A metal-based phosphorus-sulfur compound thermal battery positive electrode material and preparation method thereof

Abstract

The present invention provides a metal-based phosphorus-sulfur compound thermal battery cathode material and a preparation method thereof. The thermal battery cathode material comprises, by weight, 70-80 parts of a metal-based phosphorus-sulfur compound, 0.5-3 parts of a lithiating agent, and 10-25 parts of a eutectic salt electrolyte, wherein the metal in the metal-based phosphorus-sulfur compound is a transition metal. The preparation method comprises preparing the metal-based phosphorus-sulfur compound and the thermal battery cathode material using a solid-phase sintering method. The present invention applies transition metal phosphorus-sulfur compounds to the field of thermal battery cathode materials, leveraging their high thermal stability to ensure the performance of thermal batteries in high-temperature operating environments. Their two-dimensional layered structure facilitates rapid migration of lithium ions within the material's lattice and ensures sufficient wetting with the eutectic salt electrolyte, thereby improving the discharge performance of thermal batteries. This advances research into high-temperature cathode materials for thermal batteries.

Description

Technical Field

[0001] The present invention relates to the technical field of thermal battery positive electrode materials, and in particular to a metal-based phosphorus-sulfur compound thermal battery positive electrode material and a preparation method thereof. Background Art

[0002] A thermal battery is a reserve chemical power source, typically using molten salts such as LiCl-KCl, LiF-LiCl-LiBr, or LiCl-LiBr-KBr as its electrolyte. At room temperature, the electrolyte in a thermal battery is a non-conductive solid. Under operating conditions, the battery's internal heating system heats the stack, rapidly moltenizing the electrolyte and allowing the battery to enter operation. Due to their rapid activation, long storage life, wide operating temperature range, and high reliability, thermal batteries are an ideal reserve power source for a variety of modern weaponry, including missiles, artillery shells, rockets, decoy radars, sonobuoys, torpedoes, and life-saving devices, and hold a crucial position in the military.

[0003] The technological development of high-performance thermal batteries directly impacts the operational performance of weapon systems. To meet the energy demands of weapon systems with diverse strike objectives in modern warfare, increasingly stringent performance requirements are being placed on thermal batteries, including operating temperature range, high-temperature operating time, and specific energy. A comparative study of the common characteristics of traditional sulfide cathode materials, such as FeS2, CoS2, and NiS2, reveals that their primary drawback lies in their insufficient thermal stability. Consequently, they are unable to guarantee discharge stability during loaded discharge and safety during unloaded operation in high-temperature thermal batteries. Consequently, the development of sulfides with higher thermal decomposition temperature resistance is urgently needed to increase the utilization of cathode materials in high-temperature operating environments and further enhance battery performance. Summary of the Invention

[0004] The purpose of the present invention is to provide a metal-based phosphorus-sulfur compound thermal battery positive electrode material and a preparation method thereof, and to apply transition metal (iron or nickel) phosphorus-sulfur compounds to the field of thermal battery positive electrode materials, utilizing their good thermal stability and excellent electrochemical properties to improve the performance of thermal batteries in high-temperature working environments.

[0005] The technical solution adopted by the present invention is: a metal-based phosphorus-sulfur compound thermal battery positive electrode material, which is composed of 70 to 80 parts of a metal-based phosphorus-sulfur compound, 0.5 to 3 parts of a lithiating agent, and 10 to 25 parts of a eutectic salt electrolyte, calculated by mass, wherein the metal in the metal-based phosphorus-sulfur compound is a transition metal.

[0006] Furthermore, the chemical formula of the metal-based phosphorus-sulfur compound is FePS3 or NiPS3.

[0007] Furthermore, the lithiating agent is Li2O.

[0008] Furthermore, the eutectic salt electrolyte is one of LiCl-KCl, LF-LiCl-LiBr, LiF-LiBr-KBr and LiCl-LiBr-KBr.

[0009] The present invention also provides a method for preparing the metal-based phosphorus-sulfur compound thermal battery positive electrode material as described in any one of the above items, comprising the steps of:

[0010] S1. Mixing metal powder, phosphorus powder and sulfur powder uniformly, vacuum-sealing and performing a constant temperature reaction, and slowly cooling after the reaction to obtain a mixture;

[0011] S2, removing the vacuum package from the mixture, placing it in a protective atmosphere for a secondary constant temperature reaction, slowly cooling it after the reaction, and then ball milling and sieving to obtain a metal-based phosphorus-sulfur compound;

[0012] S3. Evenly mix the metal-based phosphorus-sulfur compound, the lithiating agent, and the eutectic salt electrolyte, place the mixture in the protective atmosphere for three constant-temperature reactions, slowly cool the mixture after the reaction, and then ball-mill and sieve the mixture to obtain the thermal battery positive electrode material.

