CN114671423A - Pure-phase titanium phosphate lithium electrolyte and preparation method and application thereof - Google Patents
Pure-phase titanium phosphate lithium electrolyte and preparation method and application thereof Download PDFInfo
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- CN114671423A CN114671423A CN202210299495.7A CN202210299495A CN114671423A CN 114671423 A CN114671423 A CN 114671423A CN 202210299495 A CN202210299495 A CN 202210299495A CN 114671423 A CN114671423 A CN 114671423A
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Abstract
The invention discloses a pure-phase titanium lithium phosphate electrolyte and a preparation method and application thereof, wherein the preparation method comprises the following steps: carrying out wet ball milling treatment on lithium hydroxide monohydrate, titanium oxide, ammonium phosphate and aluminum oxide to obtain a mixed raw material; transferring the mixed raw materials to a forced air drying box for drying treatment at the temperature of 150-300 ℃ to obtain dried blocky materials, wherein the exhaust hole end of the forced air drying box is connected with a container filled with water at the other end through a pipeline; and (3) after crushing the dried block material, calcining the crushed material at the temperature of 800-1000 ℃ to obtain the pure-phase lithium titanium phosphate electrolyte. The invention adds the low-temperature drying treatment of the oven before the mixed raw material is calcined, and NH generated by ammonium phosphate in the low-temperature drying treatment process3Can enter water through a pipeline and is dried at low temperatureThe degree of the raw material coking and phosphorization reaction is effectively inhibited; therefore, the phenomenon of severe bulking and hardening can not occur in the subsequent calcining process, the process operation difficulty is greatly reduced, and NH in the subsequent sintering process can be reduced3And (4) pollution problem. From the two aspects, the preparation method provided by the invention is beneficial to large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of solid electrolytes, in particular to a pure-phase lithium titanium phosphate electrolyte and a preparation method and application thereof.
Background
Energy is an important material basis for social development, while traditional fossil energy is increasingly deficient, and the development of the traditional fossil energy also causes serious environmental pollution, so that the development of sustainable new energy is always a research hotspot. The lithium ion battery is convenient to use and mature in technology, and is a development trend of future electrochemical energy storage. At present, increasing requirements provide higher game energy function indexes for lithium ion batteries, and high safety, high energy density, high functional rate and long service life are requirements for the development of the lithium ion batteries.
As is well known, the traditional lithium ion battery has great potential safety hazard because the traditional lithium ion battery contains flammable and explosive organic electrolyte. Secondly, at present, various performance indexes of the lithium ion battery basically reach critical points, but for increasing requirements of high energy density, fast charge and fast discharge and the like, more and more scientists put research attention on the solid-state lithium ion battery. The solid-state lithium ion battery not only reduces the potential safety hazard caused by the existence of the organic electrolyte to a great extent, but also has incomparable advantages in the aspect of improving the overall energy density of the battery, so that the solid-state lithium ion battery is a hot research subject in both academic and industrial fields. As a core constituent element of an all-solid battery, a solid electrolyte is a key material for achieving high energy density, high cycle stability, and high safety of the all-solid battery. Generally, for an ideal solid electrolyte material, it is required to have high ionic conductivity, strong selectivity, good chemical stability, high electronic resistance, good mechanical properties, low cost and simple preparation. Of the many properties, the most important is the ionic conductivity of the material itself.
The solid electrolyte of NASICON structure has stable structure and high ion conductivity, and has been noticed since the discovery, wherein Li is1.3Al0.3Ti1.7(PO4)3(LATP) is the highest conductivity and most widely studied and is now commercially available. The general synthesis of LATP can be divided into liquid phase and solid phase methods, each of which has advantages and disadvantages, but in either case, the synthesis is inevitably carried out using ammonium phosphate salts, especially ammonium dihydrogen phosphate (NH)4H2PO4) Is the main representative. This can present two very serious problems in the industry: the coke phosphorization reaction of phosphate and the discharge of ammonia gas. The former causes the product after reaction to have extremely serious swelling and hardening phenomena as shown in figure 1, and the latter releases a large amount of ammonia gas during sintering to affect the environment. Both of these problems make large-scale industrial production difficult, but such engineering process optimization is rarely mentioned in the current reports.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a pure-phase lithium titanium phosphate electrolyte, a preparation method and application thereof, and aims to solve the problems of puffing and hardening of products caused by a pyrophosphorylation reaction and environmental pollution caused by ammonia emission in the conventional solid phase method for preparing LATP.
