CN109860593A - A kind of Iron nickel sulphide and preparation method thereof and the sodium-ion battery that cathode is made of it - Google Patents
A kind of Iron nickel sulphide and preparation method thereof and the sodium-ion battery that cathode is made of it Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of Iron nickel sulphide, according to mass ratio 1:(1~3): (1~7) takes iron acylate, nickel nitrate and carbon nitrogen source organic matter, obtains mixture A after mixed grinding；Mixture A is heat-treated 1h~5h at 500 DEG C~1200 DEG C, is taken out after cooling, obtains product B, according to mass ratio is 1:(5~10 by product B and sulphur source) after mixed grinding is uniform, obtain mixture C；Mixture C is heat-treated 30min~1h at 300 DEG C~600 DEG C, is taken out after cooling, product D, i.e. Iron nickel sulphide, Iron nickel sulphide prepared by the present invention, the calabash shaped structure of the active particle with continuous carbon-coating cladding are obtained；Active particle in the structure can keep nano-scale in charge and discharge process; the carbon nano tube structure of cladding can protection materials expansion process; make the structure remained stable of active material; graphited carbon nano tube structure can provide the conductive path of high speed, and present invention gained Iron nickel sulphide can also be used as the cathode of sodium-ion battery.
Description
Technical field
The invention belongs to composite materials to synthesize field, and in particular to a kind of Iron nickel sulphide and preparation method thereof further relates to
A kind of sodium-ion battery using Iron nickel sulphide as cell negative electrode material.
Background technique
In recent years, widely distributed in the earth and rich reserves due to sodium element, room temperature sodium ion charge-discharge battery are ground
Hair have been considered as substituting lithium ion battery in the fields such as extensive energy storage, especially smart grid, with effectively solve lithium from
Sub- battery mineral lay in the low and high cost problem of lithium source effective way.In numerous anode material of lithium-ion battery systems, carbon,
The alloy-types material such as metal oxide or sulfide and Sn, Sb is a few class material systems that scholars most pay close attention to.Wherein, golden
Belong to sulfide due to theoretical capacity with higher, it is resourceful, it is potential sodium ion the advantages that low toxicity, electric conductivity is preferable
The negative electrode material of battery.Wherein iron sulfide is as sodium ion battery electrode material, is that a kind of stabilization, nontoxic and preparation are simple honest and clean
Valence material has high theoretical embedding sodium capacity (894mAh/g) and volume and capacity ratio (2950mAh/cm3).However, iron sulfide is conductive
Property is not high, low with the interface compatibility of organic electrolyte is poor, electrode material microscopic dimensions are big, effective charge and discharge active site utilization rate
Deficiency greatly hinder its electrochemistry storage sodium ability.Simultaneously as iron sulfide resistivity is larger, voltage declines when electric discharge
Comparatively fast, serious polarization phenomena can be especially generated in high-rate battery discharge, greatly shorten the working life of battery.Therefore,
Circulation volume and sustainability of the iron sulfide as negative electrode material in sodium-ion battery are promoted, is needed to be studied at present
Direction.
Summary of the invention
In order to solve problems of the prior art, the present invention provide a kind of Iron nickel sulphide and preparation method thereof and
The sodium-ion battery of cathode is made of it, the high capacity of the preparation method combination iron sulfide nickel material, be readily synthesized, preparation cost it is low
Have the function of that concerted catalysis carbon graphiteization forms carbon pipe with ferronickel, by heat treatment process, under the effect of iron nickel co-catalysis
Carbon nanotube coated particle structure is formed, nano composite structure is formed with the anode material of lithium-ion battery formed, significantly improves
The electrochemistry of iron sulfide negative electrode material stores up sodium performance.
To achieve the goals above, the technical solution adopted by the present invention is that, a kind of preparation method of Iron nickel sulphide, including
Following steps:
Step 1, according to mass ratio 1:(1~3): (1~7) takes iron acylate, nickel nitrate and carbon nitrogen source organic matter, mixing
Mixture A is obtained after grinding；
Step 2, mixture A is heat-treated to 1h~5h at 500 DEG C~1200 DEG C, is taken out after cooling, obtains product B,
Step 3, it is 1:(5~10 according to mass ratio by product B and sulphur source) after mixed grinding is uniform, obtain mixture C；
Step 4, mixture C is heat-treated to 30min~1h at 300 DEG C~600 DEG C, is taken out after cooling, obtains product D,
That is Iron nickel sulphide.
