CN110311172A - A kind of LiCuLaZrO method for preparing solid electrolyte and application - Google Patents
A kind of LiCuLaZrO method for preparing solid electrolyte and application Download PDFInfo
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Abstract
The present invention relates to a kind of LiCuLaZrO method for preparing solid electrolyte and applications, comprising the following steps: by La2O3、ZrO2, copper compound and lithium salts mixing, be added dispersing agent, by grinding, being dried to obtain presoma；By presoma in 300~809 DEG C of calcination process, it is cooled to room temperature, grinds, obtains LiCuLaZrO powder；LiCuLaZrO powder tabletting is obtained into LiCuLaZrO piece with tablet press machine, LiCuLaZrO powder is added in calcination vessel, the LiCuLaZrO piece is inserted into LiCuLaZrO powder, is sintered at 1000~1159 DEG C, it is cooled to room temperature, obtains the LiCuLaZrO solid electrolyte.Compared with prior art, the present invention has many advantages, such as that preparation method is simple, synthesis temperature is low, energy saving.
Description
Technical field
The invention belongs to electrochemical technology field, more particularly, to a kind of LiCuLaZrO solid electrolyte, preparation method and
Using.
Background technique
All-solid lithium-ion battery due to high security, have extended cycle life, energy density is high, use temperature range is wide
The features such as, become the hot spot studied now, solid electrolyte is one of core of all-solid lithium-ion battery.Solid electrolytic
High temperature solid phase synthesis is commonly used in the preparation of matter, and synthesis temperature is higher, and temperature is probably at 1600 DEG C or more；Higher synthesis temperature is made
At preparation condition harshness, the lectotype selection being unfavorable in expanded production and production process.
Chinese patent CN106684440A discloses a kind of LiBaLaZrWREAlO method for preparing solid electrolyte；With
La2O3、ZrO2、WO3, rare earth oxide, Al2O3It is raw material with lithium-containing compound, first time maturing temperature is 810~990 DEG C, the
After baking temperature is 1160~1200 DEG C；Chinese patent CN106025349A discloses a kind of LiBaLaZrREAlO solid electricity
The preparation method of matter is solved, with La2O3、ZrO2, rare earth oxide, Al2O3It is raw material with lithium-containing compound, first time maturing temperature is
810~990 DEG C, second of maturing temperature is 1160~1200 DEG C；Chinese patent CN106159319A discloses one kind
The preparation method of LiBaLaZrAlREWO lithium ion solid electrolyte, this method first time maturing temperature are 810~990 DEG C, the
After baking temperature is 1160~1200 DEG C；And Chinese patent CN105977531A discloses a kind of LiBaLaZrAlREO lithium
Ion solid electrolyte preparation method is with this method first time maturing temperature is 810~990 DEG C, and second of maturing temperature is
1160~1200 DEG C.The maturing temperature of these patents is also further reduced space；The preparation route of some preparation methods, system
Preparation Method is complicated；And the lithium ion conductivity of solid electrolyte obtained in these patents improves space there are also further.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of LiCuLaZrO solids
Electrolyte, preparation method and application.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of LiCuLaZrO method for preparing solid electrolyte, comprising the following steps:
(1) by La2O3、ZrO2, copper compound and lithium salts mixing, be added dispersing agent, by grinding, being dried to obtain presoma；
(2) presoma in step (1) is cooled to room temperature, ground, obtained in 300~809 DEG C of calcination process
LiCuLaZrO powder；
(3) the LiCuLaZrO powder tabletting in step (2) is obtained into LiCuLaZrO piece with tablet press machine, in calcination vessel
LiCuLaZrO powder is added, the LiCuLaZrO piece is inserted into LiCuLaZrO powder, is sintered at 1000~1159 DEG C,
It is cooled to room temperature, obtains the LiCuLaZrO solid electrolyte.
Need in the prior art 1600 DEG C of high temperature maturing temperature and higher presoma treatment temperature, be to obtain
Preferably, satisfactory compact texture.The present invention is added to the Cu elemental dopant that can make ceramic dense, and lithium salts is using energy shape
At the lithium salts of low lowest total of the melting point, using the characteristic of Cu element, so that each element forms compact texture in LiCuLaZrO,
So that presoma calcination process obtains temperature and is reduced to 300~809 DEG C, and in the prior art, presoma calcination process then needs 810
~990 DEG C, preliminary satisfactory compact texture could be formed；And subsequent maturing temperature of the invention is greatly reduced.
