CN113955814B - NiCl synthesized at low temperature 2 Powder and application - Google Patents
NiCl synthesized at low temperature 2 Powder and application Download PDFInfo
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Abstract
The invention relates to a low-temperature synthesized NiCl 2 Powder and application thereof, belonging to the technical field of powder preparation. The NiCl synthesized at low temperature 2 The powder is prepared from hydrated nickel chloride; uniformly mixing the raw materials and the extraction auxiliary agent in an organic solvent, drying, and calcining at 280-550 ℃ to obtain the compound; the extraction aid is chloride of transition metal element. The invention realizes that the pure phase NiCl is prepared under the condition of low temperature for the first time 2 . The preparation process has short period, low energy consumption and low cost. The product designed and prepared by the invention has the application fields of at least one of thermal batteries, super capacitors, lithium ion batteries and sodium ion batteries.
Description
Technical Field
The invention relates to a low-temperature synthesized NiCl 2 Powder and application thereof, belonging to the technical field of powder preparation.
Background
The thermal battery is widely applied to weapons and military devices as an output power supply due to the advantages of short activation time, high output energy, long storage time and the like. With the rapid development of modern weapons, higher demands are being placed on the performance index of long life, high power and rapid activation of thermal batteries. Transition metal halides have a high potential, a high specific energy and excellent thermal stability, and have been receiving a great deal of attention. Wherein NiCl 2 The potential of Li is up to 2.64V, and the theoretical specific capacity is up to 414mAhg -1 And has good thermal stability, and is a substitute for transition metal disulfide (FeS 2 、CoS 2 ) Becomes an ideal positive electrode material of the high-power thermal battery.
NiCl 2 In nature with nickel chloride hexahydrate (NiCl) 2 ·6H 2 O), niCl 2 ·6H 2 O is abundant in nature and low in cost, and can be obtained by dehydration treatmentAnhydrous NiCl 2 . Jin et al for NiCl at 870 DEG C 2 ·6H 2 O sublimates and recrystallises to obtain pure NiCl 2 The powder is then ball milled, sintered at 600 deg.c and other technological steps to obtain carbon coated NiCl 2 Composite material, test result shows that carbon coats NiCl 2 Has 641Wh kg -1 Specific energy (Jin et al Synthesis and discharge performances of NiCl) 2 by Surface modification of carbon coating as cathode material of thermal Battery.applied Surface Science,2017, 402:308-313). Guo Yong it is prepared from nickel chloride hexahydrate by air drying at 100-180deg.C and vacuum drying, treating at 600-900deg.C, scraping off black or black-green oxide layer, and pulverizing casting blank to obtain NiCl 2 Positive electrode active material (application publication number: CN 102157722 a). Liu et al used nickel chloride hexahydrate as the raw material, pre-dehydrated at 270 ℃, and then calcined at 600 ℃ for 5 hours to synthesize anhydrous NiCl 2 Tested, anhydrous NiCl 2 At 0.28Acm -2 At a current density of 243mAcm -2 Specific capacity of (Liu et al Variable-temperature preparation and performance ofNiCl) 2 as a cathode material for thermal bacteria.science China Materials,2017,60 (3): 251-257). Lin Xiaoxia by anhydrous NiCl 2 The powder is used as raw material, and anhydrous NiCl is prepared by chemical vapor deposition under inert gas protection 2 Sublimating, condensing and collecting NiCl with thickness of 2-20nm 2 A nano-sheet. In a thermal battery system formed by matching LiB alloy and ternary electrolyte (LiB-LiCl-LiBr) 2 The voltage peak value and specific energy of the nano sheet are higher than those of original anhydrous NiCl 2 (grant bulletin number: CN 109537053B). Luo Chongxiao mixing Raney Ni, naClO and surfactant in deionized water, filtering, drying, and mixing with NH 4 Mixing Cl uniformly, and roasting in a muffle furnace (roasting temperature is 400-500 ℃ and roasting time is 1-1.5 h) to obtain Raney Ni/NiCl 2 Composite positive electrode material (authorized bulletin number: CN 107492633B). In addition, niCl 2 In super powerContainer (Shinde et al Room-temperature Chemical Synthesis of 3-D Dandelion-type Nickel Chloride (NiCl) 2 @NiF) Supercapattery Nanostructured Materials, journal of Colloid and Interface Science,2020,578 (15): 547-554.) Na-ion battery (Gao et al high-Rate and Long-Life Intermediate-Temperature Na-NiCl) 2 Battery with Dual-Functional Ni-Carbon Composite nanosize network. ACS Applied Materials Interfaces,2020,12,24767-24776).
