391 results about "Platinum crucible" patented technology

A sealing glass frit which is capable of stably joining metal members or ceramic members at temperatures thereof not higher than 1000° C., and at the same time stably maintaining the joined state of the members at temperatures ranging from room temperature to 700 or 800° C. A raw material in an amount of MG 300 g is prepared such that it has a composition of 40 to 70 mol % of SiO₂, 5 to 20 mol % of Al₂O₃, 4 to 20 mol % of Na₂O, 4 to 20 mol % of K₂O, 5 to 20 mol % of ZnO, and 0.5 to 5 mol % of ZrO₂, and the total content of Na₂O and K₂O is not lower than 12 mol %. The raw material is melted in a platinum crucible at 1550° C. for 8 hours, cast in a mold of stainless steel, held at 650° C. for 2 hours, and then cooled to room temperature at 5° C./minute. The cooled raw material is pulverized in a mortar to obtain powder having a particle diameter 10 to 20 μm as a sealing glass frit.

The invention discloses an X-ray fluorescence spectroscopy analysis fusion sample preparation method of an aluminum, manganese, calcium and iron alloy, which comprises the steps of: firstly, coating a uniform protection wall layer in a platinum crucible by using lithium tetraborate, then placing an aluminum, manganese, calcium and iron sample, an oxidizing agent, a lithium borate solvent and a releasing agent into the platinum crucible in which the protection wall is coated, uniformly mixing, and then pre-oxidizing the aluminum, manganese, calcium and iron sample; and finally, melting the pre-oxidized aluminum, manganese, calcium and iron sample, and cooling to obtain an aluminum, manganese, calcium and iron sample glass fuse piece, wherein the aluminum, manganese, calcium and iron sample is a detection sample or calibration sample of the aluminum, manganese, calcium and iron alloy, and the sample glass fuse piece is a detection sample glass fuse piece or calibration sample glass fuse piece of the aluminum, manganese, calcium and iron alloy. On the premise of no corrosion to the valuable platinum crucible, the glass fuse piece can be prepared, and the prepared sample is excellent and uniform, thus the mineral effect and the grain size effect are completely eliminated.

The invention discloses a digestion method of metallurgical materials. The digestion method comprises the steps of: putting the metallurgical materials into a container, adding hydrochloric acid or nitric acid into the container, reacting under the heating condition, filtering a reaction solution after reaction is finished, collecting filtrate and cleaning residues; putting the cleaned residues in a platinum crucible, and heating to 250-600 DEG C for ashing treatment; after complete ashing of the residues, cooling to room temperature, then adding an alkali metal salt solvent, stirring uniformly, heating the mixture stirred uniformly to be 700-1050 DEG C, melting for 10-30 min, cooling, then adding 5-10ml concentrated hydrochloric acid or concentrated nitric acid, boiling, leaching, and obtaining a solution for melting the residues; and combining the filtrate with the solution for melting the residues and obtaining a digested solution. The digestion method is wide in application field, is simple in requirements on experiment instruments, and can be effectively applied in a laboratory equipped with various instruments.

The invention discloses high-refractive-index ultraviolet-transparent glass and a manufacturing method thereof. The high-refractive-index ultraviolet-transparent glass comprises following components, by weight, 5-15% of SiO2, 10-25% of B2O3, 0-5% of CaO, 0-5% of SrO, 10-50% of BaO, 10-50% of La2O3, 5-15% of Nb2O5, 0-5% of Y2O3, 0-5% of ZrO2 and 0-5% of TiO2. The invention also provides the manufacturing method of the high-refractive-index ultraviolet-transparent glass. The method includes following steps: placing quartz sand, boronic acid or boron anhydrous, calcium carbonate, strontium carbonate, barium carbonate, lanthanum oxide, niobium pentoxide, yttria, zirconium oxide and titanium dioxide according to requirement in a formula into a pure-platinum crucible with addition of a reduction agent, melting the materials at 1400-1600 DEG C for 6-10 hours with stirring for 2-3 times during the melting process, and casting the molten glass into a specified specification. The invention also discloses an application of the high-refractive-index ultraviolet-transparent glass in an ultraviolet-transparent optical fiber plate. The high-refractive-index ultraviolet-transparent glass is high in refractive index and transmittance and is good in chemical stability.

