43 results about "Phosphorus sulfide" patented technology

The invention relates to a sulfide solid electrolyte and a preparation method and application thereof, and the preparation method comprises the following steps: distributing elemental sulfur powder on the surface of lithium sulfide powder to obtain composite powder; mixing the composite powder with phosphorus sulfide and lithium halide to obtain a precursor; and sintering the precursor to obtain the sulfide solid electrolyte. According to the preparation method disclosed by the invention, the elemental sulfur powder is distributed on the surface of the lithium sulfide powder, so that the elemental sulfur powder can participate in formation of the sulfide solid electrolyte before volatilization in the sintering process, the prepared sulfide solid electrolyte does not have sulfur loss, and no impurity phase is generated in the sulfide solid electrolyte; therefore, the ionic conductivity of the sulfide solid-state electrolyte can be improved, and the electrochemical performance of an all-solid-state battery can be obviously improved when the sulfide solid-state electrolyte is used for assembling the all-solid-state battery; meanwhile, the preparation method is simple and efficient, and the obtained sulfide solid electrolyte is uniform in performance.

The invention relates to the field of new energy batteries, in particular to a sulfide solid electrolyte, a preparation method thereof and a battery, the preparation method comprises the following steps: S1, dissolving lithium sulfide and lithium halide in an anhydrous organic solvent to obtain a first material; drying the first material to obtain a first mixture; s2, mixing the first mixture with phosphorus sulfide to obtain a precursor; and S3, carrying out sintering treatment on the precursor. The preparation method of the sulfide solid electrolyte is simple and efficient in process and low in preparation cost, uniform mixing of high-melting-point raw materials can be achieved, then uniform mixing of precursors is achieved, and the solid electrolyte prepared through the method is free of impurity phases and high in batch stability.

The present invention provides a composite positive electrode for an all-solid-state lithium-sulfur battery and a method for preparing the same, belonging to the technical field of positive electrode materials for lithium-sulfur batteries. The composite positive electrode comprises a sulfur / carbon composite material with a gradient surface modification of phosphorus polysulfide and a solid electrolyte. The composite material comprises porous carbon, sulfur, and phosphorus polysulfide, with the sulfur loaded on the outer surface and / or in the pores of the porous carbon, and a phosphorus polysulfide layer with a gradient distribution of a specific structure on the surface of the sulfur / carbon composite. The present invention utilizes the sulfur / carbon composite material with a gradient surface modification of phosphorus polysulfide as a positive electrode material for an all-solid-state lithium-sulfur battery, effectively increasing the active sulfur content and specific capacity of the composite positive electrode layer. The composite positive electrode of the present invention can have an active sulfur content exceeding 50 wt%, a specific capacity calculated based on elemental sulfur exceeding 1300 mAh / g, and a specific capacity based on the total mass of the composite positive electrode exceeding 650 mAh / g. Furthermore, the composite positive electrode exhibits excellent cycle and rate performance.

The invention relates to a preparation method of a two-dimensional nano layered polymetallic phosphorus sulfide, which comprises the following steps: mechanically and uniformly mixing a lithium-containing transition metal precursor and P2S5 in an inert atmosphere, then heating for melting and calcining, adding a crude product into an alcohol-water solution, heating and stirring, centrifugally separating, washing a precipitate, and drying to obtain the two-dimensional nano layered polymetallic phosphorus sulfide. The chemical formula of the polymetallic phosphorus sulfide is LixM1aM2bM3cM4dM5ePS3, x is greater than or equal to 0 and less than or equal to 1.2, and M1, M2, M3, M4 and M5 are independently selected from Co, Fe, Mn, Ni, Ti, Cu, Zn, Cd, Cr and Mo; a + b + c + d + e = 1, and a, b, c, d and e > = 0; wherein the transverse size of the two-dimensional nano layered multi-transition metal phosphorus sulfide is 0.5-10 [mu] m, and the thickness of the nanosheet is 10-40 nm. According to the invention, the two-dimensional phosphorus sulfide nano layered material can be rapidly prepared through the reaction of the transition metal precursor and phosphorus sulfide, and the two-dimensional phosphorus sulfide nano layered material shows good activity and stability when being used as a Li-O2 battery solid electrolyte.

