CN111129533B - Application of cuprous oxide - Google Patents

Application of cuprous oxide Download PDF

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CN111129533B
CN111129533B CN201811387794.6A CN201811387794A CN111129533B CN 111129533 B CN111129533 B CN 111129533B CN 201811387794 A CN201811387794 A CN 201811387794A CN 111129533 B CN111129533 B CN 111129533B
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thermal battery
anode material
electrode
cuprous oxide
powder
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CN111129533A (en
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符立才
罗泽顺吉
周灵平
朱家俊
杨武霖
李德意
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Hunan University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M6/00—Primary cells; Manufacture thereof
    • H01M6/30—Deferred-action cells
    • H01M6/36—Deferred-action cells containing electrolyte and made operational by physical means, e.g. thermal cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides

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Abstract

The invention relates to an application of cuprous oxide; in particular to a novel thermal battery using cuprous oxide as a positive electrode material; belongs to the technical field of electrochemistry. The invention uses cuprous oxide as the anode material of the thermal battery for the first time. The thermal battery discharge system is made of Cu2O electrode, negative electrode, and separator. Cu2When used as an electrode material, O has high thermal stability and electrical conductivity, higher working voltage and higher specific capacity. The Cu with different grain diameters and different shapes2The O electrode can discharge at one time in a large current mode, and the current density can be 1-1000 mA cm‑2(ii) a The discharge temperature is high and is 340-700 ℃. While Cu of the present invention2The O electrode is simple to prepare and low in cost; the actual specific capacity is high, the effective discharge time is long, the discharge performance is excellent, and the industrial application is convenient.