The present invention discloses a growth craft of crucible descent method of neotype scintillating crystal LaBr3:Ce3+, which belongs to the domain of crystal growth. Take LaBr3.7H2O and CeBr3.7H2O as the initial raw material, and prepare anhydrous bromide LaBr3 and CeBr3 through the processing of halogenation roasting anhydration. Prepare LaBr3:Ce3+ batch according to suitable CeBr3 doping density, and mix into few active carbon powders as the deoxidizer. Fill crystallons and raw materials using special platinum crucible, and put crucible into crystal growth stove after solder seal it. Control furnace temperature between 850 Deg C and 900 Deg C. Adjust the position of crucible to make welding raw materials and crystallons, and it will form the solid liquid interface whose temperature gradient is between 20 Deg C/centimeter and 50 Deg C/centimeter. Carry on the crucible decline crystal growth at the speed of 0.3-3millimeter/hour, and it can be grown high quality and integrity LaBr3:Ce3+ single crystal. The craft has solved the key technology problems of anhydrous raw material preparation, melt mass oxidation and volatilization and so on, and LaBr3:Ce3+ single crystal can be mass grown in the condition of non-vacuum airtight crucible.

The invention discloses a method for analyzing ferrosilicon alloy components for X-ray fluorescence spectrum analysis. A method for preparing a sample comprises the following steps of: selecting a proper oxidant; adding a flux into a platinum crucible, putting the platinum crucible in a high temperature furnace, and melting the flux at high temperature to manufacture a wall built-up flux crucible with the basement of flux; mixing a ferrosilicon alloy test sample, the flux and the oxidant, pouring the mixture into the flux crucible, and covering a certain amount of mixed flux; and putting the flux crucible filled with the ferrosilicon alloy test sample, the flux, the oxidant and the mixed flux into the high temperature furnace, preliminarily oxidizing at low temperature, shifting into a high temperature zone, and melting at high temperature to prepare the ferrosilicon alloy test sample glass sample for the X-ray fluorescence spectrum analysis. In the technical scheme, elements are uniformly distributed in the prepared glass sample, and the glass sample has no particle effect and can be preserved for a long time; moreover, the operation method is simple and safe, the preparation time of the sample is short, and primary and secondary quantity elements in the ferrosilicon alloy are rapidly and accurately measured.

The invention provides a sealed sample cell for Raman spectrum measurement of high-temperature volatile molten salt and a use method thereof. The sample cell comprises a platinum crucible, a crucible cover, a hearth, a hearth cover and heating platinum wires. The use method is characterized by adopting high-temperature alumina cement to seal the gap between the crucible cover and the mouth of the platinum crucible after feeding samples to be analyzed into the platinum crucible; during measurement, providing current for the heating platinum wires to heat the samples to be analyzed to the measurement temperature, adopting a thermocouple to measure the temperature of the platinum crucible; using the sample cell by matching an upper laser inlet type micros laser Raman spectrometer. The sealed sample cell of the invention can be used for Raman spectrum analysis of the high-temperature volatile molten salt such as cryolite and NaF-AlF3 molten salt with different mol ratios. The use method of the invention can avoid the ingredients of the molten salt to be measured from being affected by escape of the volatile substances, thus improving the measurement precision of the Raman spectrum.

