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131 results about "Methane sulfonate" patented technology

Micro-pore electroplated copper filling method for three-dimensional (3D) copper interconnection high aspect ratio through-silicon-via technology

The invention discloses a micro-pore electroplated copper filling method for a three-dimensional (3D) copper interconnection high aspect ratio through-silicon-via technology. The micro-pore electroplated copper filling method comprises the following steps of: 1, preparing an electroplating solution of a copper methane sulfonate system; 2, wetting micro pores of the through-silicon-via technology through electroplating pretreatment; 3, electrifying and slotting, and increasing the ultralow current diffusion step, so that the copper ion and additives are reasonably distributed on the surfaces and inside the micro pores through the through-silicon-via technology; 4, connecting a silicon wafer where the through-silicon-via technology is positioned with a cathode of a power supply, so that the electroplating surface of the wafer is completely soaked in the electroplating solution, step-by-step current electroplating is performed under the condition that the cathode is rotated or stirred, and the electroplating conditions comprise the current density of 0.01-10A / dm<2> and the temperature of 15-30 DEG C; and 5, completely and thoroughly washing the wafer by using deionized water, performing spin-dry or blow-dry. The provided micro-pore electroplated copper filling method for the 3D copper interconnection high aspect ratio through-silicon-via technology is high in pore filling speed and thin in surface copper, hole and crack risks are avoided, and complete filling of high-difficulty hole with the depth-to-width ratio of more than 10:1 can be realized.
Owner:SHANGHAI SINYANG SEMICON MATERIALS

Method for detecting methyl methane sulfonate by gas chromatography and tandem mass spectrometry

The invention discloses a method for detecting methyl methane sulfonate by gas chromatography and tandem mass spectrometry. The method is characterized by comprising the following steps: (1) placing a sample to be detected into a volumetric flask, adding acetonitrile to make up to the volume of 10 to 25 ml, carrying out vortex mixing for 1 to 5 min, carrying out ultrasonic extraction for 10 to 15 min, sieving the obtained product by a filter membrane with the specification of 0.22 [mu]m and carrying out sample injection to detect the methyl methane sulfonate in the sample; (2) under the detection conditions, using a gas chromatography and tandem mass spectrometry combined instrument GC-MS/MS as a detection instrument for detecting the methyl methane sulfonate. In the step (1), 0.05 to 0.50 g of the sample to be detected is taken, accuracy reaches 0.1 mg, the sample to be detected is placed in the volumetric flask, the acetonitrile is added to make up to the volume of 10 to 25 ml, vortex mixing is carried out for 1 to 5 min and ultrasonic extraction is carried out for 10 to 15 min. the method can simply, rapidly, conveniently and efficiently carry out qualitative and quantitative detection on MMS (methyl methane sulfonate) in medicine raw materials, chemical reagents and foods by using the GC-MS/MS.
Owner:JIANGSU SINOGRAPHY TESTING

Paecilomyces thermophila mutant strain and mutation induction method and application thereof

The invention discloses a Paecilomyces thermophila mutant strain and a mutation induction method and application thereof. The mutation induction method includes: Paecilomyces thermophila screened from high-temperature-fermented compost and used for producing high-temperature-resistant and acid-resistant glucose oxidase is used as the original strain, protoplast ultraviolet and ethyl methane sulfonate compound mutation induction is performed, and the screened strain is subjected to budding spore diethyl sulfate-microwave compound mutation induction to obtain the Paecilomyces thermophila mutant strain. The Paecilomyces thermophila mutant strain is preserved in China General Microbiological Culture Collection Center on January 11th, 2016, and the preservation number of the mutant strain is CGMCC No. 13182. Compared with a conventional mutation induction method, the mutation induction method has the advantages that the method is high in efficiency and simple in fast in screening, the productivity of the mutant strain is high, the yield of the mutant stain is 277.65% of that of the Paecilomyces thermophila original strain, fermentation liquor enzyme activity reaches 185U/ml, production cost is lowered, and the glucose oxidase produced by the mutant strain is good in high-temperature resistance and acid resistance and can be used as feed enzyme applied to feed industry.
Owner:XUZHOU UNIV OF TECH

Method and device for preparing tin methane sulfonate through hydrogen-free electrolysis

The invention provides a method for preparing tin methane sulfonate through hydrogen-free electrolysis, and relates to the field of manufacturing the tin methane sulfonate through industrial electrolytic synthesis and can be used for directly preparing a tin methane sulfonate solution through using an electrolytic process. According to the method provided by the invention, electrolyte is a methanesulfonic acid solution; a cathode of an electrode is a gas diffusion electrode, and an anode of the electrode is solid tin; the cathode and the anode are separated through a membrane; the electrolyte temperature is controlled within a range of 0-60 DEG C; a current density is set within a range of 10-800 A/m<2>; the electrolyte is stopped until a content of free methyl sulfuric acid in the anode electrolyte is up to 0.1-10 g/L; and the anode electrolyte is filtered and concentrated, so as to prepare the tin methane sulfonate solution with different concentrations. The method provided by the invention is suitable for being carried out at the constant temperature and the constant pressure, so that the tin methane sulfonate solution with high purity can be directly obtained. The method provided by the invention has the characteristics of being simple in process, free from separation, high in product purity, low in energy consumption and low in cost.
Owner:宜兴方晶科技有限公司

