2044 results about "Solid phase reactions" patented technology

The invention discloses a method for preparing a manganese series lithium ion sieve adsorbent, and relates to a method for preparing an inorganic adsorbent for adsorbing lithium from liquid lithium resources such as brine of salt lake, seawater and the like. In the method, a cubic crystal ion sieve precursor Li1.6Mn1.6O4 is prepared from Mn2O3 and LiOH or Li2CO3 serving as raw materials by using two sections of solid-phase reactions, wherein the precursor also can be used as an anode material of a lithium ion battery. The precursor is acidized to obtain a lithium ion sieve adsorbent MnO2.0.5H2O (or expressed as H1.6Mn1.6O4), and the ion sieve is the lithium adsorbent which has high selectivity on lithium. The method has the advantages of simple and readily available raw materials, simple process, high adsorption capacity of the ion sieve, low cost, high purity of products and is easy to realize industrial production.

The invention discloses a method for preparing nitrogen-doped graphene which comprises the following steps of: drying a mixture of a carbon-containing precursor and a carbon-nitrogen-containing precursor; raising the temperature of the dried mixture to be 450-600 DEG C, and keeping the temperature to generate gray solid; and continuously raising the temperature of the gray solid to be 700-1000 DEG C, introducing protective gas, keeping the temperature to generate black solid, and obtaining the nitrogen-doped graphene. According to the method for preparing nitrogen-doped graphene in the embodiment, the nitrogen-doped graphene is obtained under normal pressure and high temperature through a solid-phase reaction, the whole preparation method is simple in process, the nitrogen-doped graphene can be obtained without complex equipment, and industrial production is easily performed. In addition, the invention also provides nitrogen-doped graphene.

(Problem)

In conventional method for producing artificial graphite, in order to obtain a product having excellent crystallinity, it was necessary to mold a filler and a binder and then repeat impregnation, carbonization and graphitization, and since carbonization and graphitization proceeded by a solid phase reaction, a period of time of as long as 2 to 3 months was required for the production and cost was high and further, a large size structure in the shape of column and cylinder could not be produced. In addition, nanocarbon materials such as carbon nanotube, carbon nanofiber and carbon nanohorn could not be produced.

(Means to Solve)

A properly pre-baked filler is sealed in a graphite vessel and is subsequently subjected to hot isostatic pressing (HIP) treatment, thereby allowing gases such as hydrocarbon and hydrogen to be generated from the filler and precipitating vapor-phase-grown graphite around and inside the filler using the generated gases as a source material, and thereby, an integrated structure of carbide of the filler and the vapor-phase-grown graphite is produced. In addition, nanocarbon materials are produced selectively and efficiently by adding a catalyst or adjusting the HIP treating temperature.

The invention relates to a preparation method of lithium iron phosphate for the carbon cladding of a lithium ion battery. The prior lithium iron phosphate preparation technical art is complex, and has high cost. The invention has the synthetic process that: ferric oxide, phosphoric acid, simple organics and doped element compound are mixed and dried, the mol ratio of phosphate radical ion, ferric ion and doped element ion is 1:y:z, wherein, y is larger than or equal to 0.95 and smaller than or equal to 1, and y plus z is equal to 1; the mixture is added with lithium source compound, added with water to be mixed and dried, the mol ratio of lithium ion and phosphate radical ion is x:1, and x is larger than or equal to 0.95 and smaller than or equal to 1.05; the mixture which reacts for 2 to 20 hours under 500 to 800 DEG C is cooled in a furnace. The invention finally produces the precursor uniformly mixed with superfine crystal grain, and during the subsequent high temperature solid phase reaction, the end product lithium iron phosphate can be produced through shorter distance diffuseness of atoms. The end product has high purity, the crystallisation is good, the capacity is high, and the cycle stability is good.

The present invention belongs to the field of electrochemical power source material preparing technology, and is especially preparation process of oxygen place doped lithium ferric phosphate powder. The oxygen place doped lithium ferric phosphate as positive pole material in lithium ion cell has the molecular expression LiFeP(MxO4-x), and is prepared through mixing the dopant and the mother body material and sintering the mixture, or through solid phase reaction of the dopant and the mother body material. The preparation process has effective doping in the oxygen place of mother body material and the prepared material can raise the capacity and the circular discharge performance of the cell effectively and thus can find its wide application as positive pole material in secondary lithium ion cell and power cell.