The invention discloses a melted sampling method for aluminum magnesium calcium iron alloy for X-ray fluorescence spectrum analysis. The melted sampling method is characterized by comprising the following steps of: hanging a layer of uniform lithium tetraborate protective wall in a platinum crucible; putting an aluminum magnesium calcium iron sample, lithium carbonate and potassium iodide into the platinum crucible in which the protective wall is hung, mixing uniformly, and covering a layer of lithium tetraborate; pre-oxidizing the aluminum magnesium calcium iron sample; and melting the oxidized aluminum magnesium calcium iron sample, and cooling to obtain a glass fuse piece of the aluminum magnesium calcium iron alloy. By the method, the sampling time is short, the manufactured glass fuse piece is uniform and perfect, and the specification of a mineral effect and a granularity effect can be eliminated completely. The glass fuse piece can be used for the X-ray fluorescence spectrum analysis, the obtained analytic result is accurate and reliable, and the requirements of modern enterprises on quick and accurate detection of analytic data are met. The method is safe, reliable, easy to operate and high in repeatability, and the application range of an X-ray fluorescence spectrum method is broadened.

The invention discloses a novel growth technology of relaxation ferroelectric mono-crystal PIMNT by using a Bridgman-Stockbarger method, belonging to the technical field of mono-crystal growth. The novel growth technology of the relaxation ferroelectric mono-crystal PIMNT comprises the steps of: regarding high-purity PbO, Nb2O5, In2O3, TiO2 and 4MgCO3.Mg(OH)2.4H2O as initial raw materials to prepare a PIMNT polycrystal material through a precursor step-by-step synthesis method, wherein the chemical constitution is xPb(In1/2Nb1/2)O3-yPb(Mg1/2Nb2/3)O3-(1-x-y)PbTiO3, where x=0.24-0.26, and y=0.43-0.45; selecting high-quality seed crystal in a [110], [111] or [001] crystallographic direction; adopting a single-layer or double-layer seamless platinum crucible to contain the seed crystal and a material ingot; putting the crucible after being sealed in a mono-crystal growth furnace; controlling the temperature of the furnace at 1350-1400 DEG C; adjusting the position of the crucible to enable the material ingot to be welded with the top part of the seed crystal so as to form a steady solid-liquid interface with a temperature gradient of 20-50 DEG C; and growing the mono-crystal at a dropping speed of the crucible of less than 1 mm/h to obtain a high-quality and large-size PIMNT mono-crystal. The novel growth technology of the relaxation ferroelectric mono-crystal PIMNT, disclosed by the invention, has the advantages of overcoming a leakage phenomenon of a high-temperature lead-rich melt, avoiding volatilization of components of the melt, and particularly lead oxide steam, efficiently solving a poly-crystallized growth problem of a solid solution with composition complexity, and being suitable for growing high-quality and large-size PIMNT mono-crystals in batches.

The invention relates to a measurement method of the phosphorous content in an iron ore, in particular to a method for measuring the phosphorous content by adopting a bismuth phosphomolybdate blue-sulfuric acid photometry. The method comprises the following steps of: weighing 0.25g of sample and putting into a platinum crucible containing about 2g of mixed fusing agent, putting in a muffle furnace with the temperature of 100 DEG C, fusing for 10min and taking out; cleaning the exterior of the platinum crucible, then putting the platinum crucible into a beaker containing about 80ml of hot water, adding 320ml of concentrated HNO on an electric furnace, heating at low temperature and dissolving, leaching the crucible out, taking the beaker out, cooling, then transferring into a 250ml volumetric flask, diluting to a scale and shaking up for later use; sucking 25ml of mother solution of a fusing sample in the platinum crucible, putting into a 50ml volumetric flask, adding 2.5ml of bismuth nitrate solution, 5ml of ammonium molybdate solution, 3ml of 8mol/L sulfuric acid solution and 5ml of ascorbic acid solution (prepared when needed), shaking up, carrying out color comparison at 750nm wavelength, measuring an absorbance value, and carrying out result conversion by using a guide sample with similar ingredients. The invention effectively solves the problem of instable absorbance value in a method for measuring the phosphorous content by adopting a traditional molybdenum blue spectrophotometry and ensures that the absorbance remains unchanged within two hours.

