CN110311172B - Preparation method and application of LiCuLaZrO solid electrolyte - Google Patents
Preparation method and application of LiCuLaZrO solid electrolyte Download PDFInfo
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Abstract
The invention relates to a preparation method and application of a LiCuLaZrO solid electrolyte, which comprises the following steps: la 2 O 3 、ZrO 2 Mixing the copper compound and the lithium salt, adding a dispersing agent, grinding and drying to obtain a precursor; roasting the precursor at 300-809 ℃, cooling to room temperature, and grinding to obtain LiCuLaZrO powder; and tabletting the LiCuLaZrO powder by using a tabletting machine to obtain a LiCuLaZrO tablet, adding the LiCuLaZrO powder into a roasting container, inserting the LiCuLaZrO tablet into the LiCuLaZrO powder, sintering at 1000-1159 ℃, and cooling to room temperature to obtain the LiCuLaZrO solid electrolyte. Compared with the prior art, the invention has the advantages of simple preparation method, low synthesis temperature, energy conservation and the like.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to a LiCuLaZrO solid electrolyte, a preparation method and application thereof.
Background
The all-solid-state lithium ion battery has the characteristics of high safety, long cycle life, high energy density, wide use temperature range and the like, so that the all-solid-state lithium ion battery becomes a hot point of current research, and the solid electrolyte is one of the core parts of the all-solid-state lithium ion battery. The preparation of the solid electrolyte is usually carried out by a high-temperature solid-phase synthesis method, the synthesis temperature is higher and is approximately more than 1600 ℃; the higher synthesis temperature causes harsh preparation conditions, which is not favorable for expanded production and equipment type selection in the production process.
Chinese patent CN106684440A discloses a preparation method of LiBaLaZrWREAlO solid electrolyte; with La 2 O 3 、ZrO 2 、WO 3 Rare earth oxide, al 2 O 3 And lithium-containing compound as raw material, the first roasting temperature is 810-990 ℃, and the second roasting temperature is 1160-1200 ℃; chinese patent CN106025349A discloses a preparation method of LiBaLaZrREAlO solid electrolyte, and La is used for preparing the solid electrolyte 2 O 3 、ZrO 2 Rare earth oxide, al 2 O 3 And lithium-containing compound as raw material, the first roasting temperature is 810-990 ℃, and the second roasting temperature is 1160-1200 ℃; chinese patent CN106159319A discloses aThe preparation method of the LiBaLaZrAlREWO lithium ion solid electrolyte comprises the steps of roasting at 810-990 ℃ for the first time and 1160-1200 ℃ for the second time; and Chinese patent CN105977531A discloses a preparation method of LiBaLaZrAlREO lithium ion solid electrolyte, wherein the first roasting temperature is 810-990 ℃, and the second roasting temperature is 1160-1200 ℃. The firing temperatures of these patents have further room for reduction; the preparation route of some preparation methods is complex; and the lithium ion conductivity of the solid electrolyte obtained in these patents has room for further improvement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a LiCuLaZrO solid electrolyte, a preparation method and application thereof.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of LiCuLaZrO solid electrolyte comprises the following steps:
(1) La 2 O 3 、ZrO 2 Mixing the copper compound and the lithium salt, adding a dispersing agent, grinding and drying to obtain a precursor;
(2) Roasting the precursor in the step (1) at 300-809 ℃, cooling to room temperature, and grinding to obtain LiCuLaZrO powder;
(3) And (3) tabletting the LiCuLaZrO powder in the step (2) by using a tabletting machine to obtain a LiCuLaZrO tablet, adding the LiCuLaZrO powder into a roasting container, inserting the LiCuLaZrO tablet into the LiCuLaZrO powder, sintering at 1000-1159 ℃, and cooling to room temperature to obtain the LiCuLaZrO solid electrolyte.
The prior art needs a high-temperature roasting temperature of 1600 ℃ and a high precursor treatment temperature, and aims to obtain a better and satisfactory compact structure. According to the invention, a Cu element dopant capable of compacting ceramics is added, lithium salt capable of forming a low minimum eutectic point is adopted as the lithium salt, and the characteristics of the Cu element are utilized to enable each element in LiCuLaZrO to form a compact structure, so that the temperature of the roasting treatment of the precursor is reduced to 300-809 ℃, and in the prior art, the roasting treatment of the precursor needs 810-990 ℃ to form a compact structure which meets the requirements preliminarily; and the subsequent roasting temperature of the invention is also greatly reduced.