Method for synthesizing crylic acid by catalyzing acetylene carbonyl through palladium

The invention provides a method for synthesizing crylic acid by catalyzing acetylene carbonyl through palladium. Acetylene, carbon monoxide and water are used as raw materials and are catalyzed to synthesize the crylic acid under the conditions that the reaction temperature is between 15 and 70 DEG C and the pressure is between 1.5 and 6MPa. The adopted catalyst uses palladium diacetate as a main catalyst; the dosage of the main catalyst is less than that of a traditional nickel-copper catalyst and is only 1/50; sulfoacid, such as methane sulfonate, trifluoromethane sulfonic acid, p-toluenesulfonic acid or the like, serves as an aid; an addition amount of the additive is that the ratio of n(-SO3H) to n(Pd2<+>) is equal to 1:1-10:1; and organic phosphine such as 2-pyridyl diphenylphosphine (2-PyPPh2) as a ligand. Compared with the nickel-copper catalyst, the catalyst has remarkable advantages that: under the mild conditions, such as the temperature of 40 DEG C and the pressure of 5 MPa, the catalyst can catalyze the acetylene carbonyl to synthesize the crylic acid at high efficiency, can effectively avoid the acetylene and the crylic acid undergoing polymerization and other side reactions, saves energy, and has safe operation and low operating expense.
Owner:CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI

Screening method for glyphosate-resisting medicago sativa plants

The invention mainly provides a medicago sativa plant resistant to herbicide and a method, particularly relates to a method for screening medicago sativa plants resistant to the herbicide by utilizing chemical mutagen EMS (ethyl methane sulfonate) for mutagenesis of medicago sativa, and discloses a culture medium screening method for glyphosate-resisting medicago sativa plants. The method is characterized by including the following steps: (1) germinating seeds by an MS culture medium; (2) performing dosage screening; (3) subjecting medicago sativa seeds to mutagenesis by median lethal dose of the EMS; (4) screening the glyphosate-resisting medicago sativa plants; (5) rescreening the resistant plants. The method has the advantages of being simple and easy to implement, taking effect fast and capable of allowing single plants of herbicide-resistant medicago sativa to be obtained within a short time. A mutagenesis way is adopted. The chemical mutagen EMS is utilized to mutate the medicago sativa seeds to generate point mutation, the single plants of the herbicide-resistant medicago sativa are screened by two ways of the culture medium and soil screening, new germplasm resources are provided for conventional breeding, and certain references are provided for herbicide-resistant breeding of other plants.
Owner:LANZHOU UNIVERSITY

Method for producing mutant of hemerocallis middendorffii by in vitro mutagenesis of ethyl methane sulfonate

A method for producing mutant of hemerocallis middendorffii by in vitro mutagenesis of ethyl methane sulfonate (EMS) amis to provide an EMS in vitro mutagenesis method for breed improvement of hemerocallis and creation of new germplasm resources and to obtain a target variant strain. The method for producing the mutant of the hemerocallis middendorffii by the in vitro mutagenesis of the ethyl methane sulfonate adopts the 1 to 2cm flower buds in normal growth and development state of the hemerocallis middendorffii as materials, inoculates callus induced by taking ovaries as explants to a differential medium, and green buds are differentiated. After the callus with buds is subjected to differentiation culture for 10 days, a callus block is treated with EMS semi-lethal dose at a concentration of 0.75-1.0 percent (w/v). The treated callus is inoculated to the differentiation medium for differentiation culture to obtain regenerated plants. When the regenerated plants grow to 1 to 2 cm high, the regenerated plants are cut down from the callus and put in a subculture medium to conduct subculture for 15 days, hemerocallis septoria tritici toxin semi-lethal dose at a concentration of 40 percent (v/v) is taken as directional selection pressure for stress screening, and disease-resistant mutant plants are obtained.
Owner:INST OF DRY LAND FARMING SHANXI ACAD OF AGRI SCI