[0013] Furthermore, in step S1, the amounts of the metal powder, phosphorus powder and sulfur powder are in accordance with the following standard: the molar ratio of the metal element, phosphorus element and sulfur element is 1:1:3 to 1:1.2:3.2; and the above substances are dispersed and mixed using a mixing device or a ball mill, and the dispersion time is 5 minutes to 30 minutes.

[0014] Furthermore, in step S1, a quartz tube with a wall thickness of 2 mm to 4 mm and a diameter of 10 mm to 30 mm is used for vacuum packaging. During the vacuum packaging, the quartz tube is evacuated to 2×10 -3 Pa, and then the quartz tube is sealed using a hydrogen flame.

[0015] Furthermore, in step S1, a single temperature zone synthesis furnace is used for a constant temperature reaction, and the single temperature zone synthesis furnace is one of a single temperature zone tubular furnace, a muffle furnace and a high temperature sintering furnace. The temperature of the single temperature reaction is 650°C to 1000°C, and the constant temperature time is 4d to 10d.

[0016] Furthermore, in step S2, the secondary constant temperature reaction adopts a single temperature zone tubular furnace, the temperature of the secondary constant temperature reaction is 400° C. to 600° C., and the constant temperature time is 1 hour to 4 hours.

[0017] Furthermore, in step S3, the temperature of the three constant temperature reactions is 250° C. to 450° C., and the constant temperature time is 4 h to 5 h.

[0018] Furthermore, the heating rates of the first constant temperature reaction, the second constant temperature reaction, and the third constant temperature reaction are all 1°C / min to 5°C / min, and the cooling rates are all 5°C / min to 10°C / min.

[0019] Furthermore, a planetary ball mill is used for ball milling, the ball milling speed is 400 r / min to 600 r / min, and the ball milling time is 1 h to 3 h.

[0020] Furthermore, the protective atmosphere is nitrogen or argon.

[0021] The present invention has the following beneficial effects: using high-purity FePS3 or NiPS3 as the main material of the thermal battery positive electrode, utilizing FePS3 or NiPS3 to still have high stability under high temperature conditions of 800°C, thereby ensuring the performance of the thermal battery in a high-temperature working environment; utilizing the two-dimensional layered structure of FePS3 or NiPS3 to assist lithium ions in achieving rapid migration within the material lattice and achieving sufficient infiltration with the eutectic salt electrolyte, thereby improving the ionic conductivity of the thermal battery positive electrode material, so that the single cell made of the metal-based phosphorus-sulfur compound thermal battery positive electrode material provided by the present invention has a high conductivity at 100mA / cm 2 Under the current density conditions, it shows an operating voltage of about 2.2V and a high specific capacity of about 400mAh / g, which improves the discharge performance of the thermal battery and promotes the research on high-temperature positive electrode materials for thermal batteries. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a physical picture of the FePS3 crystal obtained in Example 1 of the present invention;

[0023] Figure 2 This is a physical picture of the NiPS3 crystal prepared in Example 2 of the present invention;

[0024] Figure 3 1 is the XRD pattern of FePS3 prepared in Example 1 of the present invention and NiPS3 prepared in Example 2;

[0025] Figure 4 is a SEM image of FePS3 prepared in Example 1 of the present invention;

[0026] Figure 5 is the TG graph of FePS3 prepared in Example 1 of the present invention;

[0027] Figure 6 3 and 4. It is a discharge curve diagram of the FePS3 thermal battery positive electrode material prepared in Examples 1 and 2 of the present invention and the NiPS3 thermal battery positive electrode material prepared in Examples 3 and 4. DETAILED DESCRIPTION

[0028] The following describes embodiments of the present invention in detail, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present invention, and are not to be construed as limiting the present invention.