The invention relates to the technical field of electro-catalysis, in particular to transition metal phosphorus sulfide and a preparation method and application thereof. The invention provides a preparation method of transition metal phosphorus sulfide, which comprises the following steps: mixing transition metal, phosphorus and sulfur to obtain a mixture; and carrying out vacuum sintering on the mixture to obtain the transition metal phosphorus sulfide. According to the preparation method, the transition metal phosphorus sulfide is successfully prepared, the transition metal phosphorus sulfide has excellent urea electro-catalysis performance, and more efficient electro-catalysis urea oxidation can be achieved to assist water electrolysis for hydrogen production.

The invention provides a high-entropy metal phosphorus-sulfur compound nanosheet as well as a preparation method and application thereof. The preparation method of the high-entropy metal phosphorus-sulfur compound nanosheet comprises the steps that manganese powder, cobalt powder, nickel powder, copper powder, silver powder, phosphorus powder and sulfur powder are mixed according to a preset mass ratio, tableting is conducted after even grinding is conducted, and a tableting sample is obtained; vacuumizing the tableting sample and then packaging the tableting sample; heating the packaged tablet sample to 590-710 DEG C, keeping the temperature for 150-200 hours, and cooling to obtain a block sample; after grinding the block sample, dispersing the block sample in a polar solvent for ultrasonic cleaning to obtain a cleaning mixed solution; taking supernate of the cleaning mixed solution, carrying out ultrasonic crushing treatment, and centrifuging to obtain a nanosheet crude product; and cleaning the nanosheet crude product, and performing vacuum freeze drying to obtain the nanosheet product. The invention aims to solve the problem of poor catalytic performance of metal phosphorus sulfide.

A method for producing a sulfide-based inorganic solid electrolyte material, the method including a step of obtaining a sulfide-based inorganic solid electrolyte material in a vitreous state by mechanically processing a raw material composition of the sulfide-based inorganic solid electrolyte material including lithium sulfide and a phosphorus sulfide composition such that each component is vitrified in a chemical reaction, in which the phosphorus sulfide composition has three or more peaks in a range of 2θ = 22.5° or more and 24.5° or less in an X-ray diffraction analysis spectrum obtained by X-ray diffraction analysis.

The invention discloses a zinc thiophosphate material with a yolk double-shell structure as well as a preparation method and application thereof, and relates to the technical field of sodium ion batteries. The preparation method comprises the following steps: firstly, preparing a ZIF-8 precursor template through a zinc source and solvothermal reaction of 2-methylimidazole, and then sequentially carrying out coating, template etching, synchronous carbonization and vulcanization treatment and phosphorus vulcanization treatment on the ZIF-8 precursor template to finally obtain the ZnPS3 / NC-C material with the yolk double-shell structure and excellent electrochemical performance. Compared with a traditional transition metal thiophosphate preparation process, the method is safer in process, and the yolk double-shell morphology of the metal phosphorus sulfide can be accurately regulated and controlled. Compared with pure zinc thiophosphate prepared by a traditional process, the prepared ZnPS3 / NC-C material with the yolk double-shell structure has the characteristics of hollow and porous characteristics, high specific surface area and structural stability, and shows relatively high first charge-discharge efficiency and excellent cycle stability when being used as a sodium-ion battery negative electrode material.