The technical scheme of the invention is as follows:
a preparation method of a pure-phase lithium titanium phosphate electrolyte comprises the following steps:
carrying out wet ball milling treatment on lithium hydroxide monohydrate, titanium oxide, ammonium phosphate and aluminum oxide to obtain a mixed raw material;
transferring the mixed raw materials to a forced air drying box for drying treatment at the temperature of 150-300 ℃ to obtain dried blocky materials, wherein the exhaust hole end of the forced air drying box is connected with a container filled with water at the other end through a pipeline;
and (3) crushing the dried blocky material, and then calcining at the temperature of 800-1000 ℃ to obtain the pure-phase lithium titanium phosphate electrolyte.
The preparation method of the pure-phase titanium lithium phosphate electrolyte comprises the step of preparing a pure-phase titanium lithium phosphate electrolyte, wherein ammonium phosphate salt is diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
The preparation method of the pure-phase lithium titanium phosphate electrolyte comprises the following steps of carrying out wet ball milling treatment at a rotating speed of 80-300rpm for 30-720 min.
The preparation method of the pure-phase lithium titanium phosphate electrolyte comprises the step of performing wet ball milling treatment, wherein the ball-to-material ratio is 3:1-5: 1.
The preparation method of the pure-phase lithium titanium phosphate electrolyte comprises the step of transferring the mixed raw materials into a forced air drying oven for drying, wherein the drying time is 0.5-48 h.
The preparation method of the pure-phase lithium titanium phosphate electrolyte comprises the step of crushing the dried blocky material and then calcining the crushed material at the temperature of 800-1000 ℃, wherein the calcining time is 1-6h, and the heating rate is 1-10 ℃/min.
The invention discloses a pure-phase titanium lithium phosphate electrolyte, which is prepared by the preparation method of the pure-phase titanium lithium phosphate electrolyte.
The invention relates to application of a pure-phase titanium lithium phosphate electrolyte, wherein the pure-phase titanium lithium phosphate electrolyte is used for preparing a lithium ion solid-state battery.
Has the beneficial effects that: the invention provides a preparation method of a pure-phase titanium lithium phosphate electrolyte, which is characterized in that an oven low-temperature drying treatment is added before a mixed raw material is calcined, and NH generated by ammonium phosphate is generated in the low-temperature drying treatment process3The coke can enter water through a pipeline, and the coke phosphating reaction degree of the raw materials is effectively inhibited in the low-temperature drying process; therefore, the phenomenon of severe swelling and hardening can not occur in the subsequent calcining process, the process operation difficulty is greatly reduced, and simultaneously the NH in the subsequent sintering process can be reduced3And (4) pollution problem. From the two aspects, the preparation method provided by the invention is beneficial to large-scale industrial production.
Drawings
FIG. 1 is a schematic diagram of a LATP solid electrolyte synthesized by a conventional solid-phase method.
Fig. 2 is a flow chart of a method for preparing a pure-phase lithium titanium phosphate electrolyte according to the present invention.
FIG. 3 is a schematic representation of a brown block of material prepared by the method of example 1.
Fig. 4 is a schematic diagram of a pure phase lithium titanium phosphate electrolyte prepared by the method of example 1.
Fig. 5 is an XRD pattern of a pure phase lithium titanium phosphate electrolyte prepared by the method of example 1.
Detailed Description
The invention provides a pure-phase titanium lithium phosphate electrolyte and a preparation method and application thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 2, fig. 2 is a flow chart of a method for preparing a pure-phase lithium titanium phosphate electrolyte according to the present invention, as shown in the figure, the method includes the steps of:
s10, carrying out wet ball milling treatment on lithium hydroxide monohydrate, titanium oxide, ammonium phosphate and aluminum oxide to obtain a mixed raw material;
s20, transferring the mixed raw materials to a forced air drying oven for drying at the temperature of 150-300 ℃ to obtain dried blocky materials, wherein the exhaust hole end of the forced air drying oven is connected with a container filled with water at the other end through a pipeline;
s30, crushing the dried block-shaped material, and calcining at the temperature of 800-1000 ℃ to obtain the pure-phase lithium titanium phosphate electrolyte.