The preferred additive amount of Cu element, when the additive amount of Cu element is excessive, will lead to the generation of impurity in the present invention, drop
When the additive amount of the consistency of low LiCuLaZrO, Cu element is very few, the consistency effect for improving LiCuLaZrO is not significant.
In step (1), La2O3、ZrO2, copper compound and lithium salts molar ratio be 1.25~1.50:1.60~2.00:
0.10~3.00:7.15~9.80.
Preferably, in step (1), La2O3、ZrO2, copper compound and lithium salts molar ratio be 1.25~1.50:1.60~
2.00:0.10~1.50:7.15~9.80.
The present invention can further decrease the treatment temperature of sample by the content of further preferred Cu element.
In step (1), the copper compound is selected from copper oxide, copper sulphate, Kocide SD, copper nitrate, copper chloride or carbonic acid
One or more of copper.
In step (1), lithium salts in lithium hydroxide, lithium nitrate, lithium chloride, lithium oxalate, lithia or lithium carbonate one
Kind is several.
In step (1), the dispersing agent is selected from one or more of ethylene glycol, propyl alcohol or isopropanol.
In step (2), the calcining time of presoma is 5~7h.
In step (3), the method for LiCuLaZrO piece insertion LiCuLaZrO powder are as follows: in calcination vessel, from upper
Under be successively laid with one layer of LiCuLaZrO powder, one layer of LiCuLaZrO piece and one layer and LiCuLaZrO powder；It is described
The ratio of LiCuLaZrO powder total weight and the LiCuLaZrO piece total weight is 0.2~1:1.
In step (3), the sintering time of the LiCuLaZrO piece and LiCuLaZrO powder is 5~12h.
The present invention also provides a kind of answering for LiCuLaZrO solid electrolyte production lithium battery obtained using the preparation method
With.
Compared with prior art, the invention has the following advantages that
(1) synthesis temperature of the invention for preparing LiCuLaZrO solid electrolyte is lower, the roasting temperature of presoma calcination process
Degree is only 300~809 DEG C, and sintering temperature is only 1000~1159 DEG C, reduces the requirement to roasting apparatus；
(2) due to reducing the maturing temperature and sintering temperature of presoma calcination process, the energy is saved；
(3) lithium ion conductivity of LiCuLaZrO solid electrolyte prepared by the present invention is 3.32 × 10-4S·cm-1~
1.62×10-3S·cm-1, conduct electricity very well.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
The lithium ion conductivity of LiCuLaZrO solid electrolyte Britain Solartron1260+ obtained in each embodiment
1287 electrochemical workstations are measured, and measuring method is shown in the operation instruction of Solartron1260+1287 electrochemical workstation
Book.
Embodiment 1
Weigh 1.25 moles of La2O3, 1.60 moles of ZrO2, 0.10 moles copper, 2.75 molar lithium hydroxides and 4.43 rub
Your lithium nitrate is respectively that a certain amount of ethylene glycol is added in 5L ball grinder, and ball milling 2h is dry, obtains presoma.Before above-mentioned
It drives body to be put into 3L crucible, calcination 5h, is cooled to room temperature at 300 DEG C, grinds, and obtains LiCuLaZrO powder.It will be upper with tablet press machine
It states LiCuLaZrO powder and is pressed into piece and obtain LiCuLaZrO piece, LiCuLaZrO powder is added in crucible, by LiCuLaZrO piece
It is inserted into LiCuLaZrO powder, is sintered 5h at 1000 DEG C, is cooled to room temperature, obtain LiCuLaZrO solid electrolyte.It obtains
The lithium ion conductivity of LiCuLaZrO solid electrolyte is 3.32 × 10-4S·cm-1。
Embodiment 2
Weigh 1.50 moles of La2O3, 2.00 moles of ZrO2, 1.00 mol sulfuric acid copper, 0.50 mole of Kocide SD and 9.80 rub
Your lithium carbonate is respectively that a certain amount of isopropanol is added in 5L ball grinder, and ball milling 9h is dry, obtains presoma.Before above-mentioned