The invention relates to a method for preparing a Cu2Se thermoelectric material. The method for preparing the Cu2Se thermoelectric material by the low-temperature solid-phase reaction is characterized by comprising the following step: 1) weighing Cu powder and Se powder according to the molar ratio of 2:1 and mixing the Cu powder and the Se powder uniformly to obtain mixed powder, wherein the Cu powder and the Se powder serve as raw materials; 2) pressing the mixed powder into a block body by using tablet press, placing the block body into a graphite crucible, vacuumizing, sealing into a quartz glass tube, placing into a muffle furnace, performing solid-phase reaction at the temperature of between 650 and 750 DEG C for 12 to 24 hours, and grinding the obtained product into powder; and 3) performing spark plasma sintering on the powder obtained in the step 2) to obtain a compact block body, namely the Cu2Se thermoelectric material. By the method, the raw materials have low cost; the reaction temperature is low; energy is saved; and the materials are fed according to the stoichiometric ratio of the Cu2Se, so the product composition can be controlled precisely; and the repeatability is high.

The invention discloses a method for manufacturing alumina ceramic cores, which adopts sintering of solid phase reaction, comprising two sintering methods of pre-sintering and final sintering; sintering temperature decreases to 1,350 to 1,500 DEG C from more than 1,500 DEG C in the prior art and creep resistance of high temperature is favorable. The invention also discloses a method for leaching the alumina ceramic cores. As in the process of the manufacture of the alumina ceramic cores, a volatile pore forming agent is adopted so that the forming alumina ceramic cores have relatively high porosity; in core leaching, melting alkali can reach the internal part of the alumina ceramic cores so as to integrally disperse the alumina ceramic cores. In the invention, a boiling water process and a repeated alkali cooking-dissolving- alkali cooking method are adopted, thus accelerating permeation, reaction and dissolving of the melting alkali to the internal part of the ceramic cores; the core leaching speed decreases to 10 to 16 hours from 25 to 30 hours in the prior art and the core leaching speed is accelerated.

The invention discloses a nano reinforcing method for recycled aggregate concrete, which belongs to the technical fields of recycling comprehensive utilization of waste and production of building materials, and is mainly characterized by comprising the steps of: mixing and stirring a recycled aggregate and a nano particle dispersion for 5-10s; after the surface of the recycled aggregate is in a moist state, further mixing the recycled aggregate with all admixtures for 5-10s; and mixing and stirring with cement, water and a high-efficiency water reducing agent for 20-45s to obtain a nano-reinforced recycled aggregate concrete mixture. The nano reinforcing method has a principle that by changing a stirring process and introducing the nano dispersion, nano particles can be adsorbed into the opening pores and microcracks of the recycled aggregate, an admixture enriched layer is further formed on the surface of the recycled aggregate, the nano particles permeating into the interiors of the opening pores of the recycled aggregate and the admixture enriched layer formed on the surface of the recycled aggregate are used for jointly absorbing calcium hydroxide enriched on the surface and the pores of the recycled aggregate in the strength development process of the recycled aggregate concrete, a gelling material with higher strength is generated through hydration, liquid-phase or solid-phase reactions so as to reinforce the recycled aggregate per se and an interface between the recycled aggregate and set cement, and thus, the strength of the recycled aggregate concrete is enhanced. After the nano reinforcement, the recycled aggregate concrete has the 28-day compression strength improved by around 15-20%.

The invention relates to a method for synthesizing LiFePO4/C material by chemical vapor deposition supporting the solid phase reaction method, namely, the method for preparing carbon coating lithium iron battery anode material, belonging to the Li-ion battery material preparation art technical field. The characteristics of the method for synthesizing LiFePO4/C materials by solid phase and auxiliary chemical vapor deposition are that auxiliary chemical vapor deposition supporting the solid phase reaction method is adopted to synthesize the carbon coating phosphate lithium iron, namely, the LiFePO4/C material. In the method for synthesizing LiFePO4/C material by chemical vapor deposition supporting the solid phase reaction method, a precursor comprising raw materials of lithium, iron and phosphor is adopted to prepare the carbon coating phosphate lithium iron after being blended, grinded by a globe mill, treated by preheating and calcined as well as vapor deposition. The method for synthesizing LiFePO4/C material by chemical vapor deposition supporting the solid phase reaction method has the advantages that the chemical composition, carbon contents and grain size of LiFePO4 can be controlled effectively; the Li-ion battery anode material prepared has sound conductive performance and can improve the charge-discharge rate and cycling performance of the material.

The invention relates to a solid phase preparation method for gamma-alumina with gradient distribution holes. The method comprises: adopting a solid phase reaction to obtain a precursor ammonium aluminum carbonate hydroxide, and carrying out calcination to obtain gamma-alumina with a high specific surface area, gradient distribution holes and a large pore volume. The most prominent characteristic of the present invention comprises adopting a raw material solid phase reaction synthesis technology and controlling the property of the resulting gamma-alumina through synthesis conditions. In addition, the method of the present invention has characteristics of simpleness, easy operation, no requirement of addition of a pore-expanding agent, and cost saving, and is suitable for industrial mass production.