Description

Application of cuprous oxide
Technical Field
The invention relates to an application of cuprous oxide; in particular to a novel thermal battery using cuprous oxide as a positive electrode material; belongs to the technical field of electrochemistry.
1 background of the invention
Thermal cells are primary cells that use solid molten salt as the electrolyte and use an internal source of smoke and fire to bring the stack to operating temperature. The three major components of the thermal battery are a positive electrode, an electrolyte and a negative electrode. The thermal battery has the remarkable characteristics of short activation time, long service life, high specific energy, high specific power, long storage time and the like, and is widely applied to explosive projectile fuse power supplies, working power supplies of missiles and nuclear weapons, emergency power supplies of aerospace and underground mining industries and the like. With the successful research and development of novel cathodes such as LiB alloy and the like and multi-element electrolytes such as LiF-LiCl-LiBr and the like, the cathodes and the electrolytes can meet the discharge requirements of thermal batteries. However, the positive electrode material is always a key factor for preventing the discharge performance of the thermal battery from being improved.
Cu2O is a novel p-type semiconductor material, has active hole-electron pairs and good catalytic activity, and is widely applied to photocatalysis, solar cells, lithium ion batteries and the like.Chinese patent CN 105803500B discloses petal-shaped Cu2O, preparation method and application thereof, and the method is characterized in that the construction of the ultraviolet light-excited photocatalytic fuel cell and the realization of petal-shaped Cu2The deposition of O on conductive glass and the dual conversion of light and chemical energy into electrical energy. The method of anode oxidation of Jingshan Luo et al produces Cu (OH) on Cu foil2Then putting the alloy into an argon atmosphere for annealing to form Cu2O nanowire and depositing a thin Cu layer on the Cu substrate2Excellent capacity of producing hydrogen by photo-hydrolysis after O (Jingshan Luo, Ludmilla Steier, Min-Kyu Son, Marcel Schreier, Matthew T.Mayer, and Michael)
Figure BDA0001873313690000011
Cu2O Nanowire Photocathodes for Efficient and Durable Solar Water Splitting[J].Nano Letters.16,3:1848-1857)。Cu2O differs in catalysis and conductivity due to the difference in crystal exposure. Huang et al studied Cu with exposed surfaces of (100), (111) and (110)2O, their morphologies were cubic, octahedral and rhombohedral, respectively, and Cu was found2The catalytic performance, the conductivity and the like of O have crystal face selectivity: the rhombohedral dodecahedron with the exposed surface of (110) exhibits the best catalytic performance at 25 to 40 ℃; cu2The (100) side of O is non-conductive and (111) has high conductivity (Michael H.Huang, sourvav Rej and Shih-Chen Hsu, Facet-dependent properties of polymeric nanocrystals [ J.]Royal society of chemistry 2014,50: 1634-. CuCl for Min-Cheol Kim et al2·2H2O is used as a copper source, ascorbic acid is used as a reducing agent, and surfactant polyvinylpyrrolidone is added and added to respectively prepare the cubic and octahedral nano Cu2O was used as a negative electrode of a lithium ion battery, and the test results showed that octahedra having (111) planes exhibited higher reversible capacity and rate cycling performance than cubes having (100) planes (Min-Cheol Kim, Si-Jin Kim, Sang-Beom Han, Da-Hee Kwak, Eui-Tak Hwang, Da-Mi Kim, Gyu-Ho Lee, Hui-Seon Choe and Kyung-Won park, Cubic and octahedral Cu2O nanostructures as anodes for lithium-ion batteries[J].Journal of materials chemistry A,2015,3:23003-23010)。Cu2O shows higher voltage characteristic (2.15V) and specific capacity (375mAh g) in the aspect of lithium battery-1). However, no relevant disclosure in the field of thermal batteries has been found so far.
The invention uses Cu with different grain diameters and different shapes2And O powder is used as the anode material of the thermal battery. Cu2The O electrode is simple to prepare and low in cost; the material has high actual specific capacity, long effective discharge time and excellent discharge performance, and is a novel, reliable and easily-popularized high-energy-density thermal battery anode material.
Disclosure of Invention