Disclosed is a light amplified Erbium Ytterbium codoped multi-component oxide glass, comprising SiO2, Al2O3, Li2O, Yb2O3, Er2O3, B2O3, Na2O, K2O, CaO, BaO, ZnO, MgO, etc. The raw materials are added into a crucible for melting, then the obtained glass liquid is added into a platinum crucible for melting, clarifying and homogenizing by an optical glass fusion method. The invention solves the problems in the prior art of narrow gain bandwidth, low glass transition temperature, complicated preparing technology and so on. The Erbium Ytterbium codoped multi-component oxide optical glass fiber can provide transmission bandwidth of 60nm and more even gain spectrum, higher glass transition temperature, better chemical and heat stability, can satisfy the increased requirements of the current optical transmission network.

The invention relates to 3 mu m luminous rare earth ion doped fluorophosphates laser glass and a preparation method thereof. The glass comprises the following components by molar percent: 15-20% of Al(PO3)3, 13-17% of MgF2, 5-25% of CaF2, 5-25% of SrF2, 17-22% of BaF2, 18-22% of NaF and 3-5% of RF3 (R can be rare-earth elements such as Er, Pr, Tm, Ho, or Nd). The glass is prepared by using a platinum crucible and a silicon carbide rod electric furnace fusion method. The glass in the invention is transparent, has no crystallization, has high infrared transmissivity at the vicinity of 3 mu m wave band, good physical and chemical properties and stability parameter delta T of more than or equal to 150 DEG C and can obtain strong 3 mu m fluorescence under the pumping of a laser diode with a wavelength of 980 nm, and the method is suitable for preparation and application of 3 mu m luminous rare earth ion doped special glass and optical fiber materials.

The invention relates to a growth method of a fluxing agent of boron phosphate monocrystal, which comprises the steps of: 1) proportionally mixing a boron phosphate compound and the fluxing agent, putting the mixture into platinum crucible, and heating till completely fusing in a crystal growing furnace; and then cooling to the temperature being 2 to 15 DEG C above a saturation temperature, thus obtaining a high temperature melt containing boron phosphate and the fluxing agent; and 2) putting seed crystal loaded on a seed rod into the high temperature melt, keeping constant temperature for 10 to 180 minutes, reducing the temperature to saturation temperature, and rotating the seed rod at the speed of 10 to 50 revolution/minute; and reducing the temperature at the speed of 0.1 to 2 DEG C/day, lifting the crystal from the liquid surface after the crystal grows up, and cooling to room temperature at the speed of 20 to 50 DEG C/hour to obtain the boron phosphate monocrystal. The fluxing agent used by the method can reduce the viscosity of the high temperature melt, is beneficial to melt mass transportation in the process of crystal growth, avoids the formation of inclusions in the crystal, and can stably grow the transparent boron phosphate monocrystal which has cm-level size, short ultraviolet cutoff wavelength and good mechanical processing performance, is not easy to crack, does not absorb moisture, and is easy to be stored.

The invention relates to borophosphate fluorescent powder capable of emitting green fluorescence as well as a preparation method and application of the borophosphate fluorescent powder. The chemical constitution general formula of the borophosphate fluorescent powder is (Ln1-xTbx)7O6(BO3)(PO4)2, wherein Ln represents rare earth elements, and x is more than or equal to 0.01 and less than or equal to 0.1. The preparation method of the borophosphate fluorescent powder capable of emitting green fluorescence comprises the following steps: (a) adding ground NH4H2PO4, H3BO3, Ln2O3 and Tb4O7 into a covered alumina crucible, and heating to react at 300-500 DEG C for 6-12 hours, so as to obtain a head product; (b) pressing the ground head product into a wafer with the diameter of 1cm-5cm, and adding the wafer into a covered platinum crucible; and (c) putting the platinum crucible in a heating furnace containing carbon powder, calcining at 1000-1500 DEG C for 12-30 hours, and naturally cooling to obtain the borophosphate fluorescent powder. By virtue of magnetic dipole transition of electrons on a terbium ion outer layer from <5>D4 to <7>F5, the borophosphate fluorescent powder is capable of emitting green fluorescence. The preparation method of the borophosphate fluorescent powder capable of emitting green fluorescence has the beneficial effects that utilized equipment is simple and safe to operate, conditions are easy to control, and the quality of a prepared product is reliable.