In the present invention, the amount of Cu is preferably selected, and when the amount of Cu is too large, impurities are generated to reduce the density of liculazre, and when the amount of Cu is too small, the effect of improving the density of liculazre is insignificant.
In step (1), la 2 O 3 、ZrO 2 And the molar ratio of the copper compound to the lithium salt is 1.25-1.50: 1.60-2.00: 0.10 to 3.00:7.15 to 9.80.
Preferably, in step (1), la 2 O 3 、ZrO 2 And the molar ratio of the copper compound to the lithium salt is 1.25-1.50: 1.60-2.00: 0.10 to 1.50:7.15 to 9.80.
The present invention can further lower the treatment temperature of the sample by further optimizing the content of the Cu element.
In the step (1), the copper compound is selected from one or more of copper oxide, copper sulfate, copper hydroxide, copper nitrate, copper chloride or copper carbonate.
In the step (1), the lithium salt is selected from one or more of lithium hydroxide, lithium nitrate, lithium chloride, lithium oxalate, lithium oxide or lithium carbonate.
In the step (1), the dispersing agent is selected from one or more of ethylene glycol, propanol or isopropanol.
In the step (2), the roasting time of the precursor is 5-7 h.
In the step (3), the method for inserting the LiCuLaZrO pieces into the LiCuLaZrO powder comprises the following steps: in a roasting container, sequentially laying a layer of LiCuLaZrO powder, a layer of LiCuLaZrO sheets and a layer of LiCuLaZrO powder from top to bottom; the ratio of the total weight of the LiCuLaZrO powder to the total weight of the LiCuLaZrO pieces is 0.2-1: 1.
in the step (3), the sintering time of the LiCuLaZrO sheet and the LiCuLaZrO powder is 5-12 h.
The invention also provides an application of the LiCuLaZrO solid electrolyte obtained by the preparation method in the preparation of a lithium battery.
Compared with the prior art, the invention has the following advantages:
(1) The synthesis temperature of the LiCuLaZrO solid electrolyte prepared by the invention is lower, the roasting temperature of the roasting treatment of the precursor is only 300-809 ℃, the sintering temperature is only 1000-1159 ℃, and the requirement on roasting equipment is reduced;
(2) The roasting temperature and the sintering temperature of the roasting treatment of the precursor are reduced, so that the energy is saved;
(3) The lithium ion conductivity of the LiCuLaZrO solid electrolyte prepared by the invention is 3.32 multiplied by 10 -4 S·cm -1 ～1.62×10 -3 S·cm -1 And the conductivity is good.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The lithium ion conductivity of the licula zro solid electrolyte obtained in each example was measured using Solartron1260+1287 electrochemical workstation, uk, see instructions for Solartron1260+1287 electrochemical workstation.
Example 1
Weighing 1.25 mol of La 2 O 3 1.60 mol of ZrO 2 Respectively adding a certain amount of glycol into a 5L ball milling tank, adding 0.10 mol of copper oxide, 2.75 mol of lithium hydroxide and 4.43 mol of lithium nitrate, ball milling for 2h, and drying to obtain a precursor. And putting the precursor into a 3L crucible, burning for 5h at 300 ℃, cooling to room temperature, and grinding to obtain LiCuLaZrO powder. And (2) tabletting the LiCuLaZrO powder by using a tabletting machine to obtain a LiCuLaZrO tablet, adding the LiCuLaZrO powder into a crucible, inserting the LiCuLaZrO tablet into the LiCuLaZrO powder, sintering at 1000 ℃ for 5h, and cooling to room temperature to obtain the LiCuLaZrO solid electrolyte. The lithium ion conductivity of the obtained LiCuLaZrO solid electrolyte was 3.32X 10 -4 S·cm -1 。
Example 2
Weighing 1.50 mol of La 2 O 3 2.00 mol of ZrO 2 Adding a certain amount of isopropanol into a 5L ball milling tank respectively containing 1.00 mol of copper sulfate, 0.50 mol of copper hydroxide and 9.80 mol of lithium carbonate, ball milling for 9h, and drying to obtain a precursor. And putting the precursor into a 3L crucible, burning for 7h at 809 ℃, cooling to room temperature, and grinding to obtain LiCuLaZrO powder. And (2) tabletting the LiCuLaZrO powder by using a tabletting machine to obtain a LiCuLaZrO tablet, adding the LiCuLaZrO powder into a crucible, inserting the LiCuLaZrO tablet into the LiCuLaZrO powder, sintering at 1159 ℃ for 12h, and cooling to room temperature to obtain the LiCuLaZrO solid electrolyte. The lithium ion conductivity of the obtained LiCuLaZrO solid electrolyte was 8.36X 10 -4 S·cm -1 。
Example 3
