CN106935852B - Si doped gallium nitride/metal negative electrode battery material and preparation method thereof, lithium battery - Google Patents
Si doped gallium nitride/metal negative electrode battery material and preparation method thereof, lithium battery Download PDFInfo
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- 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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Abstract
The present invention provides a kind of Si doped gallium nitride/metal negative electrode battery materials and preparation method thereof, lithium battery.Above-mentioned Si doped gallium nitride/metal negative electrode battery material includes: metal substrate；And it is formed in the Si doped gallium nitride film above metal substrate, there is loose and porous structure, be crystalline state and amorphous mixed state.Si doped gallium nitride/metal negative electrode battery material specific surface area is larger, and Si3N4Tetrahedral structure and Si3N4The stable open three-dimensional frame structure of tetrahedron and Ga atomic building, also avoided while enhancing lithium ion transport efficiency lithium ion be embedded in deviate from during because of structure collapses caused by electro-chemical activity reduce problem, lithium storage content with higher and stable cycle characteristics provide new selection to develop high-performance lithium battery.
Description
Technical field
The invention belongs to field of lithium ion battery and inorganic compound semiconductor Material Field, are related to a kind of Si doping nitridation
Gallium/metal negative electrode battery material and preparation method thereof, lithium battery.
Background technique
Currently, the new a collection of electronic product such as electric car, to the requirement day of high-energy density, high power density energy battery
It is beneficial urgent.Being applied to the negative electrode material of 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 usually disordered structure, because its crystallinity is low, crystallite dimension is small, crystal face
Spacing is big and preferable with the compatibility of electrolyte, therefore is widely used in lithium battery, but can not there are still first charge-discharge
Inverse the problems such as capacity is higher, first charge-discharge efficiency is low, poor circulation, 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 apparent charge and discharge platform voltage, poor circulation the problems such as.
Summary of the invention
(1) technical problems to be solved
The present invention provides a kind of Si doped gallium nitride/metal negative electrode battery materials and preparation method thereof, lithium battery, so that
Small part solves technical problem set forth above.
(2) technical solution
According to an aspect of the invention, there is provided a kind of Si doped gallium nitride/metal negative electrode battery material, comprising: gold
Belong to substrate；And it is formed in the Si doped gallium nitride film above metal substrate；Wherein, the Si doped gallium nitride film has
Loose and porous structure is crystalline state and amorphous mixed state.
In one embodiment of this invention, one or more of following material of the material selection of above-mentioned metal substrate: copper
Foil, nickel foil, foam copper, nickel foam, the copper foil of pre-deposition graphene buffer layers, the nickel foil of pre-deposition graphene buffer layers, preliminary sedimentation
The foam copper of product graphene buffer layers or the nickel foam of pre-deposition graphene buffer layers.
In one embodiment of this invention, above-mentioned Si doped gallium nitride film with a thickness of 10 μm；And/or the Si doping
The doping ratio of Si element is 10% in gallium nitride film.
According to another aspect of the present invention, a kind of preparation of Si doped gallium nitride/metal negative electrode battery material is provided
Method, comprising: radio-frequency sputtering target is utilized, on the metallic substrate deposition Si doped gallium nitride film, acquisition Si doped gallium nitride/
Metal negative electrode battery material.
In one embodiment of this invention, above-mentioned target includes: that gallium nitride disk is sticked to Si plate by conductive silver glue
It is intermediate, wherein the diameter of Si plate 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, the mixing sputtering target material that group is concentrically arranged.
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: that Si plate is sticked to gallium nitride circle by conductive silver glue
The centre of piece, wherein the diameter of gallium nitride is equal to target rifle size, and the diameter of Si plate is attached in the corresponding groove bosom of sputter area
It is changed in nearly 1cm~3cm, the mixing sputtering target material that group is concentrically arranged.
In one embodiment of this invention, the parameter of above-mentioned radio-frequency sputtering are as follows: underlayer temperature is 300 DEG C~500 DEG C；Sputtering
Power is 100W；Vacuum degree is better than 1.5*10-7Torr；Background gas pressure is 1Pa；Nitrogen gas concn is 10ppm；Target rotation rate is
30r/min；Sedimentation time is 1hour.