The present invention is fluxing agent growth process of gallium phosphate crystal. Through using lithium carbonate and molybdenum oxide as flux, gallium oxide and ammonium dihydrogen phosphate as main material, mixing ammonium dihydrogen phosphate, gallium oxide, lithium carbonate and molybdenum oxide in the weight ratio of 1 to 1.23 to 1.12 to 6.57, setting the mixture in platinum crucible, heating to melt inside growth furnace and cooling to the temperature of 10-20 deg.c over the solution saturation point to obtain the mixed melt of gallium phosphate and the flux, introducing seed crystal into the growth furnace, lowering the temperature to 1-2 deg.c over the solution saturation point when the seed crystal begins to melt and rotating the seed crystal in 30 rpm for 24 hr, gallium phosphate crystal is grown. After lowering the temperature, the crystal is taken out of the solution. The process can eliminate water from the crystal and raise the piezoelectric performance of the crystal.

The invention discloses a method for measuring the content of alloy elements in ferrosilicon and silicon-aluminum-barium-calcium by X-ray fluorescent spectrometry, belongs to the technical field of physicochemical detection, and aims to solve the technical problem of corrosion of a platinum crucible during a sample melting manufacturing process. According to the technical scheme, the method comprises four steps: (1) oxidizing and melting a sample; (2) melting and manufacturing a sample piece; (3) drawing a working curve; (4) measuring the content of the alloy elements in the sample, wherein a sample oxidizing and melting container is a ceramic crucible which is filled with graphite carbon powder being higher than or equal to 99.85 percent in purity; a mixed flux is formed by mixing potassium nitrate, boracic acid and anhydrous sodium carbonate in the weight ratio of 1:2:3. According to the method, the possibility of the corrosion of the platinum crucible during the sample melting process is eliminated thoroughly by selecting the oxidizing container and the mixed flux; the problem about accurately analyzing and measuring the content of the alloy elements in the ferrosilicon and the silicon-aluminum-barium-calcium by the X-ray fluorescent spectrometry is solved by controlling an oxidizing agent, the melting temperature and the time and optimizing the weight the weighed sample and various reagents; therefore, the method has a good popularization prospect.

The present invention is Bridgman-Stockbarge process of growing scintillation crystal LaCl3:Ce3+, and belongs to the field of monocrystal growing technology. The initial material LaCl3 .7H2O and CeCl3 .7H2O are first prepared into anhydrous chlorides LaCl3 and CeCl3 through chlorination, roasting and dewatering; and compounded material LaCl3:Ce3+ with proper CeCl3 doping concentration and small amount of active carbon powder blended as deoxidizer is then prepared. After filling the seed crystal and material are set inside platinum crucible and the crucible is sealed up, the crucible is set in crystal growing furnace at 920-980 deg.c for soldering the material to the seed crystal and forming solid-liquid interface of temperature gradient of 20-50 deg.c/cm, and the crucible is then fallen at the speed of 0.3-3 mm/hr to grow excellent LaCl3:Ce3+ monocrystal. The process is suitable for mass production of LaCl3:Ce3+ monocrystal.