FeS2And CoS2Is two traditional thermal battery anode materials, but FeS2The decomposition temperature is low, the resistance is high, and the working life and the effective specific capacity are limited; another positive electrode material CoS2It is not suitable for large-scale production because of high cost and low discharge voltage. The present invention has been made in view of the above problems, and has developed Cu2O is used as a novel thermal battery anode material, and provides a new idea for the research of the novel thermal battery anode material.
The invention relates to application of cuprous oxide, namely adding Cu2O is used in the thermal battery anode.
As a preferred scheme, the invention relates to application of cuprous oxide, Cu2O is used as the anode material of the thermal battery.
The invention relates to application of cuprous oxide, Cu2When the O is used as the anode material of the thermal battery, the decomposition temperature is more than 700 ℃.
The invention relates to application of cuprous oxide, Cu2When O is used as the anode material of thermal battery, Cu2The O electrode discharges at a high temperature of 340-700 ℃.
The invention relates to application of cuprous oxide, namely powdery Cu2O is used as a thermal battery anode material; the powdery Cu2The grain diameter of O is 30 nm-20 μm.
Preferably, the invention relates to application of cuprous oxide, namely powdery Cu2The morphology of O is selected from irregular morphology, sphere and octahedronAt least one of a body and a truncated octahedron. In the present invention, irregular morphology refers to any morphology other than spherical, octahedral, truncated octahedral.
As a preferred scheme, the invention relates to application of cuprous oxide, Cu2When O is used as the anode material of thermal battery, Cu2O electrode at 1-1000 mA cm-2The discharge is performed at a current density.
As a preferred scheme, the invention relates to application of cuprous oxide, Cu2When O is used as the anode material of thermal battery, Cu2The O electrode is matched with LiF-LiCl-LiBr or LiCl-KCl diaphragm for use.
As a preferred scheme, the invention relates to application of cuprous oxide, Cu2When O is used as the anode material of thermal battery, Cu2The O electrode can be matched with a LiB alloy or LiSi alloy negative electrode for use.
As a preferred scheme, the invention relates to application of cuprous oxide, Cu2When O is used as the anode material of thermal battery, Cu2The specific capacity of the O electrode is 150-375 mAh g-1The specific energy is 300-800 Wh kg-1The specific power is 2.3-15 kW kg-1. The cut-off voltage was 1.5V in the above performance test.
The invention relates to the application of cuprous oxide; the thermal battery is prepared by the following steps:
firstly, 100-60 wt% of Cu with different particle sizes and different shapes2Fully and uniformly mixing O and 0-40 wt% of conductive agent (adhesive: MgO 0-50 wt%, electrolyte: LiF-LiCl-LiBr 50-100 wt% or LiCl-KCl 50-100 wt%) powder to obtain Cu2And O positive electrode material powder.
Secondly, weighing a certain mass of diaphragm (adhesive: MgO 0-50 wt%, electrolyte: LiF-LiCl-LiBr 50-100 wt% or LiCl-KCl 50-100 wt%), slowly pouring into a stainless steel mold cavity, and strickling with a ceramic blade.
Thirdly, adjusting the height of the stainless steel die cavity, and weighing a certain mass of fully mixed Cu2Slowly pouring O anode material powder into a stainless steel mold, placing the stainless steel mold on the upper layer of the diaphragm layer, scraping the diaphragm layer by using a blade again, and assembling the whole set of stainless steelAnd (5) molding.
And fourthly, applying a certain pressure to the stainless steel mould by using a tablet press, and maintaining the pressure for a period of time. To obtain Cu2O positive electrode/separator sheet.
Fifthly, adding Cu2Simply stacking the O anode/diaphragm sheet and the cathode sheet (LiB alloy or LiSi alloy) in a sandwich shape to obtain Cu2And (4) O single-heat battery.
All the steps I-V are carried out in a glove box (in an argon atmosphere).
The detection method involved in the invention is as follows:
firstly, mixing Cu2The O single heat battery discharges at the high temperature of 340-700 ℃.
② mixing Cu2The O single heat battery is 1-1000 mA cm-2The discharge is performed at a current density.
③ mixing Cu2The O-cell is discharged in a protective gas (argon) or air.
Principles and advantages
1)Cu2The O electrode can discharge at the high temperature of 340-700 ℃ and has the specific NiS2、FeS2And CoS2Wait for higher discharge temperatures (below 650 ℃);
2)Cu2the O electrode material is not decomposed above 700 ℃ and has a specific NiS2、FeS2And CoS2Higher thermal stability and lower cost;
3)Cu2o has a specific FeS2And CoS2Higher actual discharge voltage;
4)Cu2the O electrode material has small resistance and is suitable for large-current discharge;