According to a further aspect of the invention, a kind of lithium battery, including above-mentioned Si doped gallium nitride/metal negative electrode are provided
Battery material.
In one embodiment of this invention, above-mentioned lithium battery is CR2025 type button cell, initial charge capacity are as follows:
290mAh/g, discharge capacity are as follows: 350mAh/g, charging platform is in 0.2V between 0.85V, and discharge platform is in 0.65V to 0.02V
Between.
(3) beneficial effect
It can be seen from the above technical proposal that Si doped gallium nitride/metal negative electrode battery material provided by the invention 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, specific surface area is larger, and Si3N4 tetrahedral structure and Si3N4Tetrahedron is steady with Ga atomic building
Fixed open three-dimensional frame structure also avoids being embedded in abjection process in lithium ion while enhancing lithium ion transport efficiency
It is middle because electro-chemical activity caused by structure collapses reduces problem, lithium storage content with higher and stable cycle characteristics, for hair
Exhibition high performance lithium ion battery provides new selection.
Detailed description of the invention
Fig. 1 is the space structure schematic diagram of the gallium nitride of hexagonal wurtzite structure.
Fig. 2 is according to Si of embodiment of the present invention doped gallium nitride/metal negative electrode battery material preparation method flow chart.
Fig. 3 (a) is that growth Si doped gallium nitride/metal negative electrode battery material signal is sputtered according to the embodiment of the present invention
Figure；Fig. 3 (b) is the schematic cross-section cut according to self assembly of embodiment of the present invention sputtering target material along radius.
Fig. 4 is that the EDX figure of the Si doped gallium nitride material prepared according to the embodiment of the present invention and corresponding composition arrange
Table.
Fig. 5 (a) and Fig. 5 (b) is respectively the Si doped gallium nitride/metal negative electrode electricity for characterizing the embodiment of the present invention and preparing
The positive SEM figure and section SEM figure of pond material.
Fig. 6 (a) and Fig. 6 (b) is respectively the Si doped gallium nitride/metal negative electrode electricity for characterizing the embodiment of the present invention and preparing
The transmission electron microscope TEM and high-resolution-ration transmission electric-lens HRTEM of pond material scheme；Fig. 6 (c) and Fig. 6 (d) is selective electron diffraction SAED
Figure.
Fig. 7 (a), Fig. 7 (b) and Fig. 7 (c) are respectively Si doped gallium nitride/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 excellent photoelectric properties and stable chemical property, 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 extreme high pressure, common for 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 schematic diagram.From table 1 it follows that the gallium nitride of hexagonal wurtzite structure has wider direct band gap,
Its band-gap energy is 3.39eV when 300K, and lattice constant is respectivelyCome in conjunction with Fig. 1
See, wherein Ga atom be in hexagonal structure vertex and the upper and lower center of area, make hexagonal closs packing, N atom is filled in the four sides of half
In body space, Ga atom is connected with N atom with covalent bond, ligancy 4, and pairing polyhedron is that a tripartite singly bores, and is parallel to z
The Ga-N bond distance of axis is greater than the bond distance of other 3 Ga-N keys, and singly cone is connected in three-dimensional space with corner-sharing top all tripartites, they
Long Ga-N key be parallel to z-axis and be directed toward it is identical, it is whole that layer structure is presented.
Micro Si element is selectively mixed, the electrochemical properties of gallium nitride material can be effectively improved, utilizes Si original
Son forms Si in conjunction with N atom3N4The covalent bond tetrahedron and Si of structure3N4Tetrahedron and Ga atom are by corner-sharing or altogether
While connecting into the structural advantages such as open three-dimensional frame structure, it is innovatively applied to the negative electrode material of lithium ion battery,
In addition, gallium nitride material also has stable chemical property, strong acid environment can be resisted, comprehensively utilizes its space structure and stabilization
Chemical property become improvement battery capacity existing for cathode of lithium battery at this stage as lithium cell cathode material application
The new approaches of the problems such as low, poor circulation.