In the field of thermal battery applications, niCl has been reported to date 2 The synthesis process is high temperature synthesis or chemical synthesis. High temperature NiCl synthesis 2 High energy consumption, long preparation period, low purity, and extremely low chemical synthesis yield, which severely limits NiCl 2 Is a practical application of the above. Currently related to NiCl 2 The low-temperature synthesis process of (2) has not been reported, based on which a NiCl 2 A low temperature synthesis method of the powder is proposed in this context.
The invention combines liquid phase extraction and low temperature calcination technology to prepare anhydrous nickel chloride. By adding the extraction auxiliary agent, niCl is greatly reduced 2 The dehydration temperature and the discharge performance are obviously improved compared with those of high-temperature synthesized nickel chloride.
Disclosure of Invention
The invention aims at the problems and designs a NiCl 2 The low-temperature powder synthesis method greatly reduces NiCl by solvent extraction 2 Is used for the dehydration temperature of the water-absorbing material. Relative to traditional high temperature preparation of NiCl 2 The method has the advantages of simple preparation process and step, low energy consumption, low cost and the like. NiCl synthesized at low temperature 2 The thermal stability is excellent, the conductivity is good, and the thermal battery is suitable for the high-temperature discharge environment of the thermal battery.
The invention relates to NiCl synthesized at low temperature 2 Powder of NiCl synthesized at low temperature 2 The powder is prepared from hydrated nickel chloride; uniformly mixing the raw materials and the extraction auxiliary agent in an organic solvent, drying, and calcining at 280-550 ℃ after drying to obtain the compound; the extraction aid is chloride of transition metal element.
The invention relates to NiCl synthesized at low temperature 2 Powder, niCl obtained 2 Is single-phase NiCl 2 。
As a preferred embodiment; the invention relates to NiCl synthesized at low temperature 2 The preparation process of the powder comprises the following steps:
(1) Weighing nickel chloride hydrate and an extraction aid, wherein the extraction aid is 1-30at%, preferably 3-20at% of nickel chloride hydrate, dissolving the nickel chloride hydrate and the extraction aid in an alcohol and/or ether organic solvent, and uniformly stirring;
(2) Placing the solution in a drying oven at 80-180deg.C for at least 2 hr under atmospheric environment or vacuum;
(3) Calcining the dried powder in a muffle furnace at 280-550deg.C, preferably 300-450deg.C, and cooling to obtain pure phase NiCl 2 。
As a further preferred embodiment; in the step (1), the nickel chloride hydrate is NiCl 2 ·6H 2 O。
As a further preferred embodiment; in step (1), the extraction aid is selected from CrCl 3 ·6H 2 O、CoCl 3 、CoCl 2 ·6H 2 O、FeCl 2 ·4H 2 O、FeCl 3 ·6H 2 O、FeCl 3 、CuCl、CuCl 2 、CuCl 2 ·2H 2 O、ZnCl 2 Preferably copper chloride and/or cobalt chloride.
As a further preferred embodiment; in the step (1), the organic solvent is absolute ethyl alcohol.
As a preferred embodiment; the invention relates to NiCl synthesized at low temperature 2 The powder, the drying time in step (2) is 2-40h.
As a preferred embodiment; the invention relates to NiCl synthesized at low temperature 2 Calcining the powder for 2-6h in the step (3), and cooling after calcining to obtain pure-phase NiCl 2 。
The invention relates to NiCl synthesized at low temperature 2 Powder of NiCl 2 The decomposition temperature of the powder is 700-970 ℃.
The invention relates to NiCl synthesized at low temperature 2 The application of the powder comprises the steps of 2 The powder is used in at least one technical field of thermal batteries, super capacitors, lithium ion batteries and sodium ion batteries.
The invention relates to NiCl synthesized at low temperature 2 Application of the powder, niCl prepared 2 The powder was used as a thermal battery positive electrode material.
Drawings
Figure 1 is an XRD pattern of the product obtained in example 1.
FIG. 2 is a graph showing the high temperature discharge curve of the product obtained in example 1.
Figure 3 is an XRD pattern for the product obtained in example 2.
FIG. 4 is a high temperature discharge curve of the product obtained in example 2.
Figure 5 is an XRD pattern for the product obtained in example 3.
FIG. 6 is a high temperature discharge curve of the product obtained in example 3.
Figure 7 is an XRD pattern of the product obtained in example 4.
FIG. 8 is a high temperature discharge curve of the product obtained in example 4.
Figure 9 is an XRD pattern for the product obtained in example 5.
FIG. 10 is a high temperature discharge curve of the product obtained in example 5.
FIG. 11 is an XRD pattern of the product obtained in comparative example 1.