In step 1, iron acylate is pure using analyzing, and iron acylate includes ironic citrate, ferric oxalate or ferric acetate.
In step 1, carbon nitrogen source organic matter includes urea, melamine, carbodiimide, cyanuric acid or trithiocyanuric acid.
In step 1, milling time is half an hour.
In step 2, heat treatment heating rate is 2 DEG C/min~20 DEG C/min, furnace cooling.
In step 3, sulphur source is using one or more of sublimed sulfur, thioacetamide or trithiocyanuric acid.
In step 4, heat treatment heating rate is 5 DEG C/min~10 DEG C/min, furnace cooling.
Use the Iron nickel sulphide particle of above-mentioned preparation method preparation for continuous carbon-coating coated particle structure.
Another scheme of the invention is to prepare a kind of sodium-ion battery, using Iron nickel sulphide of the present invention as sodium
The negative electrode material of ion battery, Iron nickel sulphide keep nano-grade size in charge and discharge process.
Compared with prior art, the present invention at least has the advantages that the present invention prepares iron using two-step synthesis method
Nickel sulfide composite material, preparation method simple and stable, repeatability is strong, and low in raw material price can significantly reduce existing document
The preparation cost of the material of report；
Ferronickel has the function of that concerted catalysis carbon graphiteization forms carbon pipe, and during heat treatment, iron nickel co-catalysis is made
With lower formation carbon nanotube coated particle structure, anode material of lithium-ion battery of the nano composite structure to be formed is formed, significantly
The electrochemistry for improving iron sulfide negative electrode material stores up sodium performance；
Iron nickel sulphide prepared by the present invention, the active particle with continuous carbon-coating cladding are calabash shaped structure；The knot
Active particle in structure can keep nano-scale in charge and discharge process, the carbon nano tube structure of cladding can protection materials it is swollen
Swollen process, makes the structure remained stable of active material, and graphited carbon nano tube structure can provide the conductive path of high speed, make material
Material shows excellent high rate performance.
Detailed description of the invention
Fig. 1 is the XRD diagram of iron nickel bimetal sulfide.
Fig. 2 is the stereoscan photograph of iron sulfide nickel composite.
Fig. 3 is bimetallic Iron nickel sulphide charge-discharge performance figure.
Fig. 4 is the transmission plot of iron sulfide nickel composite.
Fig. 5 is bimetallic Iron nickel sulphide circulation figure.
Specific embodiment
With reference to the accompanying drawing and the present invention is further explained in detail in embodiment.
1) analytically pure iron acylate, nickel nitrate, carbon nitrogen organic compound are taken, in glass mortar after mixed grinding
To mixture, the mass ratio of source of iron and nickel source, organic compound is 1:(1~3 in mixture): (1~7), the mixture are denoted as
A；Iron acylate uses ironic citrate, ferric oxalate or ferric acetate；The organic matter is urea, melamine, carbodiimide, three
Paracyanogen acid or trithiocyanuric acid；
2) mixture A is heat-treated in low temperature tube furnace, in reaction process, iron nickel raw material co-catalysis carbon source forms iron
Nickel separates particle outer cladding carbon tube structure, takes out after cooling, obtains product B, heat treatment heating rate be 2 DEG C/min~
20 DEG C/min, heat treatment temperature is 500~1200 DEG C, and the time is 1h~5h；
3) product B and sulphur source are obtained into mixture in glass mortar after mixed grinding, the mass ratio of product B and sulphur source is
1:(5~10), which is denoted as C；The sulphur source can be sublimed sulfur, thioacetamide or trithiocyanuric acid；
4) mixture C is heat-treated in low temperature tube furnace again, heat treatment heating rate is 5~10 DEG C/min, heat treatment
Temperature is 300~800 DEG C, and the time is 30min~1h, is taken out after cooling, obtains product D, i.e. the separation iron of continuous carbon pipe cladding
Nickel sulfide, calabash shaped structure.
Embodiment 1:
It is that prepare Iron nickel sulphide process as follows by 1:1:2 according to reactant quality ratio:
1) analytically pure ironic citrate 2g, nickel nitrate 2g, urea 4g is taken to be mixed after mixed grinding in glass mortar
Object A；
2) mixture A is warming up to 800 DEG C of heat preservation 3h in low temperature tube furnace with 2 DEG C/min, takes out, is produced after cooling
Object B；
3) sublimed sulfur of product B and its 5 times of quality is obtained into mixture C in glass mortar after mixed grinding；
4) mixture C is warming up to 400 DEG C of calcining 1h in low temperature tube furnace with 5 DEG C/min again, takes out, obtains after cooling
Product D, i.e. iron nickel bimetal sulfide nano-material.