Specifically, in the conventional method for synthesizing LATP solid electrolyte by solid phase method, because the raw material contains ammonium phosphate salt, the raw material can generate serious coke phosphorization reaction during sintering to form chemical hardening cement-like substance with hard appearance and inside, and simultaneously, because the ammonium phosphate salt can also generate volatile substance ammonia gas during sintering, the sintered product can generate serious bulking and hardening phenomena, as shown in fig. 1. Based on this, the hairBefore the mixed raw material is calcined, the mixed raw material is transferred into a forced air drying oven to be dried at the temperature of 150-300 ℃, and NH generated by ammonium phosphate salt in the drying process3The raw materials can not generate serious coking and phosphorization reaction in the drying process with the temperature limited, namely the coking and phosphorization reaction degree is effectively inhibited in the process; therefore, the phenomenon of severe swelling and hardening can not occur in the subsequent calcining process, the process operation difficulty is greatly reduced, and simultaneously the NH in the subsequent sintering process can be reduced3Pollution problems; from the two aspects, the preparation method provided by the invention is beneficial to large-scale industrial production. The drying temperature of 150-300 ℃ is selected because drying moisture is incomplete and the efficiency is low when the temperature is lower than 150 ℃, and the ammonium phosphate salt is promoted to generate severe cross-linking reaction and generate a large amount of ammonia when the temperature is higher than 300 ℃, so that the finally prepared pure-phase titanium lithium phosphate electrolyte is puffed and hardened.
In some embodiments, the ammonium phosphate salt is, but is not limited to, diammonium phosphate or monoammonium phosphate.
In some embodiments, the rotation speed of the wet ball milling treatment is 80-300rpm for 30-720min, and the ball-to-material ratio in the step of performing the wet ball milling treatment is 3:1-5: 1.
In some embodiments, in the step of drying the mixed raw material, the drying time is 0.5 to 48 hours. In the time range defined by the embodiment, theoretically, the longer the drying time is, the better the drying time is, the too short drying time cannot play a role in preventing the pure-phase lithium titanium phosphate electrolyte from swelling and hardening, and the too long drying time causes the lower efficiency.
In some embodiments, in the step of calcining the dried bulk material after crushing, the calcining time is 1-6h, and the temperature rise rate is 1-10 ℃/min.
The invention also provides a pure-phase lithium titanium phosphate electrolyte, which is prepared by the preparation method of the pure-phase lithium titanium phosphate electrolyte.
The invention also provides an application of the pure-phase lithium titanium phosphate electrolyte, and the pure-phase lithium titanium phosphate electrolyte is used for preparing a lithium ion solid-state battery.
The preparation of a pure phase lithium titanium phosphate electrolyte according to the invention is further illustrated by the following specific examples:
example 1
A preparation method of a pure-phase titanium lithium phosphate electrolyte comprises the following steps:
1. lithium hydroxide monohydrate is used as a lithium source, titanium oxide is used as a titanium source, diammonium hydrogen phosphate or ammonium dihydrogen phosphate is used as a phosphorus source, and aluminum oxide is used as a doping element, and the raw materials are uniformly ground by adopting wet ball milling according to a ratio. The ball milling speed is 150rpm, the ball milling time is 360min, and the ball material ratio is 4: 1;
2. and (2) transferring the raw materials mixed in the step (1) to a blast drying oven for drying at the temperature of 200 ℃ for 24 hours, connecting an exhaust hole of the oven with one end of a high-temperature resistant pipe, and connecting the other end of the oven with a beaker filled with water. In the drying process, ammonia gas continuously circulates from the inside of the oven to the aqueous solution to complete the recovery process. After drying, the material turned into brown block-like material, as shown in fig. 3. After the titanium phosphate lithium electrolyte is slightly crushed, 100g of mixed raw materials are weighed, and the white product is obtained by calcining at 900 ℃ as shown in figure 4, so that the time-varying hardening and swelling phenomenon disappears, the titanium phosphate lithium electrolyte prepared by the embodiment is very fluffy, and the operation difficulty of the next operation procedure is effectively reduced. A99% purity corundum sintering dish is used during sintering, the powder filling thickness is 50cm, the calcining time is 4h, and the temperature rising and reducing speed is 6 ℃/min.
