CN114477232A - High-quality K2Zn3[Fe(CN)6]2Preparation of crystals and use thereof - Google Patents
High-quality K2Zn3[Fe(CN)6]2Preparation of crystals and use thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
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- C01C3/08—Simple or complex cyanides of metals
- C01C3/12—Simple or complex iron cyanides
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/38—Particle morphology extending in three dimensions cube-like
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Abstract
The invention discloses a high-quality K2Zn3[Fe(CN)6]2Process for preparing crystal from ZnSO4·7H2O as a zinc source, with K4Fe(CN)6·3H2Taking O as a single iron source, taking potassium citrate or potassium pyrophosphate as a complexing agent, and preparing K by adopting a room-temperature coprecipitation method2Zn3[Fe(CN)6]2And (4) crystals. The invention uses the complexing agent to regulate and control the grain size of the material, reduces the defects of the material and has simple preparation process, compared with other Prussian blue analogues, the material has a large open frame structure, more stable structure, higher conductivity, excellent cycle performance and good rate capability, and is an ideal potassium ion battery anode material.
Description
Technical Field
The invention belongs to the technical field of battery materials, and particularly relates to high-quality K2Zn3[Fe(CN)6]2Preparation of crystal and its application.
Background
Prussian blue analogues (e.g.: K)0.08Zn1.44[Fe(CN)6]) The open frame structure is beneficial to the desorption of large ions, so the composite material is a potassium ion battery positive electrode material with great development potential. However, the sample may generate a large amount of defects, i.e., vacancies and interstitial water, due to rapid precipitation during its preparation. The collapse of the structure can be caused in the long circulation process, the coulombic efficiency is low, and the conductivity of the material is poor.
Prussian blue analogues have been reported to have a relatively lower density than Potassium Ion batteries [ Heo, J.W., et al., Rhombohedral Potas-Zinc Hexacyanoferrate as a cathodal Material for Nonaqueous Potasum-Ion batteries. Inorg. Chem, 2019.58 (5): p. 3065. 3072.] and [ Islas-Vargas C, Guevara-Garcia A, Oliver-Tolentino M, Ramos-Sanchez G, Gonzalez I, Galvan M. Experimental and the ethical information on the origin of the high ranking volumetric of K2Zn3[ Fe (CN)6]2 [ Fe (CN) 2 ] 2. J.ectrocarom C. Soctrochem. 8; 2013A 51166. has been reported to have a relatively lower density than the prior art Potassium Ion batteries and to be applied to Potassium Ion batteries [ Heo, J.W., et al., Rhombohedral-Zinc 7 ] 2. A, though there are no more initial current cycles than the prior art Potassium Ion battery analogues, which have been reported to be applied to the prior art batteries, such a relatively lower density metals, such as the prior art Potassium Ion batteries, such as the prior art blue analogues, such as the prior art, the high density of Potassium Ion batteries, such as the high density of the prior art, the high density of the Potassium Ion batteries, high density of the Potassium Ion batteries, low density of the high density of the Potassium Ion batteries, low density of the high density of the Potassium Ion batteries, and the high density of the low density of the high density of the Potassium Ion batteries, and the high density of the low density of the high density of the batteries, and the high density of the batteries, and low density of the Potassium Ion batteries, and the low density of the batteries, and the high density of the Potassium Ion batteries, such as the high density of the batteries, such as the low density of the high density of the low density of the batteries, such as the high density of the low density of the high density of the low density of the battery, and the battery, such as, the specific discharge capacity is not high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the high-quality K2Zn3[Fe(CN)6]2Preparation of crystals and use thereof, K2Zn3[Fe(CN)6]2The crystal structure (figure 1) provides possibility for insertion/extraction of large ions during charge and discharge. By regulating and controlling the dosage of the complexing agent, the optimal crystal size is prepared, the content of vacancy and interstitial water of the material is reduced, and the open framework structure is optimized, so that the material structure is not easy to collapse in the circulating process. K prepared by the invention2Zn3[Fe(CN)6]2The battery has excellent potassium storage performance, and the battery assembled by using the potassium storage material as a positive electrode material has the advantages of relatively high specific capacity, good rate capability and the like, and has wide application prospect.