The preparation method comprises the following steps: (1) adding a lead salt and diammonium hydrogen phosphate into deionized water, stirring at room temperature, dropwise adding ammonia water into the deionized water in the stirring process, continuously stirring to obtain a mixed solution, adding the mixed solution into a hydrothermal kettle for reaction at the hydrothermal temperature of 100-200 DEG C for 10-30 hours, and filtering to obtain a filtrate; carrying out solid-liquid separation on a white product after the reaction to obtain a solid matter, drying the solid matter at 50-60 DEG C, and then carrying out high-temperature calcination to obtain lead phosphate powder; and (2) vulcanizing the lead phosphate powder to prepare the infrared detection material based on vulcanized lead phosphate. The prepared infrared detection material based on sulfurized lead phosphate is used for an infrared detector. The synthesis method has the beneficial effects that 1, the synthesis method is simple and low in cost, the used solvent is environment-friendly and green, and the synthesis method is suitable for large-scale production; and 2, the vulcanized lead phosphate disclosed by the invention has an ultra-low band gap and has the feasibility of infrared detection.

The invention relates to a preparation method of a two-dimensional nano layered polymetallic phosphorus sulfide, which comprises the following steps: mechanically and uniformly mixing a lithium-containing transition metal precursor and P2S5 in an inert atmosphere, then heating for melting and calcining, adding a crude product into an alcohol-water solution, heating and stirring, centrifugally separating, washing a precipitate, and drying to obtain the two-dimensional nano layered polymetallic phosphorus sulfide. The chemical formula of the polymetallic phosphorus sulfide is LixM1aM2bM3cM4dM5ePS3, x is greater than or equal to 0 and less than or equal to 0.86, and M1, M2, M3, M4 and M5 are independently selected from Co, Fe, Mn, Ni, Ti, Cu, Zn, Cd, Cr and Mo; a + b + c + d + e = 1, and a, b, c, d and e > = 0; wherein the transverse size of the two-dimensional nano layered multi-transition metal phosphorus sulfide is 0.5-10 [mu] m, and the thickness of the nanosheet is 10-40 nm. According to the invention, the two-dimensional phosphorus sulfide nano layered material can be rapidly prepared through the reaction of the transition metal precursor and phosphorus sulfide, and the two-dimensional phosphorus sulfide nano layered material shows good activity and stability when being used as a Li-O2 battery solid electrolyte.

The present invention relates to a method for producing a solid material according to the following general formula (I): Li 6‑x‑2y Cu x PS 5‑y X(I), wherein X is selected from the group consisting of: F, Cl, I and Br; 0.005≤x≤5; and 0≤y≤0.5; the method comprises at least introducing at least lithium sulfide, phosphorus sulfide, a halogen compound and a copper compound, optionally in one or more solvents. The present invention also relates to the solid material and its use as a solid electrolyte, especially for electrochemical devices.

Provided is a method for producing sulfide solid electrolyte having an argyrodite-type crystal structure, the method including mixing lithium sulfide, a phosphorus sulfide, and an ammonium halide to produce a solid electrolyte precursor, and firing the solid electrolyte precursor. The method for producing a sulfide solid electrolyte having an argyrodite-type crystal structure provides a method for easily producing a high-quality sulfide solid electrolyte without using an elemental halogen which complicates the handling or a lithium halide which has a considerably high hygroscopicity.

The application discloses a solid-state polymer electrolyte containing two-dimensional nano additives and a preparation method and application thereof, and belongs to the technical field of lithium metal batteries. The preparation method of the solid-state polymer electrolyte is as follows: transition metal phosphorus sulfide precursors, lithium salt and polymer are added into a dispersing agent, stirring is conducted to strip the transition metal phosphorus sulfide and lithiumize, and a polymer electrolyte precursor solution is formed; and stirring is finished to obtain a mixture slurry; wherein the transition metal phosphorus sulfide precursors include one or more of FePS3, MnPS3, CdPS3 and ZnPS3; the mixture slurry is coated on a mold, and drying is conducted to obtain the solid-state polymer electrolyte containing two-dimensional nano additives. The preparation method is a one-step lithiumization method for preparing two-dimensional nano additives, is more simple than a two-step alkali metal ion lithiumization method, has no adverse effect on the performance of lithium batteries, and can avoid the introduction of impurity water.