5)Cu2the O electrode material has small resistance, which is beneficial to reducing the activation time of the thermal battery;
6) cu with grain size of 30 nm-20 microns and irregular block, sphere, octahedron, truncated octahedron and the like2The electrode material prepared by O has better discharge performance.
7) The grain refinement is beneficial to improving Cu2The ionic conductivity of O, so that the discharge performance of the thermal battery is improved;
8) the anode material is beneficial to improving the specific capacity and the specific energy of the thermal battery.
9) The invention uses Cu with different grain diameters and different shapes2The O is used as the anode material of the thermal battery, and provides a new idea for the research of the novel anode material of the thermal battery.
Drawings
FIG. 1 shows Cu obtained in examples 1 to 82O thermal cell electrode discharge performance detection graph.
Detailed description of the invention
Example 1
Spherical Cu with D50 ═ 1 μm2Uniformly mixing O powder and conductive additive (adhesive: MgO 50 wt%, electrolyte: LiF-LiCl-LiBr 50 wt%) in a mass ratio of 4:1 to obtain Cu2O-type thermal battery anode material powder. 0.2g of cathode powder and 0.4g of separator powder (binder: MgO 50 wt%, electrolyte: LiF-LiCl-LiBr 50 wt%) were layered-pressed by powder pressing to obtain a cathode/separator sheet. Mixing Cu2After the O anode/diaphragm LiB alloy cathode plate is combined into a sandwich single cell, the current density is 0.1A cm-2And discharging at constant temperature of 500 ℃ (shown in figure 1.a and b respectively), and the test result shows that Cu2The anode material of the O-type thermal battery has three discharge stages, wherein the voltage in the stage 1 is about 2.3V, the voltage in the stage 2 is about 2.05V, and the voltage in the stage 3 is about 1.78V. When the cut-off voltage is 1.5V, the discharge time reaches 652s, and the specific capacity reaches 282mAh g-1The specific energy reaches 540Wh kg-1The active specific power reaches 2.98kW Kg-1。
Example 2
Spherical Cu with D50 ═ 230nm2Uniformly mixing O powder and conductive additive (adhesive: MgO 50 wt%, electrolyte: LiF-LiCl-LiBr 50 wt%) in a mass ratio of 4:1 to obtain Cu2O-type thermal battery anode material powder. 0.2g of the positive electrode powder was layered-pressed with 0.4g of separator powder (binder: MgO 50 wt%, electrolyte: LiF-LiCl-LiBr 50 wt%) by powder pressing. Mixing Cu2After the O anode/diaphragm LiB alloy cathode plate is combined into a sandwich single cell, the thickness of the sandwich single cell is 0.1A cm-2Discharge at-500 ℃ (FIGS. 1.c and d, respectively), testThe results show that micron Cu2The anode material of the O-type thermal battery has three discharge stages, wherein the voltage in the stage 1 is about 2.3V, the voltage in the stage 2 is about 2.05V, and the voltage in the stage 3 is about 1.78V. When the cut-off voltage is 1.5V, the discharge time reaches 763s, and the specific capacity reaches 344mAh g-1The specific energy reaches 632Wh kg-1The active specific power reaches 2.98kW Kg-1。
Example 3
Spherical Cu with D50 ═ 1 μm2Uniformly mixing O powder and conductive additive (adhesive: MgO 50 wt%, electrolyte: LiF-LiCl-LiBr 50 wt%) in a mass ratio of 4:1 to obtain Cu2O-type thermal battery anode material powder. 0.2g of the positive electrode powder was layered-pressed with 0.4g of separator powder (binder: MgO 50 wt%, electrolyte: LiF-LiCl-LiBr 50 wt%) by powder pressing. Mixing Cu2After the O anode/diaphragm sheet and the LiB alloy cathode sheet are combined into a sandwich single cell, the thickness of the sandwich single cell is 0.1A cm-2Discharge at-550 ℃ (FIGS. 1.e and f, respectively), test results show that Cu is present2The anode material of the O-type thermal battery has three discharge stages, wherein the voltage of the stage 1 is about 2.32V, the voltage of the stage 2 is about 2.05V, and the voltage of the stage 3 is about 1.78V. When the cut-off voltage is 1.5V, the discharge time reaches 605s, and the specific capacity reaches 270mAh g-1The specific energy reaches 520Wh kg-1The active specific power reaches 3.12kW Kg-1。
Example 4