In order to achieve the purpose, the invention is realized by the following technical scheme:
high-quality K2Zn3[Fe(CN)6]2Process for preparing crystal from ZnSO4·7H2O as a zinc source, with K4Fe(CN)6·3H2Taking O as a single iron source, taking potassium citrate as a complexing agent, and preparing K by adopting a room-temperature coprecipitation method2Zn3[Fe(CN)6]2And (4) crystals.
Preferably, the complexing agent can also be replaced by potassium pyrophosphate.
Preferably, said one high quality K2Zn3[Fe(CN)6]2The preparation method of the crystal comprises the following steps:
s1: weighing 0.287-0.861 g ZnSO at room temperature4·7H2Mixing O and 0.65-1.30 g of complexing agent, putting the mixture into a first magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the mixture is dissolved to obtain a solution A;
s2: weighing 0.422-0.844 g K4Fe(CN)6·3H2Placing the O into a second magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the O is dissolved to obtain a solution B;
s3: pushing the solution A into the solution B through a peristaltic pump;
s4: standing and aging for 12 hours after uniform mixing to obtain white precipitate;
s5: washing the white precipitate for several times with washing liquid, and drying to obtain K2Zn3[Fe(CN)6]2A material.
Preferably, in step S3, the second magnetic stirrer is in a magnetic stirring state all the time during the process of pushing the solution a into the solution B through the peristaltic pump.
Preferably, in step S5, the washing solution is deionized water and ethanol.
Preferably, in step S5, the drying temperature is 60 ℃ and the drying time is 24 hours.
Preferably, said one high quality K2Zn3[Fe(CN)6]2Method of using crystals, and method packageThe method comprises the following steps:
d1: preparing a PVDF solution with the concentration of 40 mg/ml by taking N-methyl pyrrolidone as a solvent;
d2: according to the mass ratio of 6: 2: 2 will K2Zn3[Fe(CN)6]2Mixing and grinding the crystal material, the carbon black and the PVDF for one hour to prepare uniform slurry;
d3: coating the slurry on aluminum foil, drying at 60 deg.C, and vacuum drying at 120 deg.C for 12 hr;
d4: punching into an electrode plate with the diameter of 1.2 cm.
Preferably, said one high quality K2Zn3[Fe(CN)6]2The application method of the crystal further comprises the following steps:
d5: and (3) assembling by using metal potassium as a counter electrode and 2.5M KFSI in TEP as electrolyte to prepare the battery.
Preferably, in step D5, the assembly is performed in a glove box.
Preferably, K is prepared by the preparation method2Zn3[Fe(CN)6]2The crystalline material is in the form of tetragonal crystal particles of 1.0-2.5 microns.
(III) advantageous effects
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention relates to a high-quality K2Zn3[Fe(CN)6]2The invention adopts room temperature coprecipitation method, the preparation process is simple, the repeatability is high, the requirement for experimental equipment is low, and the invention is suitable for industrial production. Meanwhile, the used raw materials have low manufacturing cost, low integral manufacturing cost and high yield.
(2) The invention relates to a high-quality K2Zn3[Fe(CN)6]2Preparation of crystals and application thereof, product K prepared by the invention2Zn3[Fe(CN)6]2Is micron-sized crystal particles, has the characteristics of good crystallinity, high yield and the like, has less defects, high coulombic efficiency and good rate capability compared with other Prussian blue analogues, and is a compoundThe potassium ion anode material is ideal.
Drawings
FIG. 1 shows K prepared in an example of the present invention2Zn3[Fe(CN)6]2Crystal structure diagram of the material.
FIG. 2 shows K prepared in accordance with an embodiment of the present invention2Zn3[Fe(CN)6]2X-ray diffraction pattern of the material.
FIG. 3 is K prepared according to an embodiment of the invention2Zn3[Fe(CN)6]2An X-ray photoelectron spectrum of the material.
FIG. 4 shows K prepared in accordance with an embodiment of the present invention2Zn3[Fe(CN)6]2Scanning electron micrographs of the material at 5000 x.
FIG. 5 shows K prepared according to an example of the present invention2Zn3[Fe(CN)6]2Scanning electron micrograph of material at 30000 times.
FIG. 6 shows K prepared according to an embodiment of the invention2Zn3[Fe(CN)6]2The material is used for a rate performance graph of a potassium ion battery.