Provided is a phosphorus sulfide composition for a sulfide-based inorganic solid electrolyte material, the phosphorus sulfide composition including P4S10 and P4S9, in which when a total content of P4S10, P4S9, P4S7, and P4S3 in the phosphorus sulfide composition is represented by 100 mass %, a content of P4S10 calculated from a solid 31P-NMR spectrum is 70 mass % or more and 99 mass % or less.

The invention relates to a self-storage voltage comparator, and belongs to the technical field of electronic components. The device comprises a substrate, a transition metal chalcogenide, a metal phosphorus-sulfur (selenide), a source electrode, a drain electrode and an input electrode, the metal phosphorus-sulfur (selenide) is located on the upper surface of the transition metal chalcogenide, and the input electrode is located on the upper surface of the metal phosphorus-sulfur (selenide). The source electrode and the drain electrode are located at the two ends of the transition metal chalcogenide and are electrically communicated with the transition metal chalcogenide. According to the invention, the transition metal chalcogenide and the metal phosphorus-sulfur (selenide) form an integrated device of a field effect transistor and a memristor, an input voltage is identified and compared by using a competitive mechanism between ferroelectricity and ionic conductivity of the metal phosphorus-sulfur (selenide), and a comparison result can be stored in a nonvolatile manner.

The invention discloses a lithium argyrodite sulfide solid electrolyte, a preparation method thereof and an all-solid-state battery, the chemical general formula of the electrolyte is Li7-xPS6-xMx, and the electrolyte is prepared from Li2S, LiM and excessively added P4Sy, wherein M represents halogen, 0 < = x < = 2, and y < = 10. The preparation method comprises the following steps: mixing Li2S, LiM and partially excessive P4Sy according to the stoichiometric ratio of the chemical general formula to obtain a precursor; and then preheating a container added with the residual excessive P4Sy, placing the precursor in the container, and sintering under a sealed condition to obtain the composite material. According to the method, excessive phosphorus sulfide is taken as a preparation raw material, the sealed crucible filled with the phosphorus sulfide is preheated, the ultra-high-purity lithium argyrodite sulfide solid electrolyte can be efficiently and stably synthesized, the conductivity of the electrolyte can reach 2.92 mS cm <-1 >, and the electrolyte is applied to an all-solid-state battery system.

The present invention relates to a method for manufacturing a sulfide-based solid electrolyte, the method comprising the steps of: (S1) preparing a precursor solution by adding a precursor containing an alkali metal sulfide, a phosphorus sulfide, and a halogen compound to a solvent; (S2) performing first milling on the precursor solution to prepare an intermediate product; (S3) adding a dispersant after the step (S2) and then performing second milling to adjust the particle size of the intermediate product; (S4) drying the particle size-adjusted intermediate product after the step (S3); and (S5) heat-treating the dried intermediate product, wherein the dispersant is an aliphatic compound, and the mass ratio of the solvent and the dispersant is 75: 1 to 150: 1.

A phosphorus sulfide composition for a sulfide-based inorganic solid electrolyte material, the phosphorus sulfide composition having a reactivity of 5.0 DEG C / min or more as measured by a predetermined method.

Provided is a phosphorus sulfide composition for a sulfide-based inorganic solid electrolyte material, in which Reactivity measured by a predetermined method is greater than or equal to 5.0 °C / min.

Provided is a phosphorus sulfide composition for a sulfide-based inorganic solid electrolyte material, in which Reactivity measured by a predetermined method is greater than or equal to 5.0 °C / min.