[0029] The present invention provides a metal-based phosphorus-sulfur compound thermal battery cathode material. The thermal battery cathode material comprises, by weight, 70 to 80 parts of a metal-based phosphorus-sulfur compound, 0.5 to 3 parts of a lithiating agent, and 10 to 25 parts of a eutectic salt electrolyte. The metal-based phosphorus-sulfur compound has a chemical formula of FePS3 or NiPS3, the lithiating agent is Li2O, and the eutectic salt electrolyte is one of LiCl-KCl, LF-LiCl-LiBr, LiF-LiBr-KBr, and LiCl-LiBr-KBr.

[0030] The present invention also provides a method for preparing a positive electrode material of a metal-based phosphorus-sulfur compound thermal battery, comprising the steps of:

[0031] S1. Take metal powder (iron powder or nickel powder), phosphorus powder and sulfur powder according to the standard element molar ratio of 1:1:3 to 1:1.2:3.2, and use a mixing device or a ball mill to disperse and mix the above substances for 5 minutes to 30 minutes; then put the above substances into a quartz tube with a wall thickness of 2mm to 4mm and a diameter of 10mm to 30mm, and evacuate the quartz tube to 2×10 -3 Pa, and then the quartz tube is sealed with a hydrogen flame; the packaged quartz tube is placed in a single-temperature zone synthesis furnace, and the temperature is increased to 650°C to 1000°C at a heating rate of 1°C / min to 5°C / min for a constant temperature reaction. After the constant temperature is maintained for 4d to 10d, the temperature is lowered to room temperature at a cooling rate of 5°C / min to 10°C / min to obtain a mixture, wherein the single-temperature zone synthesis furnace is one of a single-temperature zone tubular furnace, a muffle furnace and a high-temperature sintering furnace.

[0032] S2. The mixture is taken out of the quartz tube, and then placed in a single-temperature-zone tubular furnace filled with a nitrogen or argon protective atmosphere, and the temperature is increased to 400°C to 600°C at a heating rate of 1°C / min to 5°C / min for a secondary constant temperature reaction. After constant temperature for 1h to 4h, the temperature is lowered to room temperature at a cooling rate of 5°C / min to 10°C / min, and the mixture is ball-milled at a ball-milling speed of 400r / min to 600r / min using a planetary ball mill for 1h to 3h, and sieved to obtain the metal-based phosphorus-sulfur compound FePS3 or NiPS3.

[0033] S3. Weigh the metal-based phosphorus-sulfur compound (FePS3 or NiPS3), the lithiating agent and the eutectic salt electrolyte according to the above-mentioned mass fractions and mix them evenly. Place them in a nitrogen or argon protective atmosphere, heat them to 250°C~450°C at a heating rate of 1°C / min~5°C / min and carry out three constant-temperature reactions. After keeping the constant temperature for 4h~5h, cool them to room temperature at a cooling rate of 5°C / min~10°C / min. Use a planetary ball mill at a ball milling speed of 400r / min~600r / min for 1h~3h, sieve, and you can get the thermal battery positive electrode material.

[0034] In step S1, taking phosphorus powder and sulfur powder in a slightly excessive proportion can improve the utilization rate of metal. On the one hand, the cost of phosphorus powder and sulfur powder is low. On the other hand, phosphorus powder and sulfur powder can be removed by high-temperature heating, that is, removed by step S2, so as to obtain relatively pure metal-based phosphorus-sulfur compounds FePS3 or NiPS3; and the metal-based phosphorus-sulfur compounds FePS3 or NiPS3 obtained after the secondary constant temperature reaction in step S2 have a large particle size, and need to be ball milled and sieving to reduce their particle size, increase their specific surface area during thermal battery discharge, and thereby improve their discharge performance.

[0035] Several embodiments are listed below for specific description:

[0036] Example 1:

[0037] S1. Take iron powder, phosphorus powder and sulfur powder according to the standard element molar ratio of 1:1:3, use a mixing device to disperse and mix the above substances, and the dispersion time is 20 minutes; then put the above substances into a quartz tube with a wall thickness of 2mm to 4mm and a diameter of 10mm to 30mm, and evacuate the quartz tube to 2×10 -3 Pa, and then use a hydrogen flame to seal the quartz tube; then put the packaged quartz tube into a muffle furnace, heat it to 800℃ at a heating rate of 1℃ / min for a constant temperature reaction, and after keeping the temperature constant for 7 days, cool it to room temperature at a cooling rate of 5℃ / min to obtain a mixture.