The invention discloses a method for efficiently and accurately detecting the content of silicon dioxide in quartz sand. The method comprises the following steps: melting with analytically pure lithium tetraborate serving as a solvent at a high temperature in a platinum crucible to manufacture a sample wafer, namely a to-be-detected sample, required by a luminoscope, with analytically pure lithium tetraborate as a solvent before detection, adding 4N-level quartz sand to melt series standard samples, establishing a standard working curve, and finally, detecting and analyzing the to-be-detected sample according to the working curve to obtain the content of silicon dioxide. The standard samples and the to-be-detected sample are manufactured by melting through analytically pure lithium tetraborate, detection is performed by the luminoscope with the characteristics such as stable and rapid detection, and the weighed sample is large in amount and can generally reach 0.6-1.0g, which is 3-5 times the weight (0.2g) of a sample in a traditional alkali fusion detection method, so that the relative deviation during detection is much small. Moreover, analytically pure lithium tetraborate serves as the solvent, so that the melted sample is uniform and stable, and the detection result is real and reliable; and elements of analytically pure lithium tetraborate are light elements, matrix interference is almost avoided, and the reliability of the detection result obtained by the method provided by the invention is higher than that of the detection result obtained by the traditional method.

The invention discloses a method for measuring an element content in a ferrocolumbium alloy by X-fluorescence. The method comprises the following steps of: (1) hanging on a wall; (2) oxidizing; (3) smelting; (4) measuring fluorescence intensity and drawing a calibration curve; and (5) preparing a glass sample sheet to be sampled, measuring the spectral line intensity of columbium, thallium, silicon and phosphorus in the glass sample sheet to be sampled, and determining the percentage content of the columbium, thallium, silicon and phosphorus in a ferroniobium sample to be tested according to the calibration curve of the step (4). The ferroniobium glass sheet is successfully prepared by hanging lithium tetraborate on the wall and selecting barium peroxide as an oxidant for high-temperature fusion under the condition of no corrosion damage to a platinum crucible and provides a proper sample for measuring by using an X-fluorescence method. After an oxidization process of raising temperature gradually is adopted in particular, a very good oxidization effect can be achieved. The method can effectively improve the analysis speed of the element content in ferroniobium and the accuracy of analysis data and has the characteristics of simple operation and practicability.

The invention relates to a singleness phase white light fluorescent dye suitable for ultraviolet light and the manufacture method. It includes the following steps: grinding the raw material, putting into high purity corundum crucible or platinum crucible, putting into high-temperature furnace; under the condition of 1100-1400 degree centigrade and carbon or hydrogen deoxidization, heating 3-5 hours to gain the whit light fluorescent dye. The invention could be used in the new generation white light LED and the current fluorescent lamp.

This invention relates to a magnetic optical rotation glass, its components to molar percentage are: Tb2O3: 15 ~35 shares; B2O3 + SiO2: 40 ~ 80; Al2O3: 0 ~ 15; ZnO:0 ~ 30; ZrO2:0 ~ 6; AlF3 + MgF2+CaF2: 0 ~12; TiO2:0 ~ 10; InF3:0.5 ~ 7. First mix the raw materials according to composition; Preheat electric furnace to 1200 to 1300 deg C, add the mixed materials in the platinum crucible, when to 1350 to 1410 deg mix glass liquid for 3~ 5h; Reduce temperature to 1250 to 1350 deg C, pour glass liquid into the mold, precisely annealing in the annealing furnace. This invention use one time melting way, solve the problem of high temperature of glass clarification and leveling in the background technology, Rumsfeld constant is higher than the international common terbium magneto-optical glass, much higher than the magneto-optical glass containing cerium.

The invention relates to a method for recycling platinum from waste platinum crucibles. The method comprises 5 steps that: waste platinum crucibles are dissolved by using aqua regia; lead is removed by using a lead removing agent; platinum is precipitated by using ammonium chloride; platinum is refined; and platinum is calcined. According to the invention, waste platinum crucibles containing impurities such as lead, niobium, silicon and sodium are recycled as a platinum raw material; the raw material is dissolved by using aqua regia; concentrated sulfuric acid or water-soluble sulfate is added to the material, such that lead is pre-removed, and the frequency of repeated platinum precipitation by using ammonium chloride is reduced. Therefore, a platinum refining period is shortened, an agent dosage is reduced, a purification cost is reduced, and the purity of platinum sponge can be improved.