Product, XRD such as Fig. 1 of 1 products therefrom of embodiment are analyzed using Rigaku D/max2000PCX- x ray diffractometer x
It is shown, from figure 1 it appears that product is iron nickel bimetal sulfide；Resulting product is prepared into button-shaped sodium ion electricity
Pond, specific encapsulation step are as follows: sodium ion half-cell will be assembled into after product direct slicing, using new prestige electrochemical operation
It stands and constant current charge-discharge test is carried out to battery, resulting materials are assembled into button cell and surveyed by test voltage 0.01V-3.0V
Its anode material of lithium-ion battery performance is tried, as shown in figure 3, battery presents 400mAh/g under the current density of 100mA/g
Capacity, circulation 100 circle after still with 300mAh/g or more capacity, it is seen that material have excellent cycle performance, such as Fig. 3
It is shown.
Embodiment 2:
It is that prepare Iron nickel sulphide process as follows by 1:1:3 according to reactant quality ratio:
1) analytically pure ferric oxalate 2g, nickel nitrate 2g, melamine 6g is taken to be mixed after mixed grinding in glass mortar
Object is closed, which is denoted as A；
2) mixture A is warming up to 500 DEG C of heat preservation 1h in low temperature tube furnace with 8 DEG C/min, takes out, is produced after cooling
Object B；
3) thioacetamide of product B and its 4 times of quality is obtained into mixture C in glass mortar after mixed grinding；
4) mixture C is warming up to 300 DEG C of calcining 0.5h in low temperature tube furnace with the rate of 6 DEG C/min again, after cooling
It takes out, obtains product D, i.e. iron nickel bimetal sulfide；
Fig. 2 is the high power stereoscan photograph of iron sulfide nickel composite, is scanned using the S-4800 type of Japan Electronics Corporation
Electron microscope (SEM) carries out morphology observation, it can be seen that its product random orientation dense growth, Fig. 4 are iron sulfide nickel composite
Transmission plot, it can be seen that its product be hollow coated, graphited carbon-coating is produced under the concerted catalysis of nickel and source of iron,
This structure can improve the stability and electric conductivity of material.
Embodiment 3:
It is that prepare Iron nickel sulphide process as follows by 1:1:1 according to reactant quality ratio:
1) analytically pure ferric acetate 2g, nickel nitrate 2g, carbodiimide 2g is taken to be mixed after mixed grinding in glass mortar
Object is closed, which is denoted as A；
2) mixture A is warming up to 900 DEG C of heat preservation 4h in low temperature tube furnace with 12 DEG C/min, takes out, obtains after cooling
Product B；
3) trithiocyanuric acid of product B and its 3 times of quality is obtained into mixture C in glass mortar after mixed grinding；
4) mixture C is warming up to 500 DEG C of calcining 0.5h in low temperature tube furnace with 8 DEG C/min again, takes out, obtains after cooling
To product D, i.e. iron nickel bimetal sulfide；
The sample must be tested by chemical property, high rate performance is as shown in figure 5, as shown in Figure 5, sample is in 5A/g
Charge-discharge velocity under can still keep storage sodium capacity close to 200mAh/g, have excellent performance, as anode material of lithium-ion battery
Great potential.
Embodiment 4:
It is that prepare Iron nickel sulphide process as follows by 1:3:7 according to reactant quality ratio:
1) analytically pure ferric oxalate 1g, nickel nitrate 3g, carbodiimide 7g is taken to be mixed after mixed grinding in glass mortar
Object is closed, which is denoted as A；
2) mixture A is warming up to 1200 DEG C of heat preservation 5h in low temperature tube furnace with 20 DEG C/min, takes out, obtains after cooling
Product B；
3) sublimed sulfur of product B and its 2 times of quality is obtained into mixture C in glass mortar after mixed grinding；
4) mixture C is warming up to 600 DEG C of calcining 1h in low temperature tube furnace with 10 DEG C/min again, takes out, obtains after cooling
To product D, i.e. iron nickel bimetal sulfide.
