CN114516624B - Morphology-controllable ferric phosphate, preparation method thereof and lithium iron phosphate - Google Patents
Morphology-controllable ferric phosphate, preparation method thereof and lithium iron phosphate Download PDFInfo
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Abstract
The invention discloses a shape-controllable ferric phosphate, a preparation method thereof and a lithium iron phosphate, and belongs to the field of lithium iron phosphate as a lithium battery anode material. Preparing ferric salt solution by dissolving ferric salt in water; preparing a phosphate solution from phosphoric acid and an alkali solution; adding the ferric salt solution into a stirred reaction kettle, sequentially adding phosphoric acid and hydrogen peroxide into the reaction kettle, adding the phosphate solution into the reaction kettle, heating for synthesis reaction, and aging to obtain a precipitate; filtering the precipitate, washing with deionized water, drying, and sieving to obtain ferric phosphate dihydrate; and sintering and sieving the dihydrate ferric phosphate to obtain anhydrous ferric phosphate. According to the invention, iron phosphate with different sheet shapes can be prepared through adjustment of technological parameters, and the comprehensive properties such as compaction and capacity of lithium iron phosphate prepared by taking the iron phosphate as a raw material have obvious advantages.
Description
Technical Field
The invention belongs to the field of lithium iron phosphate as a lithium battery anode material, and particularly relates to iron phosphate with controllable morphology, a preparation method thereof and lithium iron phosphate prepared from the iron phosphate as a raw material.
Background
The lithium iron phosphate is a novel lithium ion battery anode material, and is widely applied to industries such as new energy automobiles, wind-solar energy storage, communication base stations, large database storage and the like due to the advantages of high safety, long cycle life, low manufacturing cost and the like. Among them, iron phosphate is an important precursor for preparing lithium iron phosphate, and morphology, size and electrochemical properties of lithium iron phosphate are highly dependent on iron phosphate. Research shows that the sheet structure is favorable for increasing the contact between the electrolyte and the anode material, and the electrochemical performance of the lithium iron phosphate material serving as the anode material of the lithium ion battery is integrally improved.
The Chinese patent application No. CN111244447B discloses a flaky ferric phosphate and a preparation method thereof, in particular a method for preparing flaky ferric phosphate by adding morphology control agents such as hexamethylenediamine, terephthalic acid and the like, wherein the morphology control agents all have two coordination points which can guide the growth of crystals, and the Fe is caused by adding complexing agents with two coordination points 3+ And PO (PO) 4 3- FePO formed by the reaction 4 ·2H 2 O particles can be gathered and grown along the horizontal direction guided by coordination points to form flaky ferric phosphate primary particles, and then the flaky primary particles are gradually gathered to form petal-shaped ferric phosphate secondary particles. Chinese patent application CN110357057a discloses a sheet iron phosphate and its preparation method and application, and in particular discloses a method for preparing iron phosphate with primary particles orderly stacked in sheet form by controlling the generation rate of iron phosphate precipitate by using citric acid or citrate as a crystal transformation agent. Although both of these methods can produce a sheet-like iron phosphate, a control agent is required to be added, and if a sheet-like iron phosphate can be directly produced, a lithium iron phosphate having more excellent properties can be produced.
Disclosure of Invention
The invention aims to provide the flaky ferric phosphate dihydrate with controllable morphology, and provides a preparation method with controllable morphology, wherein the preparation method does not need auxiliary additives, and ferric phosphate with different flaky morphologies can be prepared through adjustment of process parameters; and the lithium iron phosphate prepared by taking the iron phosphate as a raw material has obvious advantages in comprehensive properties such as compaction, capacity and the like.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the iron phosphate with controllable morphology comprises the following steps:
dissolving ferric salt in water to prepare ferric salt solution; preparing a phosphate solution from phosphoric acid and an alkali solution;
adding the ferric salt solution into a stirred reaction kettle, sequentially adding phosphoric acid and hydrogen peroxide into the reaction kettle, adding the phosphate solution into the reaction kettle, heating for synthesis reaction, and aging to obtain a precipitate;
filtering the precipitate, washing with deionized water, drying, and sieving to obtain ferric phosphate dihydrate;
and sintering and sieving the dihydrate ferric phosphate to obtain anhydrous ferric phosphate.
Further, the ferric salt is one of ferrous sulfate, ferrous chloride and ferrous oxalate.
Further, the concentration of the ferric salt solution is 0.5-2 mol/L.
Further, the solute of the alkali solution is one of sodium hydroxide, ammonia water and potassium hydroxide.
Further, the pH of the phosphate solution is between 2 and 5 after the alkaline solution is added.