The invention provides a method for recycling and synchronous harmless treatment of gold, silver and iron in roasting-cyanidation tailings, and belongs to the technical field of metallurgical waste residue utilization. The method comprises the following steps: mixing dried roasting-cyanidation tailings with a fluxing agent and a reducing agent; carrying out roasting at 750 to 900 DEG C for 3 to 5 hours; conducting water quenching on hot roasted sand for cooling; carrying out ore grinding and flotation to remove residual carbon; leaching gold and silver with an environment-friendly gold leaching agent; and conducting magnetic separation on the leaching residue to obtain fine iron powder. Containing no highly toxic cyanide, the rejects belong to general industry solid waste. As the fluxing agent is added for magnetic roasting, not only can gold and silver coated with an iron mineral be exposed, but also the fluxing agent can perform a solid-phase reaction with a silicate mineral to generate a dissoluble silicate, and gold and silver coated with the dissoluble silicate can also be exposed after ore grinding. According to the method, gold, silver and iron in the roasting-cyanidation tailings are recycled, harmless treatment is realized synchronously, and the purpose of clean production is realized.

The invention discloses a Sr-doping oxide BiCuSeO thermoelectric material and a preparation method of the Sr-doping oxide BiCuSeO thermoelectric material, belonging to the technical field of new energy source materials. The preparation method comprises the following steps of ball-milling material mixing, solid-phase sintering, ball-milling refining, and discharging plasma sintering, and specifically comprises the following steps of: mixing Bi2O3 with the purity of 99.99%, SrO with the purity of 99.99%, Cu with the purity of 99.99%, Se with the purity of 99.99% and Bi with the purity of 99.99% according to a stoichiometric ratio, uniformly mixing in a ball milling manner, carrying out cold-pressing, carrying out a solid-phase reaction, pulverizing in the ball milling manner, and then carrying out the discharging plasma sintering to prepare Bi1-xSrxCuSeOoxide block bodies (x=0-0.125). Compared with other oxide thermoelectric materials, the Sr-doping oxide BiCuSeO thermoelectric material disclosed by the invention has the advantages of high conductivity, high temperature-difference electrodynamic potential, low thermal conductivity and the like; and the preparation method has the advantages of simple and convenient process, short synthesis and formation times and the like.

The invention relates to a method for preparing black zirconia ceramics at the low temperature and belongs to the technical field of the preparation of high-temperature structural material. The method respectively uses a homogeneous precipitation method for synthesizing a nanometer coloring agent, and a coprecipitation method for synthesizing nanometer zirconia powder, and adopts Fe-Co-Ni-Mn as a coloring agent. The zirconia powder is not added with any sintering additive, only added with small amount of coloring agent and sintered at the temperature of 1150-1350 DEG C, thus obtaining the black zirconia ceramics with excellent performance and bright color. As the homogeneous precipitation method is adopted for synthesizing coloring agent powder, the monodisperse nanometer particles with uniform powder granules, narrow size distribution and high purity are obtained so that the coloring agent easily colors the particles. As the coprecipitation method is used for synthesizing zirconia powder, nanometer particles with small granularity, big superficial area and high activity are obtained, and can reduce the temperature of the solid-phase reaction, greatly reduce the sintering temperature and solve the problem that the black coloring agent oxide decomposes and volatiles at the high temperature. Simultaneously the method adopts the Fe-Co-Ni-Mn as the coloring agent, thus avoiding the poisonous function of Cr on the human body.

The invention relates to the technical field of electrode materials of lithium ion batteries and preparation of the electrode materials, in particular to a lithium nickel cobalt manganese oxygen/stannic oxide composite anode material doped with metal elements and a method for preparing the lithium nickel cobalt manganese oxygen/stannic oxide composite anode material. The lithium nickel cobalt manganese oxygen/stannic oxide composite anode material doped with the metal elements is expressed by LiNixCoyMnzRzO2/SnO2 and obtained by performing high-temperature solid-phase reaction on nickel, cobalt and manganese compounds, lithium salt, doped metal compounds and stannic compounds. By doping the metal elements and coating the stannic oxide, the initial discharge capacity, multiplying power performance and cycle stability of the material can be effectively improved. The material is prepared by using all-solid-phase reaction, and the process is simple in flow and convenient to operate.

The invention provides a method for recovering a positive electrode material precursor and lithium carbonate from a positive electrode waste material of a lithium ion battery. The method comprises carrying out mechanical crushing on the waste produced by battery production or waste or old batteries, carrying out sorting to obtain impurity-containing positive electrode powder, carrying out immersion through a reducing agent-containing volatile leaching agent to obtain extract, carrying out concentration rectification, regenerating the volatile leaching agent, adjusting ingredients of the raffinate containing Co, Ni, Mn and Li, carrying out coprecipitation on Co, Ni and Mn, carrying out solid-liquid separation, further treating the Li-rich solution to obtain high-purity lithium carbonate, and carrying out a high temperature solid-phase reaction process on the mixed materials of Co, Ni and Mn precursors to obtain a positive electrode active material. The method is simple and is free of a complicated impurity removal process and an extraction enrichment technology. The extraction agent has a wide source, high extraction selectivity and high extraction efficiency. After the extraction reaction, the extraction agent can be recovered and recycled through concentration rectification. The method reduces a cost, can produce high-quality Co, Ni and Mn precursors and high-quality lithium carbonate and has a good application prospect.