1 gallium nitride basic parameter of table
According to an aspect of the invention, there is provided a kind of Si doped gallium nitride/metal negative electrode battery material and its preparation
Method, lithium battery, one side Si are embedded in the Li in the numerous alloys formed when Li4.4Si, theoretical capacity are up to 4200mAh/g,
It can effectively improve the capacity of lithium ion battery, on the other hand, by constructing Si3N4Tetrahedral structure and Si3N4Tetrahedron and Ga
The stable open three-dimensional frame structure of atomic building, also avoids while enhancing lithium ion transport efficiency in lithium ion
Because electro-chemical activity caused by structure collapses reduces problem during insertion abjection, to the cycle life and cyclicity for improving material
It can be extremely beneficial.
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, invention is further described in detail.
In one exemplary embodiment of the invention, a kind of Si doped gallium nitride/metal negative electrode battery material is provided.
Si doped gallium nitride/metal negative electrode battery material includes: metal substrate；And it is formed in the Si doping nitridation above metal substrate
Gallium film has loose and porous structure, is crystalline state and amorphous mixed state.
The component part of above-mentioned Si doped gallium nitride/metal negative electrode battery material is described in detail below:
Wherein, the material of metal substrate includes one or more of following material: copper foil, nickel foil, foam copper, nickel foam
Or the copper foil of pre-deposition graphene buffer layers, nickel foil, foam copper, nickel foam；
In the present embodiment, the thickness of Si doped gallium nitride film is about 10 μm；Metal substrate selects copper foil；Si doping nitridation
The doping ratio of Si element is about 10% in gallium film.
Fig. 2 is according to Si of embodiment of the present invention doped gallium nitride/metal negative electrode battery material preparation method flow chart；Figure
3 (a) grow Si doped gallium nitride/metal negative electrode battery material schematic diagram to sputter according to the embodiment of the present invention；Fig. 3 (b) is
The schematic cross-section that self assembly sputtering target material according to embodiments of the present invention is cut along radius.
Referring to Fig. 2 and Fig. 3, the method for preparing above-mentioned Si doped gallium nitride/metal negative electrode battery material, comprising:
Step S202: prepare self assembly sputtering target material；
Referring to shown in Fig. 3 (a) and Fig. 3 (b), gallium nitride disk is sticked among Si plate by conductive silver glue, composition is same
The mixing sputtering target material of heart circle structure；
Wherein, the diameter of gallium nitride disk changes between 1.5 inches to 2.4 inches, passes through gallium nitride and Si target
The doping ratio for the silicon that the variation regulation of relative area ratio sputters out, the present embodiment select the gallium nitride circle that diameter is 2 inches
Piece；The diameter of Si plate is 3 inches, covers all target rifle；
As shown in Fig. 3 (b), the corresponding shape of the sputter area such as groove checked the number, wherein most deep place is our meat
The visible target as sputter depth of eye, designs lesser concentric radius of circle as follows: the corresponding groove of sputter area most
1cm~3cm near depths, is finely adjusted design to the lesser disk size of area；
It should be noted that the full-size of target rifle is 3 inches in the present embodiment, 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 practical target rifle
Long-pending and diameter；In addition, the present embodiment is so that the lesser gallium nitride disk of area is affixed on the biggish Si plate of area as an example, in practical operation
The lesser Si disk of area can also be affixed on to the biggish gallium nitride disk of area, concentric structure is formed, design face accordingly
Long-pending and diameter, regulates and controls suitable doping ratio.