Spherical Cu with D50 ═ 1 μm2Uniformly mixing O powder and a conductive additive (a binder: MgO 30 wt%, an electrolyte: LiF-LiCl-LiBr 70 wt%) in a mass ratio of 4:1 to obtain Cu2O-type thermal battery anode material powder. 0.2g of cathode powder and 0.4g of separator powder (binder: MgO 30 wt%, electrolyte: LiF-LiCl-LiBr 70 wt%) were layered-pressed by powder pressing to obtain a cathode/separator sheet. Mixing Cu2After the O anode/diaphragm sheet and the LiB alloy cathode sheet are combined into a sandwich single cell, the thickness of the sandwich single cell is 0.2A cm-2Discharge at-500 ℃ (fig. 1.g and h, respectively), test results show that Cu2The anode material of the O-shaped thermal battery has three discharge stages, wherein the voltage in stage 1 is about 2.21V, the voltage in stage 2 is about 1.98V, and the voltage in stage 3 is 1.7About 4V. When the cut-off voltage is 1.5V, the discharge time reaches 292s, and the specific capacity reaches 270mAh g-1The specific energy reaches 504Wh kg-1The active specific power reaches 6.2kW Kg-1。
Example 5
Spherical Cu with D50 ═ 1 μm2The O powder and the conductive additive (binder: MgO 50 wt%, electrolyte: LiCl-KCl 50 wt%) are uniformly mixed in a mass ratio of 4:1 to obtain Cu2O-type thermal battery anode material powder. 0.2g of the positive electrode powder and 0.4g of the separator powder (binder: MgO 50 wt%, electrolyte: LiCl-KCl 50 wt%) were layered-pressed by powder pressing to obtain a positive electrode/separator sheet. Mixing Cu2After the O anode/diaphragm sheet and the LiB alloy cathode sheet are combined into a sandwich single cell, the thickness of the sandwich single cell is 0.1A cm-2Discharge at-500 ℃ (FIGS. 1.i and j, respectively), test results show that Cu2The anode material of the O-type thermal battery has three discharge stages, wherein the voltage of the stage 1 is about 2.28V, the voltage of the stage 2 is about 2.03V, and the voltage of the stage 3 is about 1.77V. When the cut-off voltage is 1.5V, the discharge time reaches 539s, and the specific capacity reaches 244mAh g-1The specific energy reaches 456Wh kg-1The active specific power reaches 3kW Kg-1。
Example 6
Spherical Cu of 0.15g D50 ═ 1 μm2And (3) layering and pressing the O powder and 0.35g of diaphragm powder (adhesive: 50 wt% of MgO and electrolyte: 50 wt% of LiF-LiCl-LiBr) to obtain the anode/diaphragm sheet. Mixing Cu2After the O anode/diaphragm sheet and the LiB alloy cathode sheet are combined into a sandwich single cell, the thickness of the sandwich single cell is 0.1A cm-2Discharge at-500 ℃ (fig. 1.k and l, respectively), test results show that Cu2The anode material of the O-type thermal battery has three discharge stages, wherein the voltage in the stage 1 is about 2.3V, the voltage in the stage 2 is about 2.05V, and the voltage in the stage 3 is about 1.78V. When the cut-off voltage is 1.5V, the discharge time reaches 375s, and the specific capacity reaches 167mAh g-1The specific energy reaches 320Wh kg-1The active specific power reaches 3.06kW Kg-1。
Example 7
Spherical Cu with D50 ═ 1 μm2O powder and conductive additive (binder: MgO 20 wt%)The electrolyte: LiF-LiCl-LiBr 80 wt%) in a mass ratio of 4:1 to obtain Cu2O-type thermal battery anode material powder. 0.2g of cathode powder and 0.4g of separator powder (binder: MgO 20 wt%, electrolyte: LiF-LiCl-LiBr 80 wt%) were layered-pressed by powder pressing to obtain a cathode/separator sheet. Mixing Cu2After the O anode/diaphragm sheet and the LiSi alloy cathode sheet are combined into a sandwich single cell, the thickness of the sandwich single cell is 0.1A cm-2Discharge at-500 ℃ (FIG. 1.m and n, respectively), test results show that Cu2The anode material of the O-type thermal battery has three discharge stages, wherein the voltage in the stage 1 is about 2.3V, the voltage in the stage 2 is about 2.05V, and the voltage in the stage 3 is about 1.78V. When the cut-off voltage is 1.5V, the discharge time reaches 569s, and the specific capacity reaches 253mAh g-1The specific energy reaches 479Wh kg-1The active specific power reaches 3kW Kg-1。
Example 8
Octahedral Cu with D50 ═ 1 μm2Uniformly mixing O powder and conductive additive (adhesive: MgO 50 wt%, electrolyte: LiF-LiCl-LiBr 50 wt%) in a mass ratio of 4:1 to obtain Cu2O-type thermal battery anode material powder. 0.2g of cathode powder and 0.4g of separator powder (binder: MgO 50 wt%, electrolyte: LiF-LiCl-LiBr 50 wt%) were layered-pressed by powder pressing to obtain a cathode/separator sheet. Mixing Cu2After the O anode/diaphragm sheet and the LiB alloy cathode sheet are combined into a sandwich single cell, the thickness of the sandwich single cell is 0.1A cm-2Discharge at-500 ℃ (FIG. 1.o, p, respectively), test results show that Cu2The anode material of the O-type thermal battery has three discharge stages, wherein the voltage in the stage 1 is about 2.3V, the voltage in the stage 2 is about 2.05V, and the voltage in the stage 3 is about 1.78V. When the cut-off voltage is 1.5V, the discharge time reaches 637s, and the specific capacity reaches 287mAh g-1The specific energy reaches 550Wh kg-1The active specific power reaches 3.1kW Kg-1。