The sintered product of this example is XRD-tested, and the result is shown in fig. 5, and it can be seen from fig. 5 that the lithium titanium phosphate electrolyte prepared in this example is pure cubic phase and contains no other impurity phase.
Example 2
A preparation method of a pure-phase titanium phosphate lithium electrolyte comprises the following steps:
1. lithium hydroxide monohydrate is used as a lithium source, titanium oxide is used as a titanium source, diammonium hydrogen phosphate or ammonium dihydrogen phosphate is used as a phosphorus source, and aluminum oxide is used as a doping element, and the raw materials are uniformly ground by adopting wet ball milling according to a ratio. The ball milling speed is 80rpm, the ball milling time is 720min, and the ball material ratio is 3: 1;
2. and (3) transferring the raw materials mixed in the step (1) to a blast drying oven for drying at the drying temperature of 150 ℃ for 48 hours, wherein an exhaust hole of the drying oven is connected with one end of a high-temperature resistant pipe, and the other end of the drying oven is connected with a beaker filled with water. In the drying process, ammonia gas continuously circulates from the inside of the oven to the aqueous solution to complete the recovery process. And forming brown block-shaped substances after drying. After the titanium phosphate lithium electrolyte is slightly crushed, 200g of mixed raw materials are weighed, and the mixed raw materials are calcined at 1000 ℃ to obtain a white product, at the moment, the hardening and swelling phenomenon disappears, the titanium phosphate lithium electrolyte prepared by the embodiment is very fluffy, and the operation difficulty of the next operation procedure is effectively reduced. During sintering, a 99% purity corundum sintering dish is used, the powder filling thickness is 2cm, the calcination time is 1h, and the temperature rising and reducing speed is 1 ℃/min. The titanium phosphate lithium electrolyte prepared by the embodiment is fluffy, so that the operation difficulty of the next operation procedure is effectively reduced.
Example 3
A preparation method of a pure-phase titanium phosphate lithium electrolyte comprises the following steps:
1. lithium hydroxide monohydrate is used as a lithium source, titanium oxide is used as a titanium source, diammonium hydrogen phosphate or ammonium dihydrogen phosphate is used as a phosphorus source, and aluminum oxide is used as a doping element, and the raw materials are uniformly ground by adopting wet ball milling according to a ratio. The ball milling speed is 300rpm, the ball milling time is 30min, and the ball material ratio is 5: 1;
2. and (3) transferring the raw materials mixed in the step (1) to a blast drying oven for drying at the temperature of 300 ℃ for 0.5h, wherein an exhaust hole of the drying oven is connected with one end of a high-temperature resistant pipe, and the other end of the drying oven is connected with a beaker filled with water. In the drying process, ammonia gas continuously circulates from the inside of the oven to the aqueous solution to complete the recovery process. And obtaining brown block-shaped substances after drying. After the titanium phosphate lithium electrolyte is slightly crushed, 200g of mixed raw materials are weighed, and the mixed raw materials are calcined at 800 ℃ to obtain a white product, at the moment, the hardening and swelling phenomenon disappears, the titanium phosphate lithium electrolyte prepared by the embodiment is very fluffy, and the operation difficulty of the next operation procedure is effectively reduced. A99% purity corundum sintering dish is used during sintering, the powder filling thickness is 10cm, the calcining time is 6h, and the temperature rising and reducing speed is 10 ℃/min. The titanium phosphate lithium electrolyte prepared by the embodiment is fluffy, so that the operation difficulty of the next operation procedure is effectively reduced.