FIG. 7 shows K prepared according to an embodiment of the invention2Zn3[Fe(CN)6]2The material is used for a cycle performance diagram of a potassium ion battery.
FIG. 8 shows K of the present invention2Zn3[Fe(CN)6]2A flow chart of a preparation method of the material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present invention, unless otherwise expressly specified or limited, the terms "disposed," "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected or detachably connected; may be a mechanical connection; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
Example 1
As shown in FIGS. 1-7, a high quality K2Zn3[Fe(CN)6]2Process for preparing crystal from ZnSO4·7H2O as a zinc source, with K4Fe(CN)6·3H2Taking O as a single iron source, taking potassium citrate as a complexing agent, and preparing K by adopting a room-temperature coprecipitation method2Zn3[Fe(CN)6]2And (4) crystals.
The complexing agent can also be replaced by potassium pyrophosphate.
Said one high quality K2Zn3[Fe(CN)6]2The preparation method of the crystal comprises the following steps:
s1: weighing 0.287-0.861 g ZnSO at room temperature4·7H2Mixing O and 0.65-1.30 g of complexing agent, putting the mixture into a first magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the mixture is dissolved to obtain a solution A;
s2: weighing 0.422-0.844 g K4Fe(CN)6·3H2Placing the O into a second magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the O is dissolved to obtain a solution B;
s3: pushing the solution A into the solution B through a peristaltic pump;
s4: standing and aging for 12 hours after uniform mixing to obtain white precipitate;
s5: whitening with washing liquidWashing the color precipitate for several times, and drying to obtain K2Zn3[Fe(CN)6]2A material.
In step S3, the second magnetic stirrer is always in a magnetic stirring state during the process of pushing the solution a into the solution B through the peristaltic pump.
In step S5, the washing solution is deionized water and ethanol.
In step S5, the drying temperature was 60 ℃ and the drying time was 24 hours.
K prepared by the preparation method2Zn3[Fe(CN)6]2The crystalline material is in the form of tetragonal crystal particles of 1.0-2.5 microns.
Example 2
As shown in FIGS. 1-7, in this embodiment, a high quality K2Zn3[Fe(CN)6]2Process for preparing crystal from ZnSO4·7H2O as a zinc source, with K4Fe(CN)6·3H2Taking O as a single iron source, taking potassium citrate as a complexing agent, and preparing K by adopting a room-temperature coprecipitation method2Zn3[Fe(CN)6]2And (4) crystals.
Said one high quality K2Zn3[Fe(CN)6]2The preparation method of the crystal comprises the following steps:
s1: weighing 0.287g ZnSO at room temperature4·7H2Mixing O and 1.30 g of potassium citrate, putting the mixture into a first magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the mixture is dissolved to obtain a solution A;
s2: weighing 0.422 g K4Fe(CN)6·3H2Placing the O into a second magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the O is dissolved to obtain a solution B;
s3: pushing the solution A into the solution B through a peristaltic pump;
s4: standing and aging for 12 hours after uniform mixing to obtain white precipitate;
s5: washing the white precipitate for several times with washing liquid, and drying to obtain K2Zn3[Fe(CN)6]2A material.
In step S3, the second magnetic stirrer is always in a magnetic stirring state during the process of slowly pushing the solution a into the solution B through the peristaltic pump.
In step S5, the washing solution is deionized water and ethanol.
In step S5, the drying temperature was 60 ℃ and the drying time was 24 hours.
K prepared by the preparation method2Zn3[Fe(CN)6]2The crystalline material is in the form of tetragonal crystal particles of 1.0-2.5 microns.
FIG. 1 is K2Zn3[Fe(CN)6]2The crystal structure of the material, an open framework structure can be seen.
FIG. 2 is K2Zn3[Fe(CN)6]2The strong diffraction peak of the X-ray diffraction pattern of the material indicates that the crystallinity of the product is good.
FIG. 3 is K2Zn3[Fe(CN)6]2The X-ray photoelectron spectrum of the material proves the existence of K, Zn and Fe elements.
FIG. 4 and FIG. 5 are K2Zn3[Fe(CN)6]2Scanning electron micrographs of the material at 5000 times and 30000 times. It can be seen that K2Zn3[Fe(CN)6]2Has a crystal size of about 1 um.