Embodiment 5:
It is that prepare Iron nickel sulphide process as follows by 1:2:4 according to reactant quality ratio:
1) analytically pure ironic citrate 1g, nickel nitrate 2g, urea 4g is taken to be mixed after mixed grinding in glass mortar
Object, the mixture are denoted as A；
2) mixture A is warming up to 600 DEG C of heat preservation 2h in low temperature tube furnace with 10 DEG C/min, takes out, obtains after cooling
Product B；
3) thioacetamide of product B and its 5 times of quality is obtained into mixture C in glass mortar after mixed grinding；
4) mixture C is warming up to 400 DEG C of calcining 1h in low temperature tube furnace with 6 DEG C/min again, takes out, obtains after cooling
Product D, i.e. iron nickel bimetal sulfide.
Embodiment 6:
It is that prepare Iron nickel sulphide process as follows by 1:3:6 according to reactant quality ratio:
1) analytically pure ferric acetate 1g, nickel nitrate 3g, urea 6g is taken to be mixed after mixed grinding in glass mortar
Object, the mixture are denoted as A；
2) mixture A is warming up to 700 DEG C of heat preservation 2h in low temperature tube furnace with 12 DEG C/min, takes out, obtains after cooling
Product B；
3) trithiocyanuric acid of product B and its 5 times of quality is obtained into mixture C in glass mortar after mixed grinding；
4) mixture C is warming up to 450 DEG C of calcining 0.5h in low temperature tube furnace with 7 DEG C/min again, takes out, obtains after cooling
To product D, i.e. iron nickel bimetal sulfide.
Embodiment 7:
It is that prepare Iron nickel sulphide process as follows by 1:2:3 according to reactant quality ratio:
1) analytically pure ironic citrate 1g, nickel nitrate 2g, carbodiimide 3g is taken to obtain after mixed grinding in glass mortar
Mixture, the mixture are denoted as A；
2) mixture A is warming up to 900 DEG C of heat preservation 1h in low temperature tube furnace with 15 DEG C/min, takes out, obtains after cooling
Product B；
3) trithiocyanuric acid of product B and its 4 times of quality is obtained into mixture C in glass mortar after mixed grinding；
4) mixture C is warming up to 350 DEG C of calcining 1h in low temperature tube furnace with 6 DEG C/min again, takes out, obtains after cooling
Product D, i.e. iron nickel bimetal sulfide.
Embodiment 8:
It is that prepare Iron nickel sulphide process as follows by 1:1:6 according to reactant quality ratio:
1) analytically pure ferric oxalate 1g, nickel nitrate 1g, urea 6g is taken to be mixed after mixed grinding in glass mortar
Object, the mixture are denoted as A；
2) mixture A is warming up to 1000 DEG C of heat preservation 1h in low temperature tube furnace with 20 DEG C/min, takes out, obtains after cooling
Product B；
3) trithiocyanuric acid of product B and its 4 times of quality is obtained into mixture C in glass mortar after mixed grinding；
4) mixture C is warming up to 300 DEG C of calcining 2h in low temperature tube furnace with 5 DEG C/min again, takes out, obtains after cooling
Product D, i.e. iron nickel bimetal sulfide.
Embodiment 9:
It is that prepare Iron nickel sulphide process as follows by 1:2:4 according to reactant quality ratio:
1) analytically pure ironic citrate 1g, nickel nitrate 2g, melamine 4g is taken to obtain after mixed grinding in glass mortar
Mixture, the mixture are denoted as A；
2) mixture A is warming up to 650 DEG C of heat preservation 3h in low temperature tube furnace with 5 DEG C/min, takes out, is produced after cooling
Object B；
3) trithiocyanuric acid of product B and its 2 times of quality is obtained into mixture C in glass mortar after mixed grinding；
4) mixture C is warming up to 400 DEG C of calcining 3h in low temperature tube furnace with 6 DEG C/min again, takes out, obtains after cooling
Product D, i.e. iron nickel bimetal sulfide.
Claims (10)
1. a kind of preparation method of Iron nickel sulphide, which comprises the following steps:
Step 1, according to mass ratio 1:(1~3): (1~7) takes iron acylate, nickel nitrate and carbon nitrogen source organic matter, mixed grinding
After obtain mixture A；
Step 2, mixture A is heat-treated to 1h~5h at 500 DEG C~1200 DEG C, is taken out after cooling, obtains product B,
Step 3, it is 1:(5~10 according to mass ratio by product B and sulphur source) after mixed grinding is uniform, obtain mixture C；
Step 4, mixture C is heat-treated to 30min~1h at 300 DEG C~600 DEG C, is taken out after cooling, obtains product D, i.e. iron
Nickel sulfide.