Example 4
A preparation method of a pure-phase titanium phosphate lithium electrolyte comprises the following steps:
1. lithium hydroxide monohydrate is used as a lithium source, titanium oxide is used as a titanium source, diammonium hydrogen phosphate or ammonium dihydrogen phosphate is used as a phosphorus source, and aluminum oxide is used as a doping element, and the raw materials are uniformly ground by adopting wet ball milling according to a ratio. The ball milling speed is 250rpm, the ball milling time is 600min, and the ball material ratio is 5: 1;
2. and (3) transferring the raw materials mixed in the step (1) to a blast drying oven for drying at the drying temperature of 250 ℃ for 32 hours, wherein an exhaust hole of the drying oven is connected with one end of a high-temperature resistant pipe, and the other end of the drying oven is connected with a beaker filled with water. In the drying process, ammonia gas continuously circulates from the inside of the oven to the aqueous solution to complete the recovery process. And obtaining brown block-shaped substances after drying. After the titanium phosphate lithium electrolyte is slightly crushed, 200g of mixed raw materials are weighed, and the mixed raw materials are calcined at 850 ℃ to obtain a white product, at the moment, the hardening and swelling phenomenon disappears, the titanium phosphate lithium electrolyte prepared by the embodiment is very fluffy, and the operation difficulty of the next operation procedure is effectively reduced. A99% purity corundum sintering dish is used during sintering, the powder filling thickness is 8cm, the calcining time is 2h, and the temperature rising and reducing speed is 8 ℃/min. The titanium lithium phosphate electrolyte prepared by the embodiment is fluffy, so that the operation difficulty of the next operation procedure is effectively reduced.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (8)
1. A preparation method of a pure-phase titanium lithium phosphate electrolyte is characterized by comprising the following steps:
carrying out wet ball milling treatment on lithium hydroxide monohydrate, titanium oxide, ammonium phosphate and aluminum oxide to obtain a mixed raw material;
transferring the mixed raw materials to a forced air drying box for drying treatment at the temperature of 150-300 ℃ to obtain dried blocky materials, wherein the exhaust hole end of the forced air drying box is connected with a container filled with water at the other end through a pipeline;
and (3) crushing the dried blocky material, and then calcining at the temperature of 800-1000 ℃ to obtain the pure-phase lithium titanium phosphate electrolyte.
2. The method of preparing a phase-pure titanium lithium phosphate electrolyte of claim 1, wherein the ammonium phosphate salt is diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
3. The method for preparing the pure-phase lithium titanium phosphate electrolyte according to claim 1, wherein the wet ball milling treatment is performed at a rotating speed of 80-300rpm for 30-720 min.
4. The method for preparing the pure-phase titanium lithium phosphate electrolyte according to claim 1, wherein the ball-to-material ratio in the step of performing wet ball milling treatment is 3:1 to 5: 1.
5. The method for preparing the pure-phase titanium lithium phosphate electrolyte according to claim 1, wherein the step of transferring the mixed raw material to a forced air drying oven for drying is performed for 0.5 to 48 hours.
6. The method for preparing the pure-phase lithium titanium phosphate electrolyte as claimed in claim 1, wherein the step of calcining the crushed dried bulk material at the temperature of 1000 ℃ under 800-.
7. A pure-phase lithium titanium phosphate electrolyte, characterized in that it is obtained by the process for the preparation of a pure-phase lithium titanium phosphate electrolyte according to any one of claims 1 to 6.
8. Use of the phase-pure lithium titanium phosphate electrolyte according to claim 8 for the production of a lithium ion solid state battery.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106505248A (en) * | 2016-10-26 | 2017-03-15 | 中国地质大学（武汉） | A kind of glass ceramics type method for preparing solid electrolyte |
| CN111755694A (en) * | 2020-06-15 | 2020-10-09 | 宁波锋成先进能源材料研究院 | Titanium phosphate composite material and preparation method and application thereof |
| CN113346127A (en) * | 2021-05-31 | 2021-09-03 | 东风汽车集团股份有限公司 | NASICON type lithium ion solid electrolyte, preparation method and battery |
| CN113336213A (en) * | 2020-03-03 | 2021-09-03 | 台湾立凯电能科技股份有限公司 | Preparation method of lithium aluminum titanium phosphate for solid electrolyte |
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- 2022-03-25 CN CN202210299495.7A patent/CN114671423A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106505248A (en) * | 2016-10-26 | 2017-03-15 | 中国地质大学（武汉） | A kind of glass ceramics type method for preparing solid electrolyte |
| CN113336213A (en) * | 2020-03-03 | 2021-09-03 | 台湾立凯电能科技股份有限公司 | Preparation method of lithium aluminum titanium phosphate for solid electrolyte |
| CN111755694A (en) * | 2020-06-15 | 2020-10-09 | 宁波锋成先进能源材料研究院 | Titanium phosphate composite material and preparation method and application thereof |
| CN113346127A (en) * | 2021-05-31 | 2021-09-03 | 东风汽车集团股份有限公司 | NASICON type lithium ion solid electrolyte, preparation method and battery |
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