It drives body to be put into 3L crucible, calcination 7h, is cooled to room temperature at 809 DEG C, grinds, and obtains LiCuLaZrO powder.It will be upper with tablet press machine
It states LiCuLaZrO powder and is pressed into piece and obtain LiCuLaZrO piece, LiCuLaZrO powder is added in crucible, by LiCuLaZrO piece
It is inserted into LiCuLaZrO powder, is sintered 12h at 1159 DEG C, is cooled to room temperature, obtain LiCuLaZrO solid electrolyte.It obtains
The lithium ion conductivity of LiCuLaZrO solid electrolyte is 8.36 × 10-4S·cm-1。
Embodiment 3
Weigh 1.38 moles of La2O3, 1.80 moles of ZrO2, 0.20 molar nitric acid copper, 0.40 mole of copper chloride, 0.20 mole
Copper carbonate, 6.28 moles of lithium carbonates and 2.20 molar lithium hydroxides are respectively that a certain amount of propyl alcohol, ball is added in 5L ball grinder
5.5h is ground, it is dry, obtain presoma.Above-mentioned presoma is put into 3L crucible, the calcination 6h at 554 DEG C is cooled to room temperature, mill
It is broken, obtain LiCuLaZrO powder.Above-mentioned LiCuLaZrO powder is pressed into piece with tablet press machine and obtains LiCuLaZrO piece, in crucible
LiCuLaZrO piece is inserted into LiCuLaZrO powder, is sintered 8.5h at 1079 DEG C, is cooled to by middle addition LiCuLaZrO powder
Room temperature obtains LiCuLaZrO solid electrolyte.The lithium ion conductivity of obtained LiCuLaZrO solid electrolyte be 1.62 ×
10-3S·cm-1。
Embodiment 4
Weigh 1.32 moles of La2O3, 1.70 moles of ZrO2, 0.10 moles copper, 0.35 molar lithium hydroxide and 4.93 rub
Your lithium chloride is respectively that a certain amount of propyl alcohol is added in 5L ball grinder, and ball milling 3.8h is dry, obtains presoma.Before above-mentioned
It drives body to be put into 3L crucible, calcination 5.5h, is cooled to room temperature at 427 DEG C, grinds, and obtains LiCuLaZrO powder.It will with tablet press machine
Above-mentioned LiCuLaZrO powder is pressed into piece and obtains LiCuLaZrO piece, LiCuLaZrO powder is added in crucible, by LiCuLaZrO
Piece is inserted into LiCuLaZrO powder, is sintered 7h at 1040 DEG C, is cooled to room temperature, obtains LiCuLaZrO solid electrolyte.It obtains
LiCuLaZrO solid electrolyte lithium ion conductivity be 4.32 × 10-4S·cm-1。
Embodiment 5
Weigh 1.44 moles of La2O3, 1.90 moles of ZrO2, 1.15 moles copper, 0.4 molar lithium hydroxide, 5.5 moles
Lithium oxalate and 3 moles lithiums are respectively that a certain amount of propyl alcohol is added in 5L ball grinder, and ball milling 5.5h is dry, obtains forerunner
Body.Above-mentioned presoma is put into 3L crucible, calcination 6.5h, is cooled to room temperature at 681 DEG C, grinds, and obtains LiCuLaZrO powder
Body.Above-mentioned LiCuLaZrO powder is pressed into piece with tablet press machine and obtains LiCuLaZrO piece, LiCuLaZrO powder is added in crucible
LiCuLaZrO piece is inserted into LiCuLaZrO powder, is sintered 10.3h at 1119 DEG C, is cooled to room temperature, obtain by body
LiCuLaZrO solid electrolyte.The lithium ion conductivity of obtained LiCuLaZrO solid electrolyte is 8.78 × 10-4S·cm-1。
Embodiment 6
Weigh 1.50 moles of La2O3, 2.00 moles of ZrO2, 2.00 mol sulfuric acid copper, 1.00 moles of Kocide SDs and 9.80 rub
Your lithium carbonate is respectively that a certain amount of isopropanol is added in 5L ball grinder, and ball milling 9h is dry, obtains presoma.Before above-mentioned
It drives body to be put into 3L crucible, calcination 7h, is cooled to room temperature at 800 DEG C, grinds, and obtains LiCuLaZrO powder.It will be upper with tablet press machine
It states LiCuLaZrO powder and is pressed into piece and obtain LiCuLaZrO piece, LiCuLaZrO powder is added in crucible, by LiCuLaZrO piece
It is inserted into LiCuLaZrO powder, is sintered 12h at 1100 DEG C, is cooled to room temperature, obtain LiCuLaZrO solid electrolyte.It obtains
The lithium ion conductivity of LiCuLaZrO solid electrolyte is 4.02 × 10-4S·cm-1。
By comparing the solid electrolyte of Examples 1 to 6 and documents, it can be seen that the electrolyte in the present embodiment
