size of silicon plate and the face of corresponding gallium nitride disk according to the size of actual target rifle
Product and diameter；In addition, the present embodiment is so that the less gallium nitride disk of area is affixed on the larger Si plates of area as an example, in practical operation
The less Si disks of area can also be affixed on the larger gallium nitride disk of area, form concentric structure, face is designed accordingly
Product and diameter, regulate and control suitable doping ratio.
Step S204：Self assembly sputtering target material and metal substrate are placed in sputtering chamber, are vacuumized, reach certain vacuum degree
After heat substrate；
Wherein, by the metal substrate of cleaning, drying, it is clipped on the substrate pallet of sputtering chamber with spring clip, adjusts target spacing
7cm；
Wherein, when the vacuum of cavity is better than 1*10-6After Torr, substrate is heated；
It should be noted that for different magnetron sputtering systems, the vacuum level requirements before being heated are different, can basis
Actual conditions are adjusted；
Step S206：Using radio-frequency sputtering, Si doped gallium nitride films are deposited on the metallic substrate, obtain Si doping nitridations
Gallium/metal negative electrode battery material；
Wherein, vacuum is better than 1.5*10-7Torr, the present embodiment vacuum is 1*10-7Torr, proceeds by sputtering, penetrates
The parameter setting of RF sputtering is as follows：Background gas pressure 1Pa, nitrogen flow 10ppm, sputtering power 100W, preheat 15min, and target turns
Dynamic speed 30r/min, sedimentation time 1hour, then obtain Si doped gallium nitrides/metal negative electrode battery material.
So far, the preparation of Si doped gallium nitrides/metal negative electrode battery material shown in the embodiment of the present invention is completed.
Fig. 4 is the EDX figures and corresponding composition row of the Si doped gallium nitride materials prepared according to the embodiment of the present invention
Table；Fig. 5 (a) and Fig. 5 (b) are respectively and characterize Si doped gallium nitrides/metal negative electrode battery material that the embodiment of the present invention is prepared
The front SEM figures and section SEM figures of material；Fig. 6 (a) and Fig. 6 (b) are respectively and characterize the Si doping that the embodiment of the present invention is prepared
Transmission electron microscope TEM and high-resolution-ration transmission electric-lens the HRTEM figure of gallium nitride/metal negative electrode battery material；Fig. 6 (c) and Fig. 6 (d) are
SEAD SAED schemes.
As shown in figure 4, EDX analysis display the present embodiment prepares the Si element dopings ratio in Si doped gallium nitride materials
Example about 10%；As shown in Fig. 5 (a), the present embodiment prepares that Si doped gallium nitride material surfaces are loose, and little particle is in spherical
Reunite；As shown in Fig. 5 (b), sample in cross section thickness is about 10 μm, and inside is in loose porous shape, consistent with sample surfaces feature；Ginseng
According to Fig. 6 (a) and Fig. 6 (b), the interplanar distance of Si doped gallium nitride materials is 0.22nm, and spacing occurs compared with standard GaN crystal faces
Change, illustrates that the Si of doping generates influence to the structure of GaN；Further look at SEAD SAED figures, such as Fig. 6 (c)
With Fig. 6 (d) Suo Shi, sample is presented the state that crystalline state mixes with amorphous state.
Fig. 7 (a), Fig. 7 (b) and Fig. 7 (c) are respectively Si doped gallium nitrides/metal negative electrode battery according to embodiments of the present invention
The first time of the lithium ion battery of material assembling, second and third time charging and discharging curve figure.The present embodiment Si is adulterated and is nitrogenized
Gallium/metal negative electrode battery material as lithium ion battery negative material, be that, to electrode, Celgard films are from metal lithium sheet
Barrier film, volume ratio be 1: 1 LiPF6 (1mol/L)/EC+DEC solution for electrolyte is assembled into CR2025 type button cells, and make
Constant current charge-discharge test is carried out with CT2001A battery test systems, test voltage is 3V~0.02V, its electrochemical properties such as Fig. 7
It is shown.As seen from the figure：Si doped gallium nitrides/metal negative electrode battery material its initial charge capacity prepared by above-described embodiment is：
290mAh/g, discharge capacity is：350mAh/g, mainly between 0.2V to 0.85V, discharge platform mainly exists charging platform
Between 0.65V to 0.02V, first charge-discharge efficiency is effectively increased；And 3 times charging and discharging curve almost overlaps, and explanation has
Preferable cycle performance, effectively improves that the irreversible capacity produced after lithium ion battery first charge-discharge is high, electro-chemical activity
The problem of reduction.
In sum, Si doped gallium nitrides/metal negative electrode battery material that the present invention is provided adulterates by using appropriate Si
Gallium nitride material, obtains the loose and porous structure of state that crystalline state mixes with amorphous state, increases the specific surface area of material, with
During making lithium ion battery negative, the alloy that Li forms high power capacity is embedded in by Si, improves the capacity of lithium battery, and
Due to the Si of the stabilization that material has3N4Tetrahedron connects into the three-dimensional framework of opening with Ga atoms by corner-sharing or common side
Structure, it is to avoid because of the problem of electro-chemical activity reduction caused by structure collapses during Lithium-ion embeding abjection, improving lithium
While ion battery capacity, its electro-chemical activity is also enhanced, with good cycle performance, comprising Si doped gallium nitrides/
The lithium battery of metal negative electrode battery material has charge and discharge platform and charge/discharge capacity higher, and with good cyclicity
Energy.