[0038] S2. The mixture was taken out of the quartz tube and placed in a single-temperature zone tubular furnace filled with argon protective atmosphere. The temperature was raised to 550°C at a heating rate of 1°C / min for secondary constant temperature reaction. After constant temperature for 3 hours, the temperature was lowered to room temperature at a cooling rate of 5°C / min. The mixture was ball milled at a ball milling speed of 400 r / min for 1 hour and sieved to obtain a metal-based phosphorus-sulfur compound FePS3. The crystal physical picture, XRD test results and SEM test results are shown in Figures 2 and 3. Figure 1 、 3 and 4.

[0039] S3. Weigh 8g of metal-based phosphorus-sulfur compound FePS3, 0.2g of lithiating agent Li2O and 1.8g of eutectic salt electrolyte LiF-LiCl-LiBr and mix them evenly. Place them in an argon protective atmosphere, heat them to 400℃ at a heating rate of 1℃ / min and carry out three constant-temperature reactions. After keeping the temperature constant for 4h, cool them to room temperature at a cooling rate of 5℃ / min. Use a planetary ball mill at a ball milling speed of 400r / min for 1h, and sieve to obtain FePS3 thermal battery positive electrode material.

[0040] Thermal stability test: reference Figure 5 The FePS3 prepared in this embodiment has almost no decomposition phenomenon under 800°C conditions, has good thermal stability, and can ensure the performance of the thermal battery in a high-temperature working environment.

[0041] Discharge performance test: The prepared FePS3 thermal battery cathode material was used as the positive electrode, LiF-LiCl-LiBr / MgO as the electrolyte, and LiB alloy as the negative electrode. A single cell with a diameter of 17.5 mm was pressed and a discharge experiment was conducted at a constant current of 100 mA / cm 2 , the voltage of the single cell is 2.16V. When the cut-off voltage is 1.7V, the specific capacity of the thermal battery is about 398mAh / g. Figure 6 As shown in the FePS3-1 curve.

[0042] Example 2:

[0043] S1. Take iron powder, phosphorus powder and sulfur powder according to the standard element molar ratio of 1:1:3, use a mixing device to disperse and mix the above substances, and the dispersion time is 20 minutes; then put the above substances into a quartz tube with a wall thickness of 2mm to 4mm and a diameter of 10mm to 30mm, and evacuate the quartz tube to 2×10 -3 Pa, and then use a hydrogen flame to seal the quartz tube; then put the packaged quartz tube into a muffle furnace, heat it to 800℃ at a heating rate of 1℃ / min for a constant temperature reaction, and after keeping the temperature constant for 7 days, cool it to room temperature at a cooling rate of 5℃ / min to obtain a mixture.

[0044] S2. The mixture is taken out of the quartz tube, and then placed in a single-temperature-zone tubular furnace filled with argon protective atmosphere, and the temperature is increased to 550°C at a heating rate of 1°C / min for a secondary constant-temperature reaction. After constant temperature for 3 hours, the mixture is cooled to room temperature at a cooling rate of 5°C / min. The mixture is ball-milled in a planetary ball mill at a ball-milling speed of 400 r / min for 1 hour, and sieved to obtain the metal-based phosphorus-sulfur compound FePS3.

[0045] S3. Weigh 7.8g of metal-based phosphorus-sulfur compound FePS3, 0.2g of lithiating agent Li2O and 2.0g of eutectic salt electrolyte LiF-LiCl-LiBr and mix them evenly. Place them in an argon protective atmosphere, heat them to 400℃ at a heating rate of 1℃ / min and carry out three constant-temperature reactions. After keeping the temperature constant for 4h, cool them to room temperature at a cooling rate of 5℃ / min. Use a planetary ball mill at a ball milling speed of 400r / min for 1h, and sieve to obtain FePS3 thermal battery positive electrode material.

[0046] Discharge performance test: The prepared FePS3 thermal battery cathode material was used as the positive electrode, LiF-LiCl-LiBr / MgO as the electrolyte, and LiB alloy as the negative electrode. A single cell with a diameter of 17.5 mm was pressed and a discharge experiment was conducted at a constant current of 100 mA / cm 2 , the cell voltage is 2.16V. When the cut-off voltage is 1.7V, the specific capacity of the thermal battery is about 410mAh / g. This result also shows that FePS3 has good discharge repeatability as the positive electrode material of the thermal battery. Figure 6 As shown in the FePS3-2 curve.