Example 3
In this embodiment, a high quality K2Zn3[Fe(CN)6]2Process for preparing crystal from ZnSO4·7H2O as a zinc source, with K4Fe(CN)6·3H2Taking O as a single iron source, taking potassium citrate as a complexing agent, and preparing K by adopting a room-temperature coprecipitation method2Zn3[Fe(CN)6]2And (4) crystals.
Said one high quality K2Zn3[Fe(CN)6]2The preparation method of the crystal comprises the following steps:
s1: weighing 0.287g ZnSO at room temperature4·7H2Mixing O and 0.65g of potassium citrate, putting the mixture into a first magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the mixture is dissolved to obtain a solution A;
s2: weigh 0.422 g K4Fe(CN)6·3H2Placing the O into a second magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the O is dissolved to obtain a solution B;
s3: pushing the solution A into the solution B through a peristaltic pump;
s4: standing and aging for 12 hours after uniform mixing to obtain white precipitate;
s5: washing the white precipitate for several times with washing liquid, and drying to obtain K2Zn3[Fe(CN)6]2A material.
In step S3, the second magnetic stirrer is always in a magnetic stirring state during the process of slowly pushing the solution a into the solution B through the peristaltic pump.
In step S5, the washing solution is deionized water and ethanol.
In step S5, the drying temperature was 60 ℃ and the drying time was 24 hours.
K prepared by the preparation method2Zn3[Fe(CN)6]2The crystalline material is in the form of tetragonal crystal particles of 1.0-2.5 microns.
Example 4
In this embodiment, a high quality K2Zn3[Fe(CN)6]2Process for preparing crystal from ZnSO4·7H2O as a zinc source, with K4Fe(CN)6·3H2Taking O as a single iron source, taking potassium citrate as a complexing agent, and preparing K by adopting a room-temperature coprecipitation method2Zn3[Fe(CN)6]2And (4) crystals.
Said one high quality K2Zn3[Fe(CN)6]2The preparation method of the crystal comprises the following steps:
s1: weighing 0.861g of ZnSO at room temperature4·7H2Mixing O and 1.30 g of potassium citrate, putting the mixture into a first magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the mixture is dissolved to obtain a solution A;
s2: weigh 0.844 g K4Fe(CN)6·3H2Placing the O into a second magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the O is dissolved to obtain a solution B;
s3: pushing the solution A into the solution B through a peristaltic pump;
s4: standing and aging for 12 hours after uniform mixing to obtain white precipitate;
s5: washing the white precipitate for several times with washing liquid, and drying to obtain K2Zn3[Fe(CN)6]2A material.
In step S3, the second magnetic stirrer is always in a magnetic stirring state during the process of slowly pushing the solution a into the solution B through the peristaltic pump.
In step S5, the washing solution is deionized water and ethanol.
In step S5, the drying temperature was 60 ℃ and the drying time was 24 hours.
K prepared by the preparation method2Zn3[Fe(CN)6]2The crystalline material is in the form of tetragonal crystal particles of 1.0-2.5 microns.
Example 5
Based on example 1, the high-quality K2Zn3[Fe(CN)6]2The application method of the crystal comprises the following steps:
d1: preparing a PVDF solution with the concentration of 40 mg/ml by taking N-methyl pyrrolidone as a solvent;
d2: according to the mass ratio of 6: 2: 2 will K2Zn3[Fe(CN)6]2Mixing and grinding the crystal material, the carbon black and the PVDF for one hour to prepare uniform slurry;
d3: coating the slurry on aluminum foil, drying at 60 deg.C, and vacuum drying at 120 deg.C for 12 hr;
d4: punching into an electrode plate with the diameter of 1.2 cm.
Said one high quality K2Zn3[Fe(CN)6]2The application method of the crystal further comprises the following steps:
d5: and (3) assembling by using metal potassium as a counter electrode and 2.5M KFSI in TEP as electrolyte to prepare the battery. The battery is a 2032 type button battery.
In step D5, the assembly is performed in a glove box.
To test the cathode material K2Zn3[Fe(CN)6]2The electrochemical performance of the prepared battery is 100 mAg-1The test was performed at current density and the first cycle discharge capacity was recorded, as well as the recorder capacity retention after 100 cycles.