Pretreatment temperature and maturing temperature it is lower, and obtain solid electrolyte lithium ion conductivity and documents in
Lithium ion conductivity it is suitable, therefore, from the heatproof degree and preparation process to Preparation equipment power conservation requirement angle come
It says, the solid electrolyte in the present embodiment has apparent advantage.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (9)
1. a kind of LiCuLaZrO method for preparing solid electrolyte, which comprises the following steps:
(1) by La2O3、ZrO2, copper compound and lithium salts mixing, be added dispersing agent, by grinding, being dried to obtain presoma；
(2) presoma in step (1) is cooled to room temperature, ground in 300~809 DEG C of calcination process, obtain LiCuLaZrO powder
Body；
(3) the LiCuLaZrO powder tabletting in step (2) is obtained into LiCuLaZrO piece with tablet press machine, is added in calcination vessel
The LiCuLaZrO piece is inserted into LiCuLaZrO powder, is sintered, is cooled at 1000~1159 DEG C by LiCuLaZrO powder
Room temperature obtains the LiCuLaZrO solid electrolyte.
2. a kind of LiCuLaZrO method for preparing solid electrolyte according to claim 1, which is characterized in that step (1)
In, La2O3、ZrO2, copper compound and lithium salts molar ratio be 1.25~1.50:1.60~2.00:0.10~3.00:7.15~
9.80。
3. a kind of LiCuLaZrO method for preparing solid electrolyte according to claim 2, which is characterized in that step (1)
In, La2O3、ZrO2, copper compound and lithium salts molar ratio be 1.25~1.50:1.60~2.00:0.10~1.50:7.15~
9.80。
4. a kind of LiCuLaZrO method for preparing solid electrolyte according to claim 1, which is characterized in that step (1)
In, the copper compound is selected from one of copper oxide, copper sulphate, Kocide SD, copper nitrate, copper chloride or copper carbonate or several
Kind.
5. a kind of LiCuLaZrO method for preparing solid electrolyte according to claim 1, which is characterized in that step (1)
In, the lithium salts is selected from one or more of lithium hydroxide, lithium nitrate, lithium chloride, lithium oxalate, lithia or lithium carbonate.
6. a kind of LiCuLaZrO method for preparing solid electrolyte according to claim 1, which is characterized in that step (1)
In, the dispersing agent is selected from one or more of ethylene glycol, propyl alcohol or isopropanol.
7. a kind of LiCuLaZrO method for preparing solid electrolyte according to claim 1, which is characterized in that step (2)
In, the calcining time of presoma is 5~7h.
8. a kind of LiCuLaZrO method for preparing solid electrolyte according to claim 1, which is characterized in that step (3)
In, the method for LiCuLaZrO piece insertion LiCuLaZrO powder are as follows: in calcination vessel, be successively laid with one layer under upper
LiCuLaZrO powder, one layer of LiCuLaZrO piece and one layer and LiCuLaZrO powder；The LiCuLaZrO powder gross weight
The ratio of amount and the LiCuLaZrO piece total weight is 0.2~1；When the sintering of the LiCuLaZrO piece and LiCuLaZrO powder
Between be 5~12h.
9. a kind of application of preparation method as described in claim 1, which is characterized in that obtained using the preparation method
LiCuLaZrO solid electrolyte makes lithium battery.
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| JP2019006634A (en) * | 2017-06-26 | 2019-01-17 | 日立金属株式会社 | Manufacturing method of solid electrolyte, and solid electrolyte |
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2019
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| CN105186031A (en) * | 2015-09-21 | 2015-12-23 | 中国科学院上海硅酸盐研究所 | Garnet-structured ceramic electrolyte material, preparation method and application therefor |
| US20170179521A1 (en) * | 2015-12-17 | 2017-06-22 | Jeffrey Sakamoto | Slurry Formulation for the Formation of Layers for Solid State Batteries |
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