FIG. 12 is a graph showing the high temperature discharge curve of the product obtained in comparative example 1.
FIG. 13 is an XRD pattern of the product obtained in comparative example 2.
FIG. 14 is a high temperature discharge curve of the product obtained in comparative example 2.
Figure 15 is an XRD pattern for the product obtained in comparative example 3.
FIG. 16 is a graph showing the high temperature discharge curve of the product obtained in comparative example 3.
Example 1
(1) Weighing one part of raw material NiCl 2 ·6H 2 O and one part of extraction auxiliary CuCl 2 ·2H 2 O, wherein the extraction auxiliary agent is 5at percent of the raw materials, the extraction auxiliary agent and the raw materials are dissolved in absolute ethyl alcohol,stirring uniformly, wherein the mass of the absolute ethyl alcohol is 4 times of that of the raw materials.
(2) The solution is placed in a drying oven, the drying temperature is 100 ℃, the drying time is 8 hours, and the drying environment is the atmosphere.
(3) Calcining the product obtained in the step (2) in a muffle furnace, wherein the calcining temperature is 300 ℃, and the heating rate is 10 ℃ min -1 Calcination time was 3h. And (5) taking out the sample after the muffle furnace is cooled to room temperature, scraping off the surface product, and sealing and storing the residual product.
XRD analysis showed that NiCl prepared by the above procedure 2 Can well correspond to anhydrous NiCl 2 Is a single-phase structure (fig. 1).
(4) The obtained NiCl 2 The powder is matched with LiB negative electrode and LiF-LiCl-LiBr diaphragm to be assembled into a monomer thermal battery system which is 100mA cm in length -2 Discharging at 500 ℃ below zero, and the cut-off voltage is 2.0V.
The test results showed (FIG. 2) that NiCl was obtained by the above procedure 2 The voltage peak value of (2.50V) and the specific capacity of 229mAhg -1 Specific energy of 553Whkg -1 。
Example 2
(1) Weighing one part of raw material NiCl 2 ·6H 2 O and one part of extraction auxiliary CuCl 2 ·2H 2 And O, wherein the extraction auxiliary agent is 15at percent of the raw materials, the extraction auxiliary agent and the raw materials are dissolved in absolute ethyl alcohol, and the mass of the absolute ethyl alcohol is 4 times of that of the raw materials after the extraction auxiliary agent and the raw materials are uniformly stirred.
(2) The solution is placed in a drying oven, the drying temperature is 80 ℃, the drying time is 16 hours, and the drying environment is the atmosphere.
(3) Calcining the product obtained in the step (2) in a muffle furnace, wherein the calcining temperature is 350 ℃, and the heating rate is 5 ℃ min -1 Calcination time was 6h. And (5) taking out the sample after the muffle furnace is cooled to room temperature, scraping off the surface product, and sealing and storing the residual product.
XRD analysis showed that NiCl prepared by the above procedure 2 Can well correspond to anhydrous NiCl 2 Is a single-phase structure (fig. 3).
(4) Will be spentThe obtained NiCl 2 The powder is matched with LiB negative electrode and LiF-LiCl-LiBr diaphragm to be assembled into a monomer thermal battery system which is 100mA cm in length -2 Discharging at 500 ℃ below zero, and the cut-off voltage is 2.0V.
The test results showed (FIG. 4) that NiCl was obtained by the above procedure 2 The voltage peak value of (2.49V) and the specific capacity of 235mAhg -1 Specific energy of 561W h kg -1 。
Example 3
(1) Weighing one part of raw material NiCl 2 ·6H 2 O and one part of extraction auxiliary CuCl, wherein the extraction auxiliary is 3at percent of the raw materials, the extraction auxiliary and the extraction auxiliary are dissolved in absolute ethyl alcohol, and the mass of the absolute ethyl alcohol is 4.5 times of that of the raw materials.
(2) The solution is placed in a drying oven, the drying temperature is 100 ℃, the drying time is 12 hours, and the drying environment is the atmosphere.
(3) Calcining the product obtained in the step (2) in a muffle furnace, wherein the calcining temperature is 400 ℃, and the heating rate is 10 ℃ min -1 Calcination time was 3h. And (5) taking out the sample after the muffle furnace is cooled to room temperature, scraping off the surface product, and sealing and storing the residual product.
XRD analysis showed that NiCl prepared by the above procedure 2 Can well correspond to anhydrous NiCl 2 Is a single-phase structure (fig. 5).
(4) The obtained NiCl 2 The powder is matched with LiB negative electrode and LiF-LiCl-LiBr diaphragm to be assembled into a monomer thermal battery system which is 500mA cm in length -2 Discharging at 500 ℃ below zero, and the cut-off voltage is 1.8V.
