KR20030072836A - Fabrication of hollow spheres and tubes of iron(III) oxide - Google Patents

Fabrication of hollow spheres and tubes of iron(III) oxide Download PDF

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KR20030072836A
KR20030072836A KR1020020012080A KR20020012080A KR20030072836A KR 20030072836 A KR20030072836 A KR 20030072836A KR 1020020012080 A KR1020020012080 A KR 1020020012080A KR 20020012080 A KR20020012080 A KR 20020012080A KR 20030072836 A KR20030072836 A KR 20030072836A
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iron
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oxide
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정은선
임미선
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김영백
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide [Fe2O3]
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • C01P2004/34Spheres hollow

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Abstract

PURPOSE: A hollow sphere and tube manufactured using iron(III) oxide is provided which is used as catalyst for treating carbon monoxide and nitrogen oxide and applied to fabrication of electronic circuit, and a manufacturing method of the hollow sphere and tube manufactured using iron(III) oxide is provided. CONSTITUTION: The manufacturing method of hollow sphere and tube manufactured using iron(III) oxide comprises the steps of dissolving iron(III) acetoacetate into a biphilicity solvent; applying the dissolved solution to water having pH of 9 to 12 in which spherical and fiber type templates are dispersed so that an iron oxide film is formed on the surface of the templates; aging the mixture at the temperature range of 0 to 200 deg.C for 10 minutes to 24 hours; drying the washed mixture after washing the surface of the aged mixture; and removing the templates by burning the templates at temperature of about 600 deg.C, or decomposing the templates using acid or base according to nature of the templates so that the hollow sphere is obtained in case of spherical template, and tube is obtained in case of fiber type template, wherein the ion(III) oxide is reduced to iron by being reacted with carbon monoxide, hydrogen and incompletely oxidized nitrogen in any step, wherein the spherical template includes toluene, benzene, polystyrene dissolved toluene and benzene, hexane, mineral oil and paraffin oil, and surfactant such as TWEEN and cetyl ammonium bromide is additionally added to the spherical template, and wherein the fiber type template includes hair of animal, silk thread, cotton yarn, PET yarn and polylactate yarn.

Description

산화철로 제조된 전공구, 튜브 및 제조 방법 {Fabrication of hollow spheres and tubes of iron(III) oxide}Tools, tubes and manufacturing methods made of iron oxide {Fabrication of hollow spheres and tubes of iron (III) oxide}

본 발명은 여러 가지 유기 물질을 템플레이트로 하여 이를 산화철 전구체로 처리하여 산화철로 코팅하고 유기 물질을 가열하여 제거하거나 화학적으로 제거하여 나노 크기로부터 마이크론 크기에 이르는 산화철 혹은 철로 된 전공구와 튜브를 제조하는 것이다.In the present invention, various organic materials are used as templates, and the iron oxide precursors are coated with iron oxides, and the organic materials are heated and removed or chemically removed to prepare iron and iron tools and tubes ranging from nano size to micron size. will be.

본 발명은 촉매 및 전자 회로 제작에 응용될 수 있는 산화철, 철로 된 미세 전공 구와 튜브를 제조하는 것이다.The present invention is to produce micro-hole spheres and tubes of iron oxide, iron that can be applied to the production of catalysts and electronic circuits.

철(III) 아세토아세테이트를 양쪽친화성 용매에 녹이고 이를 템플레이트가 퍼져 있는 pH 9-12사이의 물에 가하면 산화철 막이 템플레이트의 표면에 생성된다. 이러한 혼합물을 섭씨 0도에서 200도 사이에서 10분-24시간 숙성시킨 후 표면을 씻어내고 건조 시킨 후, 섭씨 600도 정도에서 템플레이트를 태워 제거하거나, 템플레이트의 성질에 따라 산 또는 염기로 분해 시키면 구형의 템플레이트의 경우전공구, 섬유 형태의 템플레이트의 경우 튜브가 얻어진다. 산화철은 어느 단계에서든지 일산화 탄소, 수소 및 불완전 산화 질소와 반응시켜 철로 환원 시킬 수 있다.Iron (III) acetoacetate is dissolved in an affinity solvent and added to water between pH 9-12, where the template is spread, to form an iron oxide film on the surface of the template. After the mixture is aged between 0 and 200 degrees Celsius for 10 minutes-24 hours, the surface is washed and dried, and then burned and removed from the template at 600 degrees Celsius, or decomposed into acid or base depending on the properties of the template. In the case of a template, a tube is obtained in the case of a tool or a fiber-shaped template. Iron oxide can be reduced to iron at any stage by reaction with carbon monoxide, hydrogen and incomplete nitrogen oxides.

실시예 1Example 1

톨루엔 1mL와 pH 10의 물에 무게비 10%의 농도로 준비한 철(III) 아세토아세테이트 THF 용액을 몇 방울 가하고 구형 입자가 사라지지 않을 때까지 격렬히 교반한다. 교반하지 않아고 구형 입자가 형태를 유지하면 이를 상온에서 6시간 정도 방치 한 후 구형 입자를 떠내어 물에 세척한다. 톨루엔을 서서히 날려 보내면 구형 산화철 전공체가 얻어진다.Add a few drops of iron (III) acetoacetate THF solution prepared in a concentration of 10% by weight to 1 mL of toluene and pH 10 water and stir vigorously until the spherical particles do not disappear. If the spherical particles remain in the form without stirring, they are left at room temperature for about 6 hours and then the spherical particles are removed and washed in water. Slowly blowing off toluene yields a spherical iron oxide precursor.