Further, the concentration of the phosphate solution is 0.5-2 mol/L.
Further, the temperature of the synthesis reaction is 80-100 ℃ and the reaction time is 1-5 h.
Further, the sintering temperature is 400-700 ℃ and the sintering time is 4-6 h.
The iron phosphate with controllable morphology is prepared by the method.
The lithium iron phosphate is prepared by taking the iron phosphate prepared by the method as a raw material, adding lithium carbonate, a carbon source and an additive to mix, grinding and sintering.
The ferric phosphate dihydrate prepared by the method is in a sheet shape, the addition amount of the alkali solution is a key for controlling the shape of the ferric phosphate dihydrate, the pH value of the reaction is different according to the addition amount of the alkali solution, the sheet shape and the size of the dimension are changed, and the particle size distribution are also changed. When the alkali liquor addition amount is large, the reaction pH is high, the flaky size of the particles is small, the granularity distribution is narrow, when the alkali liquor addition amount is small, the reaction pH is low, the flaky size of the particles is large, the granularity is large, and the granularity distribution is wide. The method is a key parameter and a control method for controlling the morphology of the ferric phosphate dihydrate, and can control the pH value of the reaction by adjusting the addition amount of the alkali solution in the synthesis process, thereby controlling the morphology and the size of the ferric phosphate dihydrate without any other morphology control agent or crystal transfer agent. The ferric phosphate dihydrate prepared by the method has the advantages of large morphology, large flake size, large granularity, wide distribution and higher tap density, and is particularly suitable for being used as a raw material of high-pressure dense ferric phosphate. The method provided by the invention is simple and flexible to operate, low in cost and suitable for mass production.
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The foregoing and/or additional aspects and advantages of the present invention will become apparent and may be readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a flow chart of a preparation method of morphology-controllable ferric phosphate provided by the invention;
FIG. 2 is an SEM image of the iron phosphate prepared in example 1 of the present invention;
FIG. 3 is a PSD of iron phosphate produced in example 1 of the present invention;
FIG. 4 is an SEM image of the iron phosphate produced in example 3 of the present invention;
FIG. 5 is a PSD of iron phosphate produced in example 3 of the present invention;
fig. 6A-6D are graphs of pH versus anhydrous iron phosphate morphology size and tap density, lithium iron phosphate compaction and capacity for an embodiment of the invention.
Detailed Description
In order to make the above features and advantages of the present invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
The embodiment provides an iron phosphate and a preparation method thereof, and the preparation method comprises the following steps:
1mol/L ferrous sulfate solution is prepared, phosphoric acid and sodium hydroxide are prepared into 1mol/L phosphate solution, and the sodium hydroxide is added in an amount such that the pH value of the phosphate solution is 2.27. Adding ferrous sulfate solution into a stirred reaction kettle, adding phosphoric acid for acidification and hydrogen peroxide for oxidation, then adding phosphate solution, heating to 90 ℃, reacting for 4 hours, ageing for 2 hours, discharging, washing, filtering and drying to obtain ferric phosphate dihydrate. And sintering the ferric phosphate dihydrate at 600 ℃ for 4 hours to obtain the anhydrous ferric phosphate.
And carrying out SEM characterization on the ferric phosphate dihydrate prepared by the operation, wherein the primary particles are in a sheet shape with larger size. The results are shown in FIG. 2; PSD test is carried out on the ferric phosphate dihydrate prepared by the operation, the granularity is 10 mu m, and the result is shown in figure 3; the particle size of the anhydrous ferric phosphate after sintering is 7 mu m, and the tap density is 0.8g/cm 3 。
Grinding anhydrous ferric phosphate, lithium carbonate, carbon source and additive mixture, and sintering to obtain lithium iron phosphate with compaction of 2.65g/cm 3 The specific discharge capacity was 156mAh/g.
Example 2
The embodiment provides an iron phosphate and a preparation method thereof, and the preparation method comprises the following steps:
1mol/L ferrous sulfate solution is prepared, phosphoric acid and sodium hydroxide are prepared into 1mol/L phosphate solution, and the sodium hydroxide is added in an amount such that the pH value of the phosphate solution is 2.51. Adding ferrous sulfate solution into a stirred reaction kettle, adding phosphoric acid for acidification and hydrogen peroxide for oxidation, then adding phosphate solution, heating to 90 ℃, reacting for 4 hours, ageing for 2 hours, discharging, washing, filtering and drying to obtain ferric phosphate dihydrate. And sintering the ferric phosphate dihydrate at 600 ℃ for 5 hours to obtain the anhydrous ferric phosphate.