The test results showed (FIG. 6), niCl obtained by the above procedure 2 The voltage peak of (2.29V) and the specific capacity of 327mAhg -1 Specific energy of 724Whkg -1 。
Example 4
(1) Weighing one part of raw material NiCl 2 ·6H 2 O and one part of extraction auxiliary CoCl 2 ·6H 2 And O, wherein the extraction auxiliary agent is 10at percent of the raw materials, the extraction auxiliary agent and the raw materials are dissolved in absolute ethyl alcohol, and the mass of the absolute ethyl alcohol is 3.5 times of that of the raw materials through uniform stirring.
(2) The solution is placed in a drying oven, the drying temperature is 120 ℃, the drying time is 10 hours, and the drying environment is the atmosphere.
(3) Calcining the product obtained in the step (2) in a muffle furnace, wherein the calcining temperature is 500 ℃, and the heating rate is 5 ℃ min -1 Calcination time was 3h. And (5) taking out the sample after the muffle furnace is cooled to room temperature, scraping off the surface product, and sealing and storing the residual product.
XRD analysis showed that NiCl prepared by the above procedure 2 Can well correspond to anhydrous NiCl 2 Is a single-phase structure (fig. 7).
(4) The obtained NiCl 2 The powder is matched with LiB negative electrode and LiF-LiCl-LiBr diaphragm to be assembled into a monomer thermal battery system which is 100mA cm in length -2 Discharging at 500 ℃ below zero, and the cut-off voltage is 2.0V.
The test results showed (FIG. 8), niCl obtained by the above procedure 2 The voltage peak of (2.48V) and the specific capacity of 216mAhg -1 Specific energy of 505 Wh kg -1 。
Example 5
(1) Weighing one part of raw material NiCl 2 ·6H 2 O and one part of extraction auxiliary FeCl 3 ·6H 2 And O, wherein the extraction auxiliary agent is 5at percent of the raw material, the extraction auxiliary agent and the raw material are dissolved in absolute ethyl alcohol, and the mass of the absolute ethyl alcohol is 3.8 times of that of the raw material.
(2) The solution is placed in a drying oven, the drying temperature is 100 ℃, the drying time is 12 hours, and the drying environment is the atmosphere.
(3) Calcining the product obtained in the step (2) in a muffle furnace, wherein the calcining temperature is 300 ℃, and the heating rate is 5 ℃ min -1 Calcination time was 3h. And (5) taking out the sample after the muffle furnace is cooled to room temperature, scraping off the surface product, and collecting the residual product.
XRD analysis showed that NiCl prepared by the above procedure 2 Can well correspond to anhydrous NiCl 2 Is a single-phase structure (fig. 9).
(4) The obtained NiCl 2 Powder and LiB negative electrode, liF-LiCl-LiBr diaphragm are matched and assembled into monomer heatBattery system and at 100mA cm -2 Discharging at 500 ℃ below zero, and the cut-off voltage is 2.0V.
The test results showed (FIG. 10) that NiCl was obtained by the above procedure 2 The voltage peak value of (2.41V) and the specific capacity of (206 mAhg) -1 Specific energy of 474 Wh kg -1 。
Comparative example 1
(1) Weighing one part of raw material NiCl 2 ·6H 2 O and one part of extraction auxiliary CuCl 2 ·2H 2 And O, wherein the extraction auxiliary agent is 30at percent of the raw materials, the extraction auxiliary agent and the raw materials are dissolved in absolute ethyl alcohol, and the mass of the absolute ethyl alcohol is 4 times of that of the raw materials after the extraction auxiliary agent and the raw materials are uniformly stirred.
(2) The solution is placed in a drying oven, the drying temperature is 100 ℃, the drying time is 8 hours, and the drying environment is the atmosphere.
(3) Calcining the product obtained in the step (2) in a muffle furnace, wherein the calcining temperature is 300 ℃, and the heating rate is 10 ℃ min -1 Calcination time was 3h. And (5) taking out the sample after the muffle furnace is cooled to room temperature, scraping off the surface product, and sealing and storing the residual product.
XRD analysis showed that NiCl prepared by the above procedure 2 Can better correspond to anhydrous NiCl 2 A small amount of clutter was generated for the standard PDF card of (fig. 11).
(4) The obtained NiCl 2 The powder is matched with LiB negative electrode and LiF-LiCl-LiBr diaphragm to be assembled into a monomer thermal battery system which is 100mA cm in length -2 Discharging at 500 ℃ below zero, and the cut-off voltage is 2.0V.