The test shows that the discharge capacity of the first circle is 64.5mAhg-1As shown in fig. 7. After 100 cycles, the capacity retention rate was 91%. The lithium iron phosphate anode material is used as a positive electrode material of a potassium ion battery and shows excellent electrochemical performance.
In conclusion, K prepared by the invention2Zn3[Fe(CN)6]2The battery has excellent potassium storage performance, and the battery assembled by using the lithium iron phosphate as the anode material has the advantages of relatively high specific capacity, good rate capability and the like, and has wide application prospect.
It is noted that in the present disclosure, unless otherwise explicitly specified or limited, a first feature "on" or "under" a second feature may be directly contacted with the first and second features, or indirectly contacted with the first and second features through intervening media. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (7)
1. High-quality K2Zn3[Fe(CN)6]2The preparation method of the crystal is characterized in that ZnSO is used4·7H2O as a zinc source, with K4Fe(CN)6·3H2Taking O as a single iron source, taking potassium citrate as a complexing agent, and preparing K by adopting a room-temperature coprecipitation method2Zn3[Fe(CN)6]2And (4) crystals.
2. A high quality K according to claim 12Zn3[Fe(CN)6]2The preparation method of the crystal is characterized in that the complexing agent can be replaced by potassium pyrophosphate.
3. A high quality K according to claim 1 or 22Zn3[Fe(CN)6]2The preparation method of the crystal is characterized by comprising the following steps:
s1: weighing 0.287-0.861 g ZnSO at room temperature4·7H2Mixing O and 0.65-1.30 g of complexing agent, putting the mixture into a first magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the mixture is dissolved to obtain a solution A;
s2: weighing 0.422-0.844 g K4Fe(CN)6·3H2Placing the O into a second magnetic stirrer, adding 50 mL of deionized water, and magnetically stirring for 0.5 hour until the O is dissolved to obtain a solution B;
s3: pushing the solution A into the solution B through a peristaltic pump;
s4: standing and aging for 12 hours after uniform mixing to obtain white precipitate;
s5: use ofWashing the white precipitate with washing liquid for several times, and drying to obtain K2Zn3[Fe(CN)6]2A material.
4. A high quality K according to claim 32Zn3[Fe(CN)6]2The method for producing a crystal is characterized in that, in step S3, the second magnetic stirrer is kept in a state of magnetic stirring all the time while the solution a is being pushed into the solution B by the peristaltic pump.
5. A high quality K according to claim 42Zn3[Fe(CN)6]2The method for preparing the crystal is characterized in that in step S5, the washing solution is deionized water and ethanol.
6. A high quality K according to claim 52Zn3[Fe(CN)6]2A method for producing a crystal, characterized in that, in step S5, the drying temperature is 60 ℃ and the drying time is 24 hours.
7. A high quality K according to claim 62Zn3[Fe(CN)6]2The application method of the crystal is characterized by comprising the following steps:
d1: preparing a PVDF solution with the concentration of 40 mg/ml by taking N-methyl pyrrolidone as a solvent;
d2: according to the mass ratio of 6: 2: 2 will K2Zn3[Fe(CN)6]2Mixing and grinding the crystal material, the carbon black and the PVDF for one hour to prepare uniform slurry;
d3: coating the slurry on aluminum foil, drying at 60 deg.C, and vacuum drying at 120 deg.C for 12 hr;
d4: punching into an electrode plate with the diameter of 1.2 cm.
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| CN114768780A (en) * | 2022-05-25 | 2022-07-22 | 天津科技大学 | Preparation method and application of Zn-Fe Prussian blue analogue composite material |
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| CN107673371A (en) * | 2017-09-06 | 2018-02-09 | 华中科技大学 | Pyrophosphate aids in the preparation method of the Prussian blue similar thing of synthesized high-performance |
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| CN110002465A (en) * | 2019-03-29 | 2019-07-12 | 华中科技大学 | A kind of white analog positive electrode in Prussia, preparation method and application |
| CN113206224A (en) * | 2021-04-08 | 2021-08-03 | 华南理工大学 | Core-shell structure Prussian blue potassium ion battery positive electrode material modified by polymeric organic matters and preparation method thereof |
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| CN114768780A (en) * | 2022-05-25 | 2022-07-22 | 天津科技大学 | Preparation method and application of Zn-Fe Prussian blue analogue composite material |
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