Weighing 1.38 mol of La 2 O 3 1.80 mol of ZrO 2 Respectively adding a certain amount of propanol into a 5L ball milling tank containing 0.20 mol of copper nitrate, 0.40 mol of copper chloride, 0.20 mol of copper carbonate, 6.28 mol of lithium carbonate and 2.20 mol of lithium hydroxide, carrying out ball milling for 5.5h, and drying to obtain a precursor. And putting the precursor into a 3L crucible, burning for 6h at 554 ℃, cooling to room temperature, and grinding to obtain LiCuLaZrO powder. And (2) tabletting the LiCuLaZrO powder by using a tabletting machine to obtain a LiCuLaZrO tablet, adding the LiCuLaZrO powder into a crucible, inserting the LiCuLaZrO tablet into the LiCuLaZrO powder, sintering at 1079 ℃ for 8.5h, and cooling to room temperature to obtain the LiCuLaZrO solid electrolyte. The lithium ion conductivity of the obtained LiCuLaZrO solid electrolyte was 1.62X 10 -3 S·cm -1 。
Example 4
Weighing 1.32 mol of La 2 O 3 1.70 mol of ZrO 2 Respectively adding a certain amount of propanol into a 5L ball milling tank, adding 0.10 mol of copper oxide, 0.35 mol of lithium hydroxide and 4.93 mol of lithium chloride, ball milling for 3.8h, and drying to obtain a precursor. And putting the precursor into a 3L crucible, burning for 5.5h at 427 ℃, cooling to room temperature, and grinding to obtain LiCuLaZrO powder. The LiCuLaZrO powder is pressed into tablets by a tablet machine to obtain LiCuLaZrO tablets, and LiCuLaZrO powder is added into a crucibleAnd inserting the LiCuLaZrO pieces into the LiCuLaZrO powder, sintering at 1040 ℃ for 7h, and cooling to room temperature to obtain the LiCuLaZrO solid electrolyte. The lithium ion conductivity of the obtained LiCuLaZrO solid electrolyte was 4.32X 10 -4 S·cm -1 。
Example 5
Weighing 1.44 mol of La 2 O 3 1.90 mol of ZrO 2 1.15 mol of copper oxide, 0.4 mol of lithium hydroxide, 5.5 mol of lithium oxalate and 3 mol of lithium oxide are respectively put into a 5L ball milling tank, a certain amount of propanol is added, ball milling is carried out for 5.5h, and drying is carried out to obtain a precursor. And putting the precursor into a 3L crucible, burning for 6.5h at 681 ℃, cooling to room temperature, and grinding to obtain LiCuLaZrO powder. And (2) tabletting the LiCuLaZrO powder by using a tabletting machine to obtain a LiCuLaZrO tablet, adding the LiCuLaZrO powder into a crucible, inserting the LiCuLaZrO tablet into the LiCuLaZrO powder, sintering at 1119 ℃ for 10.3h, and cooling to room temperature to obtain the LiCuLaZrO solid electrolyte. The lithium ion conductivity of the obtained LiCuLaZrO solid electrolyte was 8.78X 10 -4 S·cm -1 。
Example 6
Weighing 1.50 mol of La 2 O 3 2.00 mol of ZrO 2 Respectively adding a certain amount of isopropanol into a 5L ball milling tank, adding 2.00 mol of copper sulfate, 1.00 mol of copper hydroxide and 9.80 mol of lithium carbonate, ball milling for 9h, and drying to obtain a precursor. And putting the precursor into a 3L crucible, burning for 7h at 800 ℃, cooling to room temperature, and grinding to obtain LiCuLaZrO powder. And (2) tabletting the LiCuLaZrO powder by using a tabletting machine to obtain a LiCuLaZrO tablet, adding the LiCuLaZrO powder into a crucible, inserting the LiCuLaZrO tablet into the LiCuLaZrO powder, sintering at 1100 ℃ for 12h, and cooling to room temperature to obtain the LiCuLaZrO solid electrolyte. The lithium ion conductivity of the obtained LiCuLaZrO solid electrolyte was 4.02X 10 -4 S·cm -1 。
By comparing the solid electrolytes of examples 1 to 6 with the reference, it can be seen that the pretreatment temperature and the firing temperature of the electrolyte in this example are both low, and the lithium ion conductivity of the obtained solid electrolyte is equivalent to that in the reference, so the solid electrolyte in this example has significant advantages in terms of temperature resistance of the manufacturing equipment and energy saving requirements during the manufacturing process.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (8)
1. A preparation method of LiCuLaZrO solid electrolyte is characterized by comprising the following steps:
(1) La 2 O 3 、ZrO 2 Mixing the copper compound and the lithium salt, adding a dispersing agent, grinding and drying to obtain a precursor;
(2) Roasting the precursor in the step (1) at 300-809 ℃, cooling to room temperature, and grinding to obtain LiCuLaZrO powder;
(3) Tabletting the LiCuLaZrO powder in the step (2) by using a tabletting machine to obtain a LiCuLaZrO tablet, adding the LiCuLaZrO powder into a roasting container, inserting the LiCuLaZrO tablet into the LiCuLaZrO powder, sintering at 1000-1159 ℃, and cooling to room temperature to obtain the LiCuLaZrO solid electrolyte;
in step (1), la 2 O 3 、ZrO 2 The molar ratio of the copper compound to the lithium salt is 1.25-1.50: 1.60-2.00: 0.80-3.00: 7.15 to 9.80.