Unless there are specified, all being used in specification and claim represents content, reaction condition of composition etc.
Numeral, it is thus understood that be in all situations to be subject to term " about " to be modified.Therefore, otherwise anticipated unless be referred to as phase, this theory
Numerical parameter in bright book and appended claims is approximation, can be according to the required characteristic as obtained by present disclosure
Change.Certainly, according to actual needs, Si doped gallium nitrides/metal negative electrode battery material that the present invention is provided is also comprising others
Conventional preparation method and step, because the innovation with invention is unrelated, here is omitted.
Particular embodiments described above, has been carried out further in detail to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail bright, should be understood that the specific embodiment that the foregoing is only invention, be not intended to limit the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc. should be included in protection of the invention
Within the scope of.
Claims (10)
1. a kind of Si doped gallium nitrides/metal negative electrode battery material, including：
Metal substrate；And
It is formed at the Si doped gallium nitride films above metal substrate；
Wherein, the Si doped gallium nitrides film has loose and porous structure, is crystalline state and amorphous mixed state.
2. negative battery material according to claim 1, the material selection Copper Foil of the metal substrate, nickel foil, foam copper,
The Copper Foil of nickel foam or pre-deposition graphene buffer layers, nickel foil, foam copper and nickel foam.
3. negative battery material according to claim 1, the thickness of the Si doped gallium nitrides film is 10 μm；And/or
The doping ratio of Si elements is 10% in the Si doped gallium nitrides film.
4. a kind of preparation method of the doped gallium nitrides of Si according to claim 1/metal negative electrode battery material, including：
Using radio-frequency sputtering target, Si doped gallium nitride films are deposited on the metallic substrate, obtain Si doped gallium nitrides/metal and bear
Pole battery material.
5. preparation method according to claim 4, the target includes：Gallium nitride disk is bonded at by conductive silver glue
In the middle of Si plates, wherein, the diameter of Si plates is equal to target rifle size, and the diameter of gallium nitride disk is most deep in the corresponding groove of sputter area
It is changed in 1cm~3cm near place, constitutes the mixing sputtering target material of concentric structure.
6. preparation method according to claim 5, the diameter of the gallium nitride disk between 1.5 inches to 2.4 inches,
It is preferred that 2 inches.
7. preparation method according to claim 4, the target includes：Si plates are bonded at gallium nitride by conductive silver glue
The centre of disk, wherein, the diameter of gallium nitride is equal to target rifle size, and the diameter of Si plates is in the corresponding groove bosom of sputter area
It is changed in neighbouring 1cm~3cm, constitutes the mixing sputtering target material of concentric structure.
8. preparation method according to claim 4, the parameter of the radio-frequency sputtering is：
Underlayer temperature is 300 DEG C~500 DEG C；
Sputtering power is 100W；
Vacuum is better than 1.5*10-7Torr；
Background gas pressure is 1Pa；
Nitrogen flow is 10ppm；
Target rotation speed is 30r/min；
Sedimentation time is 1hour.
9. a kind of lithium battery, including the Si doped gallium nitrides/metal negative electrode battery any one of the claims 1 to 3
Material.
10. lithium battery according to claim 9, the lithium battery is CR2025 type button cells, its initial charge capacity
For：290mAh/g, discharge capacity is：350mAh/g, charging platform between 0.2V to 0.85V, discharge platform in 0.65V extremely
Between 0.02V.
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| CN110073535A (en) * | 2019-02-21 | 2019-07-30 | 京东方科技集团股份有限公司 | Lithium ion battery and preparation method thereof |
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| CN107576541B (en) * | 2017-07-22 | 2020-05-12 | 复旦大学 | Method for preparing in-situ power-up indium arsenide/gallium antimonide superlattice semiconductor sample of transmission electron microscope |
| CN110073535A (en) * | 2019-02-21 | 2019-07-30 | 京东方科技集团股份有限公司 | Lithium ion battery and preparation method thereof |
| CN109994323A (en) * | 2019-03-29 | 2019-07-09 | 中国科学院半导体研究所 | Amorphous gallium nitride/Graphene electrodes material, preparation method and supercapacitor |
| CN110336028A (en) * | 2019-04-30 | 2019-10-15 | 中国科学院半导体研究所 | Cell negative electrode material and preparation method thereof, lithium battery |
| CN114914410A (en) * | 2022-04-12 | 2022-08-16 | 广州大学 | Interface interaction for constructing built-in electric field for high-performance lithium ion storage |
| CN114914410B (en) * | 2022-04-12 | 2024-04-12 | 广州大学 | Interface interaction construction of built-in electric field for high performance lithium ion storage |
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