Claims (6)

1. The application of the cuprous oxide is characterized in that: mixing Cu2O is used in the anode of the thermal battery; the thermal battery is prepared by the following steps:
firstly, 60-100 wt% of Cu2O and 0 to 40 wt% of carbonFully and uniformly mixing the electrolyte powder to obtain Cu2O positive electrode material powder; the conductive agent powder is composed of the following components:
adhesive agent: 0 to 50 wt% of MgO,
electrolyte: 50-100 wt% of LiF-LiCl-LiBr or 50-100 wt% of LiCl-KCl;
secondly, weighing a certain mass of diaphragm, slowly pouring the diaphragm into a stainless steel die cavity, and scraping the diaphragm with a ceramic blade; the membrane consists of the following components:
adhesive agent: 0 to 50 wt% of MgO,
electrolyte: 50-100 wt% of LiF-LiCl-LiBr or 50-100 wt% of LiCl-KCl;
thirdly, adjusting the height of the stainless steel die cavity, and weighing a certain mass of fully mixed Cu2Slowly pouring O anode material powder into a stainless steel mold, placing the O anode material powder on the upper layer of the diaphragm layer, scraping the O anode material powder by using a blade again, and assembling the whole set of stainless steel mold;
fourthly, applying a certain pressure to the stainless steel mould by using a tablet press, and maintaining the pressure for a period of time; to obtain Cu2O positive electrode/separator sheet;
fifthly, adding Cu2Simply stacking the O anode/diaphragm sheet and the cathode sheet in a sandwich shape to obtain Cu2An O single heat cell;
powdery Cu2O is used as a thermal battery anode material; the powdery Cu2The grain diameter of O is 30 nm-20 mu m;
Cu2when O is used as the anode material of thermal battery, Cu2The specific capacity of the O electrode is 150-375 mAh g-1The specific energy is 300-800 Wh kg-1The specific power is 2.3-15 kW kg-1。
2. Use of cuprous oxide according to claim 1, characterized in that: cu2When the O is used as the anode material of the thermal battery, the decomposition temperature is more than 700 ℃.
3. Use of cuprous oxide according to claim 1, characterized in that: cu2When O is used as the anode material of thermal battery, Cu2The O electrode is carried out at the high temperature of 340-700 DEG CAnd (4) discharging.
4. Use of cuprous oxide according to claim 1, characterized in that: powdery Cu2The shape of the O is selected from at least one of irregular blocks, spheres, octahedrons and truncated octahedrons.
5. Use of cuprous oxide according to claim 1, characterized in that: cu2When O is used as the anode material of thermal battery, Cu2O electrode at 1-1000 mA cm-2The discharge is performed at a current density.
6. Use of cuprous oxide according to claim 1, characterized in that: cu2When O is used as the anode material of thermal battery, Cu2The O electrode can be matched with a LiB alloy or LiSi alloy negative electrode for use.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4044192A (en) * 1970-07-10 1977-08-23 Catalyst Research Corporation Thermal batteries
CN107611389A (en) * 2017-08-31 2018-01-19 上海空间电源研究所 A kind of thermal cell aoxidizes copper-based composite positive pole and its production and use

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4044192A (en) * 1970-07-10 1977-08-23 Catalyst Research Corporation Thermal batteries
CN107611389A (en) * 2017-08-31 2018-01-19 上海空间电源研究所 A kind of thermal cell aoxidizes copper-based composite positive pole and its production and use

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"A Long-Life Thermal Cell";Lawrence H. Thaller et al;《Journal of The Electrochemical Society》;19661231;第113卷(第4期);第309页左栏最后一段到第310页左栏最后一段和第312页右栏第2-3段 *

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