Step S204: self assembly sputtering target material and metal substrate being placed in sputtering chamber, vacuumized, and reach certain vacuum degree
After heat substrate；
Wherein, it by the metal substrate of cleaning, drying, is clipped on the substrate pallet of sputtering chamber with spring clip, adjusts target spacing
7cm；
Wherein, when the vacuum degree of cavity is better than 1*10-6After Torr, substrate is heated；
It should be noted that the vacuum level requirements before being heated are different for different magnetron sputtering systems, it can basis
Actual conditions are adjusted；
Step S206: utilizing radio-frequency sputtering, deposits Si doped gallium nitride film on the metallic substrate, obtains Si doping nitridation
Gallium/metal negative electrode battery material；
Wherein, vacuum degree is better than 1.5*10-7Torr, the present embodiment vacuum degree are 1*10-7Torr starts to be sputtered, penetrate
The parameter setting of RF sputtering is as follows: background gas pressure 1Pa, nitrogen gas concn 10ppm, sputtering power 100W, preheats 15min, and target turns
Dynamic rate 30r/min, sedimentation time 1hour, then obtain Si doped gallium nitride/metal negative electrode battery material.
So far, Si doped gallium nitride/metal negative electrode battery material preparation shown in the embodiment of the present invention is completed.
Fig. 4 is that the EDX figure of the Si doped gallium nitride material prepared according to the embodiment of the present invention and corresponding composition arrange
Table；Fig. 5 (a) and Fig. 5 (b) is respectively the Si doped gallium nitride/metal negative electrode battery material for characterizing the embodiment of the present invention and preparing
The positive SEM figure and section SEM figure of material；Fig. 6 (a) and Fig. 6 (b) is respectively the Si doping for characterizing the embodiment of the present invention and preparing
Gallium nitride/metal negative electrode battery material transmission electron microscope TEM and high-resolution-ration transmission electric-lens HRTEM figure；Fig. 6 (c) and Fig. 6 (d) are
Selective electron diffraction SAED figure.
As shown in figure 4, EDX is analysis shows that the present embodiment prepares the Si element doping ratio in Si doped gallium nitride material
Example about 10%；As shown in Fig. 5 (a), it is loose that the present embodiment prepares Si doped gallium nitride material surface, 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 material is 0.22nm, and spacing occurs compared with standard GaN crystal face
Variation illustrates that the Si of doping produces influence to the structure of GaN；Selective electron diffraction SAED figure is further looked at, such as Fig. 6 (c)
With shown in Fig. 6 (d), the state that crystalline state is mixed with amorphous state is presented in sample.
Fig. 7 (a), Fig. 7 (b) and Fig. 7 (c) are respectively Si doped gallium nitride/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/negative electrode material of the metal negative electrode battery material as lithium ion battery, selecting metal lithium sheet is to electrode, and Celgard film is
Diaphragm, LiPF6 (1mol/L)/EC+DEC solution of volume ratio 1: 1 are that electrolyte is assembled into CR2025 type button cell, and makes
Constant current charge-discharge test is carried out with CT2001A battery test system, test voltage is 3V~0.02V, electrochemical properties such as Fig. 7
It is shown.As seen from the figure: its initial charge capacity of Si doped gallium nitride/metal negative electrode battery material prepared in the above embodiments are as follows:
290mAh/g, discharge capacity are as follows: 350mAh/g, mainly in 0.2V between 0.85V, discharge platform mainly exists charging platform
0.65V effectively increases first charge-discharge efficiency between 0.02V；And 3 times charging and discharging curve is almost overlapped, and explanation has
Preferable cycle performance effectively improves irreversible capacity height, the electro-chemical activity generated after lithium ion battery first charge-discharge
The problem of reduction.
It is adulterated in conclusion Si doped gallium nitride/metal negative electrode battery material provided by the invention passes through using appropriate Si
Gallium nitride material obtains the loose and porous structure of state that crystalline state is mixed with amorphous state, increases the specific surface area of material, with
During making negative electrode of lithium ion battery, the alloy that Li forms high capacity is embedded in by Si, improves the capacity of lithium battery, and
The stable Si having due to material3N4Side connects into open three-dimensional framework by corner-sharing or altogether for tetrahedron and Ga atom
Structure avoids the problem of being reduced during lithium ion insertion abjection because of electro-chemical activity caused by structure collapses, is improving lithium
While ion battery capacity, its electro-chemical activity is also enhanced, there is good cycle performance, comprising Si doped gallium nitride/
The lithium battery of metal negative electrode battery material charge and discharge platform with higher and charge/discharge capacity, and there is good cyclicity
Energy.