The test results showed (FIG. 12) that NiCl was obtained by the above procedure 2 The voltage peak value of (2.52V) and the specific capacity of (168) mAhg -1 Specific energy of 399 Wh kg -1 。
Comparative example 2
(1) Weighing one part of raw material NiCl 2 ·6H 2 O, no extraction auxiliary agent is added, the raw materials are dissolved in absolute ethyl alcohol, and the absolute ethyl alcohol is stirred uniformly, wherein the mass of the absolute ethyl alcohol is 4.2 times of that of the raw materials.
(2) The solution is placed in a drying oven, the drying temperature is 120 ℃, the drying time is 16 hours, and the drying environment is the atmosphere.
(3) Calcining the product obtained in the step (2) in a muffle furnace, wherein the calcining temperature is 600 ℃, and the heating rate is 10 ℃ min -1 Calcination time was 3h. And (5) taking out the sample after the muffle furnace is cooled to room temperature, scraping off the surface product, and sealing and storing the residual product.
XRD analysis showed that NiCl prepared by the above procedure 2 Can well correspond to anhydrous NiCl 2 Is a single-phase structure (fig. 13).
(4) The obtained NiCl 2 The powder is matched with LiB negative electrode and LiF-LiCl-LiBr diaphragm to be assembled into a monomer thermal battery system which is 200mA cm in length -2 Discharging at 500 ℃ below zero, and the cut-off voltage is 2.0V.
The test results showed (FIG. 14) that NiCl was obtained by the above procedure 2 The voltage peak of (2.52V) and the specific capacity of 206mAhg -1 Specific energy of 467 Wh kg -1 。
Comparative example 3
(1) Weighing one part of raw material NiCl 2 ·6H 2 O, no extraction auxiliary agent is added, the raw materials are dissolved in absolute ethyl alcohol, and the absolute ethyl alcohol is stirred uniformly, wherein the mass of the absolute ethyl alcohol is 4.2 times of that of the raw materials.
(2) The solution is placed in a drying oven, the drying temperature is 120 ℃, the drying time is 16 hours, and the drying environment is the atmosphere.
(3) Calcining the product obtained in the step (2) in a muffle furnace, wherein the calcining temperature is 300 ℃, and the heating rate is 5 ℃ min -1 Calcination time was 3h. And (5) taking out the sample after the muffle furnace is cooled to room temperature, scraping off the surface product, and sealing and storing the residual product.
XRD analysis showed that NiCl prepared by the above procedure 2 Poor crystallinity, and is not suitable for anhydrous NiCl 2 Standard PDF card of (fig. 15).
(4) The obtained NiCl 2 The powder is matched with LiB negative electrode and LiF-LiCl-LiBr diaphragm to be assembled into a monomer thermal battery system which is 100mA cm in length -2 Discharging at 500 ℃ below zero, and the cut-off voltage is 2.0V.
The test results show (FIG. 16) that by the above stepsObtaining NiCl 2 The voltage peak value of (2.32V) and the specific capacity of 24mAhg -1 Specific energy of 52Whkg -1 。
Claims (5)
1. NiCl synthesized at low temperature 2 Powder, its characterized in that: the preparation process comprises the following steps:
(1) Weighing nickel chlorohydrate and an extraction auxiliary agent, wherein the extraction auxiliary agent is 1-20at% of nickel chlorohydrate, dissolving the nickel chlorohydrate and the extraction auxiliary agent in an organic solvent, and uniformly stirring;
(2) Placing the above solution in a drying oven at 80-180deg.C for at least 2h under atmospheric environment or vacuum;
(3) Calcining the dried powder in a muffle furnace at 280-550 ℃ for 2-6h, and cooling to obtain pure-phase NiCl 2 ；
In the step (1), the nickel chloride hydrate is NiCl 2 ·6H 2 O；
In the step (1), the extraction auxiliary agent is CuCl;
in the step (1), the organic solvent is absolute ethyl alcohol.
2. A low temperature synthetic NiCl according to claim 1 2 Powder, its characterized in that: the drying time in step (2) is 2-40h.
3. A low temperature synthetic NiCl according to any one of claims 1-2 2 Powder, its characterized in that: the obtained NiCl 2 The decomposition temperature of the powder is 700-970 ℃.
4. A low temperature synthetic NiCl according to any one of claims 1-2 2 The use of a powder characterized in that: comprises the steps of NiCl 2 The powder is used in at least one technical field of thermal batteries, super capacitors, lithium ion batteries and sodium ion batteries.
5. A cryogenically synthesized N according to claim 4iCl 2 The use of a powder characterized in that: niCl prepared 2 The powder was used as a thermal battery positive electrode material.
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