The invention relates to a perovskite type material preparation method and equipment, and a machining method of a photovoltaic device made from a perovskite type material. The invention provides the method for preparing the perovskite type material by a gaseous phase-solid phase reaction and a method for preparing a matrix deposited with a precursor BX2 film by adopting a vapor deposition method, and provides special equipment for the methods. The perovskite type material preparation method can be used for machining a photovoltaic element, and the obtained photovoltaic element has excellent photoelectric property.

The invention discloses a preparation method of a graded porous carbon material. The preparation method comprises the following steps: sufficiently grinding a reaction raw material, obtaining a carbon precursor material having a core-shell structure by virtue of solid-phase reaction, carbonizing the carbon precursor material in one step at high temperature in an inert atmosphere, and removing a template to obtain the graded porous carbon material. The prepared graded porous carbon material is large in specific surface area and has an adjustable micropore-mesoporous graded porous structure; when being applied to the fields such as super-capacitors and lithium-sulfur batteries, the graded porous carbon material is excellent in electrochemical properties. The method is simple in process, environment-friendly and capable of realizing low-cost large-scale preparation of the graded porous carbon material.

The invention discloses a method for preparing solar-grade silicon through purification of industrial silicon (2N). The method comprises that: the industrial silicon is subjected to primary pulverization pretreatment and is put into a high-temperature solid-phase reaction furnace; the industrial silicon and active gas are subjected to gas-solid reaction at high temperature to achieve the aim of removing metal impurities; then crystalline silicon is cleaned; the purity of the crystalline silicon reaches as high as 99.999 percent (5N), and is further subjected to vacuum melting of electron beams and oriented condensation treatment; finally, active atmosphere plasma is adopted to further purify the crystalline silicon, and volatile elements which have high activity and are easily oxidized to generate high saturated vapor pressure are removed; and polysilicon is cast in an integrated furnace for casting plasma polysilicon and is directly used for manufacturing a cell chip. The method combines high-temperature gas-solid reaction to remove the metal impurities, the electron beams to remove the volatile elements and a plasma purification and casting integrated furnace technology, improves the purity of the polysilicon to 99.99999 percent (7N) and, fully meets requirement of a solar cell industry on the solar-grade silicon.

The invention provides a barium titanate/polyvinylidene fluoride composite dielectric film and a preparation method thereof. The film comprises barium titanate and polyvinylidene fluoride with the weight ratio of 1.5-5.0:1, and the thickness of the film is less than 50 mu m. In the frequency range of 100 Hz-1 MHz, the relative dielectric constant of the film can reach more than 70, and the dielectric loss is lower than 5*10<-2>. By compounding BaTiO3 ceramic and PVDF polymer, the dielectric film material with high dielectric constant and low dielectric loss is prepared. According to the invention, the barium titanate/polyvinylidene fluoride composite dielectric film with uniform distribution of ceramic particles, controllable thickness, high dielectric constant and low dielectric loss is prepared by preparing barium titanate ceramic powder through solid phase reaction or chemical coprecipitation and then using high temperature drying gel method or solvent induced phase separation gel method. The dielectric film is especially suitable for capacitor, ferroelectric memory, and other electronic devices.

The invention provides a novel quasi garnet-structured lithium ion conductor (Li7-xLa3Zr2-xSbxO12, wherein x is more than 0 and less than or equal to 0.5) crystalline-state ceramic solid electrolyte material and a synthesis method thereof, and belongs to the field of lithium ion batteries. A novel quasi garnet-structured lithium ion conductor is synthesized by conventional solid-phase reaction. X-ray diffraction (XRD) diffraction peaks of Sb-doped samples show that the Sb-doped samples all have crystalline -state cubic phase quasi garnet-structures in the Sb doped range. The maximum lithium ion conductivity can reach 3.42*10<-4>S/cm at room temperature (30 DEG C). The sample is synthesized by the conventional solid phase method, a preparation process is simple, and sintering time is short. Zr is partially replaced by high-valence Sb, so the lithium ion vacancy is increased, the ionic conductivity is improved obviously, and antimonous oxide is low in price compared with zirconia, so manufacturing cost is reduced. Therefore, the synthesized compact ceramic solid electrolyte material can be probably applied to a lithium ion battery.