The invention relates to the technical field of lithium batteries, in particular to a positive electrode material of a sulfide-based solid-state lithium battery and the lithium battery comprising the positive electrode. Phosphate-coated nickel-rich layered oxide positive electrode powder is modified by sulfur-rich phosphorus sulfide molecules to prepare a gradient vulcanized phosphate-coated nickel-rich layered oxide positive electrode, the gradient vulcanized phosphate-coated nickel-rich layered oxide positive electrode is compounded with sulfide electrolyte and vapor growth carbon fibers (VGCF) to obtain a composite electrode, and then the composite electrode is compounded with an electrolyte sheet to prepare the lithium battery. The gradient sulfurized phosphate coated nickel-rich layered oxide positive electrode and the sulfide solid electrolyte show interface compatibility, and the all-solid-state battery assembled by the gradient sulfurized phosphate coated nickel-rich layered oxide positive electrode, the sulfide solid electrolyte and the lithium metal negative electrode has good electrochemical performance and cycling stability. The protective layer effectively restrains the space charge layer and stabilizes the nickel-rich layered oxide positive electrode / sulfide electrolyte interface, and the practical process of the sulfide-based all-solid-state lithium battery is better promoted due to the characteristics of simple structure, convenience in preparation and large-scale production.

The invention discloses a preparation method and application of a three-dimensional flower-shaped NixPy-NixSy composite structure, and belongs to the field of NixPy-NixSy composite materials.According to the method, nickel nitrate hexahydrate, ammonium fluoride and urea are selected for preparing a reaction solution, a high-temperature sealed reaction is conducted for sample manufacturing, the sample is made to react with phosphorus powder to manufacture pure-phase NixPy, and the pure-phase NixPy is prepared; according to the preparation method, NixPy-NixSy is used as a raw material and further reacts with sulfur powder to generate the composite material NixPy-NixSy, so that the NixPy-NixSy composite material with regular morphology and excellent dispersity is formed, the NixPy-NixSy composite material has relatively large specific surface area and forms more active contact positions, and meanwhile, the reaction temperature of the synthesis method is far lower than the high temperature required by other methods, so that the particle size is convenient to control, and the preparation method is suitable for industrial production. Therefore, the turnover frequency and the relative reactivity of the crystal face are convenient to estimate, the emission of toxic and harmful gas PH3 is reduced, the phosphating efficiency is remarkably improved, and the transition metal phosphorus sulfide is applied to the field of humidity sensitivity for the first time to construct a novel humidity sensor.

The present disclosure is concerned with unsymnietrical phosphorus disulfide compounds and methods of making the same. 'The disclosed compounds can be useful as therapeutics, for example, anti-viral agents, anti-cancer reagents, and anti-alcoholism drugs. In addition, the disclosed methods are useful in that methods have the advantages of short reaction time, green solvent, high atom economy, and avoidance of using harsh reagents such as oxidants, chlorinating reagents, and transition metal catalysts. This abstract is intended as a scanning tool for purposes of searching in the particular art and is not intended to be limiting of the present invention.

The invention relates to a preparation method of a two-dimensional nano layered transition metal phosphorus sulfide, which comprises the following steps: mechanically and uniformly mixing a transition metal precursor and P2S5 in an inert atmosphere, heating for melting and calcining, adding a crude product into an alcohol-water solution, heating and stirring, centrifugally separating, washing a precipitate, and drying to obtain the two-dimensional nano layered transition metal phosphorus sulfide. The two-dimensional nanometer layered transition metal phosphorus sulfide is obtained; the transverse size of the two-dimensional nano layered transition metal phosphorus sulfide is 1-20 microns, and the thickness of the nanosheet is 5-30 nm. Through simple process steps, the two-dimensional nano layered transition metal phosphorus sulfide which is difficult to obtain by a conventional method can be obtained, the special morphology has abundant active sites exposed on the surface, and the reaction kinetics of the Li-O2 battery is accelerated; and meanwhile, the nanosheet structure can provide more geometric spaces and improve the charge-discharge specific capacity of the battery, so that the Li-O2 battery positive electrode catalyst can show excellent performances of high specific capacity, low overpotential and long cycle life.