It is all to be used in specification and claim the content for indicating composition, reaction condition etc. unless there are specified
Number, it is thus understood that be to be modified by the term of " about " in all situations.Therefore, unless being known as mutually otherwise anticipating, this theory
Numerical parameter in bright book and appended claims is approximation, can be according to the resulting required characteristic of content through the invention
Change.Certainly, according to actual needs, Si doped gallium nitride/metal negative electrode battery material provided by the invention also includes others
Common preparation method and step, since the innovation of same invention is unrelated, details are not described herein again.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
Describe in detail it is bright, it should be understood that be not intended to restrict the invention the foregoing is merely the specific embodiment of invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in protection of the invention
Within the scope of.
Claims (11)
1. a kind of Si doped gallium nitride/metal negative electrode battery material, comprising:
Metal substrate；And
The Si doped gallium nitride film being formed in above metal substrate；
Wherein, the Si doped gallium nitride film has loose and porous structure, is crystalline state and amorphous mixed state.
2. negative battery material according to claim 1, one of following material of the material selection of the metal substrate
It is or several: copper foil, nickel foil, foam copper, nickel foam, the copper foil of pre-deposition graphene buffer layers, pre-deposition graphene buffer layers
The nickel foam of nickel foil, the foam copper of pre-deposition graphene buffer layers or pre-deposition graphene buffer layers.
3. negative battery material according to claim 1, the Si doped gallium nitride film with a thickness of 10 μm；And/or
The doping ratio of Si element is 10% in the Si doped gallium nitride film.
4. a kind of Si doped gallium nitride/metal negative electrode battery material preparation method according to claim 1, comprising:
Using radio-frequency sputtering target, Si doped gallium nitride film is deposited on the metallic substrate, and it is negative to obtain Si doped gallium nitride/metal
Pole battery material.
5. the preparation method according to claim 4, the target includes: to be sticked to gallium nitride disk by conductive silver glue
Among Si plate, wherein the diameter of Si plate is equal to target rifle size, and the diameter of gallium nitride disk is most deep in the corresponding groove of sputter area
Locate to be changed in 1cm~3cm nearby, the mixing sputtering target material that group is concentrically arranged.
6. preparation method according to claim 5, the diameter of the gallium nitride disk is between 1.5 inches to 2.4 inches.
7. preparation method according to claim 6, the diameter of the gallium nitride disk is 2 inches.
8. the preparation method according to claim 4, the target includes: that Si plate is sticked to 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 plate is in the corresponding groove bosom of sputter area
It is changed in neighbouring 1cm~3cm, the mixing sputtering target material that group is concentrically arranged.
9. the preparation method according to claim 4, the parameter of the radio-frequency sputtering are as follows:
Underlayer temperature is 300 DEG C~500 DEG C；
Sputtering power is 100W；
Vacuum degree is better than 1.5*10-7Torr；
Background gas pressure is 1Pa；
Nitrogen gas concn is 10ppm；
Target rotation rate is 30r/min；
Sedimentation time is 1hour.
10. a kind of lithium battery, including the doped gallium nitride of Si described in any one of the claims 1 to 3/metal negative electrode battery
Material.
11. lithium battery according to claim 10, the lithium battery is CR2025 type button cell, initial charge capacity
Are as follows: 290mAh/g, discharge capacity are as follows: 350mAh/g, charging platform in 0.2V between 0.85V, discharge platform 0.65V extremely
Between 0.02V.
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| WO2020168517A1 (en) * | 2019-02-21 | 2020-08-27 | 京东方科技集团股份有限公司 | Lithium ion battery and preparation method therefor |
| 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 |
| CN110336028B (en) * | 2019-04-30 | 2021-03-30 | 中国科学院半导体研究所 | Battery negative electrode material, preparation method thereof and lithium battery |
| CN113036107A (en) * | 2021-03-10 | 2021-06-25 | 深圳职业技术学院 | Graphene battery negative electrode material layer, preparation method thereof and lithium ion battery |
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