And carrying out SEM characterization on the ferric phosphate dihydrate prepared by the operation, wherein the primary particles are in a sheet shape with larger size. PSD test is carried out on the ferric phosphate dihydrate prepared by the operation, the granularity is 8 mu m, and the result is shown in figure 4; the particle size of the anhydrous ferric phosphate after sintering is 6 mu m, and the tap density is 0.7g/cm 3 。
Grinding anhydrous ferric phosphate, lithium carbonate, carbon source and additive mixture, and sintering to obtain lithium iron phosphate with compaction of 2.62g/cm 3 The specific discharge capacity was 155mAh/g.
Example 3
The embodiment provides an iron phosphate and a preparation method thereof, and the preparation method comprises the following steps:
1mol/L ferrous sulfate solution is prepared, phosphoric acid and sodium hydroxide are prepared into 1mol/L phosphate solution, and the sodium hydroxide is added in an amount such that the pH value of the phosphate solution is 4.21. Adding ferrous sulfate solution into a stirred reaction kettle, adding phosphoric acid for acidification and hydrogen peroxide for oxidation, then adding phosphate solution, heating to 90 ℃, reacting for 4 hours, ageing for 2 hours, discharging, washing, filtering and drying to obtain ferric phosphate dihydrate. And sintering the ferric phosphate dihydrate at 600 ℃ for 4 hours to obtain the anhydrous ferric phosphate.
And carrying out SEM characterization on the ferric phosphate dihydrate prepared by the operation, wherein the primary particles are in the shape of small-size flakes. The results are shown in FIG. 4; PSD test is carried out on the ferric phosphate dihydrate prepared by the operation, the granularity is 6 mu m, and the result is shown in figure 5; the particle size of the anhydrous ferric phosphate after sintering is 3.5 mu m, and the tap density is 0.55g/cm 3 。
Grinding anhydrous ferric phosphate, lithium carbonate, carbon source and additive mixture, and sintering to obtain lithium iron phosphate with compaction of 2.5g/cm 3 The specific discharge capacity was 154mAh/g.
Example 4
The embodiment provides an iron phosphate and a preparation method thereof, and the preparation method comprises the following steps:
preparing a ferrous sulfate solution with the concentration of 1.5mol/L, preparing a phosphate solution with the concentration of 1.5mol/L by using phosphoric acid and ammonia water, wherein the addition amount of the ammonia water is such that the pH value of the phosphate solution is 3.86. Adding ferrous sulfate solution into a stirred reaction kettle, adding phosphoric acid for acidification and hydrogen peroxide for oxidation, then adding phosphate solution, heating to 80 ℃, reacting for 5 hours, ageing for 2 hours, discharging, washing, filtering and drying to obtain ferric phosphate dihydrate. And sintering the ferric phosphate dihydrate at 700 ℃ for 6 hours to obtain the anhydrous ferric phosphate.
And carrying out SEM characterization on the ferric phosphate dihydrate prepared by the operation, wherein the primary particles are in the shape of small-size flakes. PSD test is carried out on the iron phosphate dihydrate prepared by the operation, the granularity is 10.8 mu m, the granularity of the anhydrous iron phosphate after sintering is 8.5 mu m, and the tap density is 0.67g/cm 3 。
Grinding anhydrous ferric phosphate, lithium carbonate, carbon source and additive mixture, and sintering to obtain lithium iron phosphate with compaction of 2.6g/cm 3 The specific discharge capacity was 154mAh/g.
Example 5
The embodiment provides an iron phosphate and a preparation method thereof, and the preparation method comprises the following steps:
2mol/L ferrous sulfate solution is prepared, phosphoric acid and sodium hydroxide are prepared into 2mol/L phosphate solution, and the addition amount of the sodium hydroxide is such that the pH value of the phosphate solution is 5. Adding ferrous sulfate solution into a stirred reaction kettle, adding phosphoric acid for acidification and hydrogen peroxide for oxidation, then adding phosphate solution, heating to 100 ℃, reacting for 1h, ageing for 2h, discharging, washing, filtering and drying to obtain ferric phosphate dihydrate. The anhydrous ferric phosphate is obtained by sintering the ferric phosphate dihydrate at 400 ℃ for 6 hours.
And carrying out SEM characterization on the ferric phosphate dihydrate prepared by the operation, wherein the primary particles are in the shape of small-size flakes. PSD test is carried out on the iron phosphate dihydrate prepared by the operation, the granularity is 5 mu m, the granularity of the anhydrous iron phosphate after sintering is 3 mu m, and the tap density is 0.50g/cm 3 。
Grinding anhydrous ferric phosphate, lithium carbonate, carbon source and additive mixture, and sintering to obtain lithium iron phosphate with compaction of 2.45g/cm 3 The specific discharge capacity was 152mAh/g.