[0047] Example 3:

[0048] S1. Nickel powder, phosphorus powder and sulfur powder were taken in a standard element molar ratio of 1:1.2:3.2 and dispersed and mixed using a ball mill for 30 min. The above substances were then placed in a quartz tube with a wall thickness of 2 mm to 4 mm and a diameter of 10 mm to 30 mm. The quartz tube was evacuated to 2×10 -3 Pa, and then use a hydrogen flame to seal the quartz tube; then put the packaged quartz tube into a muffle furnace, heat it to 800℃ at a heating rate of 1℃ / min for a constant temperature reaction, and after keeping the temperature constant for 8 days, cool it to room temperature at a cooling rate of 5℃ / min to obtain a mixture.

[0049] S2. The mixture was taken out of the quartz tube and placed in a single-temperature zone tubular furnace filled with nitrogen protective atmosphere. The temperature was raised to 600°C at a heating rate of 1°C / min for secondary constant temperature reaction. After constant temperature for 3 hours, the temperature was lowered to room temperature at a cooling rate of 5°C / min. The mixture was ball milled at a ball milling speed of 600 r / min for 2 hours using a planetary ball mill. The mixture was sieved to obtain a metal-based phosphorus-sulfur compound NiPS3. The crystal physical picture and XRD test results are shown as follows: Figure 2 and 3 shown.

[0050] S3. Weigh 7g of metal-based phosphorus-sulfur compound, 0.2g of lithiating agent Li2O and 2.8g of eutectic salt electrolyte LiF-LiCl-LiBr and mix them evenly. Place them in a nitrogen protective atmosphere, heat them to 420℃ at a heating rate of 1℃ / min and carry out three constant temperature reactions. After keeping the temperature constant for 5h, cool them to room temperature at a cooling rate of 5℃ / min. Use a planetary ball mill at a ball milling speed of 600r / min for 2h, and sieve to obtain NiPS3 thermal battery positive electrode material.

[0051] The thermal decomposition temperature of NiPS3 prepared in this example is also higher than 800°C, and it has similar physical structure and electrochemical properties to those of FePS3 prepared in Example 1.

[0052] Discharge performance test: The prepared NiPS3 thermal battery cathode material was used as the positive electrode, LiF-LiCl-LiBr / MgO as the electrolyte, and LiB alloy as the negative electrode. A single cell with a diameter of 17.5 mm was pressed and a discharge experiment was conducted at a constant current of 100 mA / cm 2 , the voltage of the single cell is 2.27V. When the cut-off voltage is 1.7V, the specific capacity of the thermal battery is about 400mAh / g. Figure 6 As shown in the NiPS3-1 curve.

[0053] Example 4:

[0054] S1. Nickel powder, phosphorus powder and sulfur powder were taken in a standard element molar ratio of 1:1.2:3.2 and dispersed and mixed using a ball mill for 30 min. The above substances were then placed in a quartz tube with a wall thickness of 2 mm to 4 mm and a diameter of 10 mm to 30 mm. The quartz tube was evacuated to 2×10 -3 Pa, and then use a hydrogen flame to seal the quartz tube; then put the packaged quartz tube into a muffle furnace, heat it to 800℃ at a heating rate of 1℃ / min for a constant temperature reaction, and after keeping the temperature constant for 8 days, cool it to room temperature at a cooling rate of 5℃ / min to obtain a mixture.

[0055] S2. The mixture was taken out of the quartz tube, and then placed in a single-temperature-zone tubular furnace filled with a nitrogen protective atmosphere, and heated to 600°C at a heating rate of 1°C / min for a secondary constant-temperature reaction. After being kept at this temperature for 3 hours, the mixture was cooled to room temperature at a cooling rate of 5°C / min. The mixture was ball-milled in a planetary ball mill at a ball-milling speed of 600 r / min for 2 hours, and sieved to obtain the metal-based phosphorus-sulfur compound NiPS3.

[0056] S3. Weigh 7.5g of metal-based phosphorus-sulfur compound, 0.2g of lithiating agent Li2O and 2.3g of eutectic salt electrolyte LiF-LiCl-LiBr and mix them evenly. Place them in a nitrogen protective atmosphere, heat them to 420℃ at a heating rate of 1℃ / min and carry out three constant temperature reactions. After keeping the temperature constant for 5h, cool them to room temperature at a cooling rate of 5℃ / min. Use a planetary ball mill at a ball milling speed of 600r / min for 2h, and sieve to obtain NiPS3 thermal battery positive electrode material.