2. the preparation method of Iron nickel sulphide according to claim 1, which is characterized in that in step 1, iron acylate is adopted
Pure with analyzing, iron acylate includes ironic citrate, ferric oxalate or ferric acetate.
3. the preparation method of Iron nickel sulphide according to claim 1, which is characterized in that in step 1, carbon nitrogen source organic matter
Including urea, melamine, carbodiimide, cyanuric acid or trithiocyanuric acid.
4. the preparation method of Iron nickel sulphide according to claim 1, which is characterized in that in step 1, milling time is half
Hour.
5. the preparation method of Iron nickel sulphide according to claim 1, which is characterized in that in step 2, heat treatment heating speed
Rate is 2 DEG C/min~20 DEG C/min, furnace cooling.
6. the preparation method of Iron nickel sulphide according to claim 1, which is characterized in that in step 3, sulphur source is using distillation
One or more of sulphur, thioacetamide or trithiocyanuric acid.
7. the preparation method of Iron nickel sulphide according to claim 1, which is characterized in that in step 4, heat treatment heating speed
Rate is 5 DEG C/min~10 DEG C/min, furnace cooling.
8. a kind of Iron nickel sulphide of the preparation of the preparation method as described in claim 1~7, which is characterized in that Iron nickel sulphide
Grain is continuous carbon-coating coated particle structure.
9. a kind of sodium-ion battery, which is characterized in that cell negative electrode material uses Iron nickel sulphide according to any one of claims 8.
10. sodium-ion battery according to claim 9, Iron nickel sulphide keep nano-grade size in charge and discharge process.
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| CN110224126A (en) * | 2019-06-14 | 2019-09-10 | 陕西科技大学 | A kind of Iron nickel sulphide nano material and its preparation method and application |
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| CN111900385A (en) * | 2020-07-29 | 2020-11-06 | 肇庆市华师大光电产业研究院 | Novel negative electrode material of potassium ion battery and preparation method thereof |
| CN112408496A (en) * | 2020-11-09 | 2021-02-26 | 邵阳学院 | Nitrogen and sulfur co-doped carbon @ FeS nanotube and preparation method and application thereof |
| CN113224303A (en) * | 2021-05-08 | 2021-08-06 | 陕西科技大学 | Preparation method of iron cyanamide material for realizing graphitized carbon coating by in-situ autocatalysis |
| CN113548700A (en) * | 2021-07-26 | 2021-10-26 | 河南师范大学 | Preparation method of iron-nickel-nitrogen-carbon nano material |
| CN113793760A (en) * | 2021-08-19 | 2021-12-14 | 江苏工程职业技术学院 | Preparation method of one-step electro-deposition nickel-iron sulfide nano composite electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110224126A (en) * | 2019-06-14 | 2019-09-10 | 陕西科技大学 | A kind of Iron nickel sulphide nano material and its preparation method and application |
| CN111312999A (en) * | 2020-02-20 | 2020-06-19 | 肇庆市华师大光电产业研究院 | Preparation method of graphene-coated nickel-iron bimetallic sulfide sodium-ion battery negative electrode material |
| CN111900385A (en) * | 2020-07-29 | 2020-11-06 | 肇庆市华师大光电产业研究院 | Novel negative electrode material of potassium ion battery and preparation method thereof |
| CN111900385B (en) * | 2020-07-29 | 2022-04-26 | 肇庆市华师大光电产业研究院 | Novel negative electrode material of potassium ion battery and preparation method thereof |
| CN112408496A (en) * | 2020-11-09 | 2021-02-26 | 邵阳学院 | Nitrogen and sulfur co-doped carbon @ FeS nanotube and preparation method and application thereof |
| CN113224303A (en) * | 2021-05-08 | 2021-08-06 | 陕西科技大学 | Preparation method of iron cyanamide material for realizing graphitized carbon coating by in-situ autocatalysis |
| CN113548700A (en) * | 2021-07-26 | 2021-10-26 | 河南师范大学 | Preparation method of iron-nickel-nitrogen-carbon nano material |
| CN113793760A (en) * | 2021-08-19 | 2021-12-14 | 江苏工程职业技术学院 | Preparation method of one-step electro-deposition nickel-iron sulfide nano composite electrode |
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