Method for preparing solution of tin methane sulfonate

The invention relates to a method for preparing a solution of tin methane sulfonate for electroplating. The method is characterized by comprising the following steps that: 1) an anion exchange membrane is used for dividing an electrolytic cell into a cathode chamber and an anode chamber, wherein the electrolyte used in the anode chamber is a solution of methane sulfonic acid with the mass concentration of between 20 and 40 percent, and the electrolyte used in the cathode chamber is a solution of methane sulfonic acid with the mass concentration of between 10 and 50 percent; the anode in the anode chamber is made of a tin plate or tin flower, and the cathode in the cathode chamber is made of a tin plate or copper plate; and 2) the anode and the cathode are connected with a DC power supply for electrolysis, the electrolytic temperature is between 20 and 60 DEG C, and under the action of the DC with the voltage of 1.8 to 3V, the anode is subjected to anodic dissolution and enters the anode chamber; and when the concentration of tin ion in the anode chamber reaches between 100 and 130g/L, the electrolysis stops, and the electrolyte in the anode chamber is taken out and filtered, and the filtrate is subjected to vacuum concentration at a temperature of between 40 and 120 DEG C, so that the solution of tin methane sulfonate, of which the content of tin ion is 300 to 310g/L, can be obtained. The method has the advantages of less equipment investment, simple process and high product purity.
Owner:XIAOCHANG GOLDEN COCK CHEM

Method for preparing micro-nano needle conical structure for copper interconnection by electrochemical deposition

The invention discloses a method for preparing micro-nano needle conical structure for copper interconnection by electrochemical deposition; a conductive base material is used as a cathode and is placed in a electroplating solution containing copper ions, complexing agents and additives, after current is applied, the electrocrystallization grows vertically along one-dimension which is vertical to the surface direction, thereby the micro-nano needle conical structure for copper interconnection is formed on the conductive base material surface; the copper ion is provided by copper methane sulfonate or is mainly provided by copper methane sulfonate, and is supplemented by more than one or two of cupric chloride, copper pyrophosphate and cupric nitrate. The invention provides a preparation method which has the advantages of simple process, low cost without special requirements for substrate shape and material, and is suitable for industrialized batch production of micro-nano needle conical structure for copper interconnection; in addition, according to the preparation method provided by the invention, a copper needle conical crystal structure can be directly formed on the surface of the required base material, and the structure can be used as device and material, thereby providing possibility for realization of industrialized production and wide application.
Owner:SHANGHAI JIAO TONG UNIV

Preparation method of 1-(4, 5-dihydro-2-thiazolinyl)-3-mercaptoazetidine hydrochloride

The invention discloses a method for synthesis of 1-(4, 5-dihydro-2-thiazolinyl)-3-mercaptoazetidine hydrochloride. With 2-methylthio-2-thiazoline (I) as the raw material, the method of the invention comprises the steps of: in the presence of alkali, reacting 2-methylthio-2-thiazoline (I) with 3-hydroxyazetidine hydrochloride so as to obtain 1-(4, 5-dihydro-2-thiazolinyl)-3-hydroxyazetidine (II), and reacting (II) with methyl sulfonylchloride in the presence of alkali so as to obtain 1-(4, 5-dihydro-2-thiazolinyl)-3-methane sulfonate group azetidine (III), subjecting (III) to a reaction with potassium thioacetate so as to obtain 1-(4, 5-dihydro-2-thiazolinyl)-3-thioacetic acid ester group azetidine (IV), in the presence of alkali, subjecting (IV) to hydrolysis and then to acidification with dilute hydrochloric acid, thus obtaining the 1-(4, 5-dihydro-2-thiazolinyl)-3-mercaptoazetidine hydrochloride (V). With easily available and inexpensive starting material, the method of the invention simplifies the synthesis route, improves the raw material utilization ratio and the overall yield. An intermediate obtained in the reaction can be subjected to refinement by a recrystallization method or to a next reaction directly, so that the yield is high and the "three wastes" produced during the reaction process are few. In addition, with low cost, the method of the invention is beneficial for industrial production.
Owner:GUANGZHOU BAIYUNSHAN PHARMA HLDG CO LTD BAIYUNSHAN PHARMA GENERAL FACTORY

Electroplating copper cylinder solution suitable for oversize current density and electroplating method

The invention discloses an electroplating copper cylinder solution suitable for the oversize current density and an electroplating method. The electroplating copper cylinder solution comprises the following components by concentration: 150-240 g / L of copper methane sulfonate, 40-70 g / L of methanesulfonic acid, 30-50 mg / L of chloridion, 2-5 mg / L of bis-(sodium sulfopropyl)-disulfide, 40-100 mg / L ofpolyethylene glycol, 40-80 mg / L of Janus green, and the balance of DI pure water. The components are evenly mixed to form the electroplating copper cylinder solution suitable for the oversize currentdensity; before electroplating, a wafer needs to be subjected to vacuum treatment through a pretreatment solution; the pretreatment solution is the DI pure water, the wafer is mounted through an electroplating hanger, and then is vacuumized in vacuum equipment for 5-10 min through the DI pure water; and after vacuumizing, electroplating is conducted in the electroplating copper cylinder solution.According to the electroplating copper cylinder solution provided by the invention, the problem is completely solved, especially through adding of the Janus green, an additive is adsorbed on the surface of a seed layer, a copper cylinder is evenly electroplated on the surface of a substrate, and performance indexes that scorch is avoided, and the arch rate is less than or equal to 5% can be met.
Owner:江苏矽智半导体科技有限公司
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