To provide a method for producing a phosphorus sulfide composition, which can stably yield a sulfide inorganic solid electrolyte material with improved lithium ion conductivity, a method for producing a sulfide inorganic solid electrolyte material and a method for evaluating a phosphorus sulfide composition.SOLUTION: A method for producing a phosphorus sulfide composition includes the step of selecting a phosphorus sulfide composition that includes three or more peaks in the range of 2θ=22.5° or more and 24.5° or less, in an X-ray diffraction analysis spectrum.SELECTED DRAWING: None

This disclosure provides systems, methods, and apparatus related to lithium phosphorus sulfide halide-polymer composites. In one aspect, a lithium phosphorus sulfur halide (LiPSX) solution and a polymer solution are provided. X is chlorine, bromine, iodine, or combinations thereof. LiPSX of the LiPSX solution and a polymer of the polymer solution are precipitated by mixing the LiPSX solution and the polymer solution. A LiPSX solvent of the LiPSX solution and a polymer solvent of the polymer solution are removed from the LiPSX and the polymer to form polymer-embedded LiPSX.

The invention provides a fly ash slag and sludge synergistic stabilization treatment method which comprises the following steps: S1, adding a composite conditioner into sludge, destroying a colloid structure through microwave-assisted heating, and synchronously reducing the moisture content from 80% to 35% or below in combination with plate-frame pressure filtration; s2, 3%-5% of modified zeolite is doped, free water is preferentially adsorbed, a microporous water locking structure is formed, and moisture remigration in the subsequent curing reaction is avoided; in order to solve the problem of high water content of sludge, a microwave-chemical coupling dehydration and modified zeolite water locking technology is adopted, the water content is reduced from 80% to 35% or below, the upper limit of traditional curing water content 60% is broken through, water interference is eliminated through a staged dry-wet mixing process, and meanwhile, due to the fact that the heavy metal locking time is short, the water content is reduced to 30% or below. A double-effect stable system of vulcanization-phosphate chemical precipitation and geopolymer physical wrapping is constructed, slow-release pH regulation and hydrophobic membrane protection are combined, the locking life is prolonged to 3 times that of a traditional method, and strength improvement and long-acting stability collaborative optimization are achieved.

The present invention provides a method for producing a sulfide-based inorganic solid electrolyte material, the present invention relates to a method for producing a sulfide-based inorganic solid electrolyte material, which comprises a step for obtaining a glass-state sulfide-based inorganic solid electrolyte material by mechanically treating a starting material composition of a sulfide-based inorganic solid electrolyte material containing a lithium sulfide and a phosphorus sulfide composition to chemically react the components and vitrify the components at the same time. The phosphorus sulfide composition has three or more peaks in the range of 2 [theta] = 22.5-24.5 DEG (inclusive) in an X-ray diffraction analysis spectrum obtained by X-ray diffraction analysis of the phosphorus sulfide composition.

The invention relates to a wet-process phosphoric acid deep cadmium removal method based on dialkyl dithiophosphate, which comprises the following steps: (1) taking mixed alcohol of one or more than one straight-chain or branched-chain alcohol as a raw material, reacting with phosphorus pentasulfide, filtering to obtain thiophosphoric acid filtrate, and reacting the thiophosphoric acid filtrate with metal oxide to synthesize dialkyl dithiophosphate (DDP); (2) roughly dividing the conventional wet-process phosphoric acid process into phosphorite pretreatment, phosphorite decomposition, dilute acid sedimentation, dilute acid concentration and concentrated acid sedimentation; and mixing the DDP with the cadmium-containing wet-process phosphoric acid slurry, dilute phosphoric acid or concentrated phosphoric acid for reaction to generate hydrophobic cadmium complex precipitate, and filtering after the reaction is finished to obtain purified phosphoric acid, thereby realizing removal of cadmium. According to the method, no HS gas is generated, and occupational hazards are avoided; raw material cost is low; the cadmium removal rate is gt; the phosphorus loss is as low as 0.5%; the method is suitable for wet-process phosphoric acid slurry, dilute phosphoric acid and concentrated phosphoric acid and can be directly integrated to an existing production line, the cadmium content of the cadmium-containing phosphoric acid after cadmium removal is smaller than or equal to 2 ppm, and the phosphorus loss rate is smaller than or equal to 3%.