2. The method for preparing LiCuLaZrO 2 solid electrolyte according to claim 1, wherein in the step (1), la is added 2 O 3 、ZrO 2 And the molar ratio of the copper compound to the lithium salt is 1.25-1.50: 1.60-2.00: 0.80-1.50: 7.15 to 9.80.
3. The method of claim 1, wherein in the step (1), the copper compound is selected from one or more of copper oxide, copper sulfate, copper hydroxide, copper nitrate, copper chloride and copper carbonate.
4. The method for preparing a solid electrolyte of LiCuLaZrO according to claim 1, wherein in the step (1), the lithium salt is one or more selected from lithium hydroxide, lithium nitrate, lithium chloride, lithium oxalate, lithium oxide and lithium carbonate.
5. The method for preparing LiCuLaZrO solid electrolyte according to claim 1, wherein in the step (1), the dispersing agent is one or more selected from ethylene glycol, propanol or isopropanol.
6. The method for preparing a solid electrolyte of LiCuLaZrO 2 according to claim 1, wherein in the step (2), the calcination time of the precursor is 5-7 h.
7. The method for preparing a solid electrolyte of LiCuLaZrO 2 according to claim 1, wherein in the step (3), the LiCuLaZrO powder is inserted into the LiCuLaZrO powder by the method comprising the following steps: in a roasting container, sequentially laying a layer of LiCuLaZrO powder, a layer of LiCuLaZrO sheets and a layer of LiCuLaZrO powder from top to bottom; the ratio of the total weight of the LiCuLaZrO powder to the total weight of the LiCuLaZrO pieces is 0.2-1; the sintering time of the LiCuLaZrO tablet and the LiCuLaZrO powder is 5-12 h.
8. Use of the preparation process according to claim 1, wherein a lithium battery is produced using the LiCuLaZrO solid electrolyte obtained by the preparation process.
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Citations (4)
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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 |
| CN109037759A (en) * | 2017-06-09 | 2018-12-18 | 中国科学院上海硅酸盐研究所 | Prepare the sintering method of fine and close carbuncle type lithium ion solid electrolyte |
| JP2019006634A (en) * | 2017-06-26 | 2019-01-17 | 日立金属株式会社 | Manufacturing method of solid electrolyte, and solid electrolyte |
| CN109244549A (en) * | 2018-09-03 | 2019-01-18 | 江西理工大学 | Method for preparing garnet electrolyte sheet with high density and high conductivity by guiding crystal growth |
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| US10700378B2 (en) * | 2015-12-17 | 2020-06-30 | The Regents Of The University Of Michigan | Slurry formulation for the formation of layers for solid state batteries |
| WO2017112804A1 (en) * | 2015-12-21 | 2017-06-29 | Johnson Ip Holding, Llc | Solid-state batteries, separators, electrodes, and methods of fabrication |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN109037759A (en) * | 2017-06-09 | 2018-12-18 | 中国科学院上海硅酸盐研究所 | Prepare the sintering method of fine and close carbuncle type lithium ion solid electrolyte |
| JP2019006634A (en) * | 2017-06-26 | 2019-01-17 | 日立金属株式会社 | Manufacturing method of solid electrolyte, and solid electrolyte |
| CN109244549A (en) * | 2018-09-03 | 2019-01-18 | 江西理工大学 | Method for preparing garnet electrolyte sheet with high density and high conductivity by guiding crystal growth |
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