Example 6
The embodiment provides an iron phosphate and a preparation method thereof, and the preparation method comprises the following steps:
preparing a ferrous sulfate solution with the concentration of 0.5mol/L, preparing a phosphate solution with the concentration of 0.5mol/L by using phosphoric acid and sodium hydroxide, wherein the addition amount of the sodium hydroxide is such that the pH value of the phosphate solution is 2.0. Adding ferrous sulfate solution into a stirred reaction kettle, adding phosphoric acid for acidification and hydrogen peroxide for oxidation, then adding phosphate solution, heating to 90 ℃, reacting for 3 hours, ageing for 2 hours, discharging, washing, filtering and drying to obtain ferric phosphate dihydrate. And sintering the ferric phosphate dihydrate at 600 ℃ for 4 hours to obtain the anhydrous ferric phosphate.
And carrying out SEM characterization on the ferric phosphate dihydrate prepared by the operation, wherein the primary particles are in a sheet shape with larger size. PSD test is carried out on the iron phosphate dihydrate prepared by the operation, the granularity is 8 mu m, the granularity of the anhydrous iron phosphate after sintering is 6 mu m, and the tap density is 0.9g/cm 3 。
Grinding anhydrous ferric phosphate, lithium carbonate, carbon source and additive mixture, and sintering to obtain lithium iron phosphateThe density was 2.7g/cm 3 The specific discharge capacity was 157mAh/g.
The effect of pH adjustment of the alkali solution amount of the above examples on the morphology size and tap density of anhydrous ferric phosphate, lithium iron phosphate compaction and capacity can be presented in Table 1 below.
Properties of Anhydrous ferric phosphate and lithium iron phosphate prepared in examples 1
To further illustrate what table 1 is intended to express, pH versus anhydrous iron phosphate morphology size and tap density, lithium iron phosphate compaction and capacity are plotted against the data in table 1, see fig. 6A-6D. As can be seen from fig. 6A-6D, the particle flake size of the anhydrous ferric phosphate is about small and the tap density is about small when the reaction pH is about high (i.e., the lye addition is about large); the prepared lithium iron phosphate has small compaction and smaller capacity; conversely, when the reaction pH is about low (i.e., the lye addition is about small), the particle flake size of the anhydrous ferric phosphate is about large and the tap density is about large; the prepared lithium iron phosphate has about large compaction and larger capacity.
Although the present invention has been described with reference to the above embodiments, it should be understood that the invention is not limited thereto, and that modifications and equivalents may be made thereto by those skilled in the art, which modifications and equivalents are intended to be included within the scope of the present invention as defined by the appended claims.
Claims (9)
1. The preparation method of the iron phosphate with controllable morphology is characterized by comprising the following steps:
dissolving ferric salt in water to prepare ferric salt solution; preparing a phosphate solution from phosphoric acid and an alkali solution, wherein the pH value of the phosphate solution is between 2 and 5 after the alkali solution is added;
adding the ferric salt solution into a stirred reaction kettle, sequentially adding phosphoric acid and hydrogen peroxide into the reaction kettle, adding the phosphate solution into the reaction kettle, heating for synthesis reaction, and aging to obtain a precipitate;
filtering the precipitate, washing with deionized water, drying, and sieving to obtain ferric phosphate dihydrate;
and sintering and sieving the dihydrate ferric phosphate to obtain anhydrous ferric phosphate.
2. The method of claim 1, wherein the iron salt is one of ferrous sulfate, ferrous chloride, and ferrous oxalate.
3. The method of claim 1, wherein the concentration of the iron salt solution is 0.5 to 2mol/L.
4. The method of claim 1, wherein the solute of the alkaline solution is one of sodium hydroxide, ammonia, and potassium hydroxide.
5. The method of claim 1, wherein the phosphate solution has a concentration of 0.5 to 2mol/L.
6. The method according to claim 1, wherein the temperature of the synthesis reaction is 80 to 100 ℃ and the reaction time is 1 to 5 hours.
7. The method of claim 1, wherein the sintering temperature is 400 to 700 ℃ and the sintering time is 4 to 6 hours.
8. A morphology-controllable iron phosphate, characterized in that it is prepared by the method of any one of claims 1-7.
9. The lithium iron phosphate is characterized in that the lithium iron phosphate prepared by the method of any one of claims 1-7 is used as a raw material, and lithium carbonate, a carbon source and an additive are added for mixing, grinding and sintering to prepare the lithium iron phosphate.
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