[0057] Discharge performance test: The prepared NiPS3 thermal battery cathode material was used as the positive electrode, LiF-LiCl-LiBr / MgO as the electrolyte, and LiB alloy as the negative electrode. A single cell with a diameter of 17.5 mm was pressed and a discharge experiment was conducted at a constant current of 100 mA / cm 2 , the cell voltage is 2.27V. When the cut-off voltage is 1.7V, the specific capacity of the thermal battery is also around 400mAh / g. This result also shows that NiPS3 has good discharge repeatability as a positive electrode material for thermal batteries. Figure 6 As shown in the NiPS3-2 curve.

[0058] According to Examples 1-4, high-purity FePS3 or NiPS3 is used as the main material of the thermal battery positive electrode, and FePS3 or NiPS3 still has high stability under high temperature conditions of 800°C to ensure the performance of the thermal battery in a high-temperature working environment; the two-dimensional layered structure of FePS3 or NiPS3 is used to assist lithium ions in rapid migration within the material lattice and achieve sufficient infiltration with the eutectic salt electrolyte to improve the ionic conductivity of the thermal battery positive electrode material, so that the single cell made of the metal-based phosphorus-sulfur compound thermal battery positive electrode material provided by the present invention has a conductivity of 100mA / cm 2 Under the current density conditions, it shows an operating voltage of about 2.2V and a high specific capacity of about 400mAh / g, which improves the discharge performance of the thermal battery and promotes the research on high-temperature positive electrode materials for thermal batteries.

[0059] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A metal-based phosphorus-sulfur compound thermal battery positive electrode material, characterized in that: The composition of the thermal battery positive electrode material is as follows, in parts by mass: 70 to 80 parts of a metal-based phosphorus-sulfur compound, 0.5 to 3 parts of a lithiating agent, and 10 to 25 parts of a eutectic salt electrolyte, wherein the metal in the metal-based phosphorus-sulfur compound is a transition metal; the metal-based phosphorus-sulfur compound is FePS3 or NiPS3.

2. The metal-based phosphorus-sulfur compound thermal battery positive electrode material according to claim 1, characterized in that: The lithiating agent is Li2O.

3. A metal-based phosphorus-sulfur compound thermal battery positive electrode material according to any one of claims 1-2, characterized in that: The eutectic salt electrolyte is one of LiCl-KCl, LF-LiCl-LiBr, LiF-LiBr-KBr and LiCl-LiBr-KBr.

4. The method for preparing the positive electrode material of the metal-based phosphorus-sulfur compound thermal battery according to any one of claims 1 to 3, characterized in that: Including steps: S1. Mixing metal powder, phosphorus powder and sulfur powder uniformly, vacuum sealing and performing a constant temperature reaction, and slowly cooling after the reaction to obtain a mixture; S2, removing the vacuum package from the mixture, placing it in a protective atmosphere for a secondary constant temperature reaction, slowly cooling it after the reaction, and then ball milling and sieving to obtain a metal-based phosphorus-sulfur compound; S3, uniformly mixing the metal-based phosphorus-sulfur compound, the lithiating agent, and the eutectic salt electrolyte, placing the mixture in the protective atmosphere for three constant-temperature reactions, slowly cooling the mixture after the reaction, and then ball-milling and sieving to obtain the thermal battery positive electrode material; The temperature of the first isothermal reaction is 650℃~1000℃, and the isothermal time is 4d~10d; the temperature of the second isothermal reaction is 400℃~600℃, and the isothermal time is 1h~4h; the temperature of the third isothermal reaction is 250℃~450℃, and the isothermal time is 4h~5h.

5. The method for preparing the positive electrode material of the metal-based phosphorus-sulfur compound thermal battery according to claim 4, characterized in that: In step S1, the amounts of the metal powder, phosphorus powder and sulfur powder are in accordance with the following standard: the molar ratio of the metal element, phosphorus element and sulfur element is 1:1:3 to 1:1.2:3.

2.

6. The method for preparing the positive electrode material of the metal-based phosphorus-sulfur compound thermal battery according to claim 4, characterized in that: A planetary ball mill is used for ball milling, the ball milling speed is 400r / min~600r / min, and the ball milling time is 1h~3h.

7. The method for preparing the positive electrode material of the metal-based phosphorus-sulfur compound thermal battery according to claim 4, characterized in that: The protective atmosphere is nitrogen or argon.

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