실시예 2Example 2

폴리스타이렌 5% 및 TWEEN 3%가 녹아 있는 톨루엔 1mL와 pH 12의 물을 격렬히 교반하여 에멀젼을 제조한다. 이때 초음파 발생기를 사용하면 입자의 크기는 10-100nm, 호모게나이저를 사용하면 1-5 마이크로 미터, vortex나 손으로 교반하면 10-50 마이크로미터의 지름을 가지는 구를 얻어낼 수 있다. 이 에멀젼에 무게비 10% 농도의 철(III) 아세토아세테이트 THF 용액을 몇 방을 가한 후 상온에서 섭씨 70도 사이에서 4시간 숙성한 후 상온으로 식혀 물로 세척하면 구형 산화철/폴리스타이렌 전공구가 얻어진다. 이들을 공기중에서 건조한후, 일산화탄소가 흐르는 쿼르츠 튜브에 넣어 섭씨 80도에서 24시간 방치하면 산화철이 환원되어 철/폴리스타이렌 전공구가 얻어진다. 철/폴리스타이렌 전공구를 섭씨 600도까지 서서히 가열한 후 600도에서 24시간 방치하여 폴리스타이렌을 태워 제거하면 철 전공구가 얻어진다.An emulsion is prepared by vigorously stirring 1 mL of toluene in which 5% polystyrene and 3% TWEEN are dissolved and water at pH 12. At this time, the size of the particles is 10-100nm using the ultrasonic generator, 1-5 micrometers using the homogenizer, and a sphere having a diameter of 10-50 micrometers can be obtained by stirring with a vortex or by hand. Spherical iron oxide / polystyrene tools are obtained by adding several parts of iron (III) acetoacetate THF solution in a 10% weight ratio to the emulsion and aging for 4 hours at room temperature to 70 degrees Celsius. After drying in air, they are placed in a quartz tube flowing with carbon monoxide and left at 80 degrees Celsius for 24 hours to reduce iron oxide to obtain an iron / polystyrene tool. The iron / polystyrene tool is heated slowly to 600 degrees Celsius and left at 600 degrees for 24 hours to burn and remove polystyrene to obtain iron tools.

실시예 3Example 3

폴리스타이렌 5% 및 TWEEN 3%가 녹아 있는 톨루엔 1mL와 pH 12의 물을 격렬히 교반하여 에멀젼을 제조한다. 여기에 무게비 10% 농도의 철(III) 아세토아세테이트 THF 용액을 몇 방을 가한 후 상온에서 섭씨 70도에서 4시간 숙성한 후 상온으로 식혀 물로 세척하면 구형 산화철/폴리스타이렌 전공체가 얻어진다. 얻어진 전공체를 취하여 공기중에서 건조시킨 후 섭씨 600도까지 서서히 가열하고 600도에서 24시간 방치하여 산화철 전공체를 얻어낸다. 얻어진 산화철 전공체를 쿼르츠 튜브에서 일산화 탄소를 흘리며 섭씨 100도에서 200도 사이로 4시간에서 12시간 방치하면 환원된 철 전공구가 얻어진다.An emulsion is prepared by vigorously stirring 1 mL of toluene in which 5% polystyrene and 3% TWEEN are dissolved and water at pH 12. After adding several rooms of the iron (III) acetoacetate THF solution in a concentration of 10% by weight and aging for 4 hours at 70 degrees Celsius at room temperature, it is cooled to room temperature and washed with water to obtain a spherical iron oxide / polystyrene precursor. The obtained whole body is taken out, dried in air, and gradually heated to 600 degrees Celsius, and left at 600 degrees for 24 hours to obtain an iron oxide precursor. The obtained iron oxide precursor was left for 4 to 12 hours at 100 to 200 degrees Celsius with carbon monoxide flowing from a quartz tube to obtain a reduced iron tool.

실시예 4Example 4

개털이나 사람의 머리털을 pH 10 물에 넣고 여기에 10% 농도로 준비한 철(III) 아세틸 아세테이트 THF 용액을 몇 방울 가하고 상온에서 24시간 방치한다. 얻어진 물질을 섭씨 600도에서 가열하여 털을 제거하면 산화철로 된 튜브가 얻어진다.Place hair or human hair in pH 10 water, add a few drops of iron (III) acetyl acetate THF solution prepared at 10% concentration, and leave at room temperature for 24 hours. The obtained material is heated at 600 degrees Celsius to remove the hair, which results in a tube of iron oxide.

실시예 5Example 5

명주실 0.1g을 pH 10의 물 5mL에 넣고 여기게 철(III) 아세틸 아세테이트 10% THF용액 0.5 mL를 가한 후 상온에서 4시간 내지 24시간 방치한다. 얻어진 생성물을 물로 세척한 후 공기중에서 말린 후 이를 일산화 탄소가 흐르는 쿼르츠 튜브에 넣고 섭씨 100-200도로 12-24시간 가열한다. 얻어진 생성물을 600도까지 온도를 서서히 올린 후 600도에서 24시간 방치하여 명주실을 태워 없애면 철 튜브가 얻어진다.0.1 g of silk thread is added to 5 mL of water at pH 10, and 0.5 mL of iron (III) acetyl acetate and 10% THF solution are added thereto, followed by 4 to 24 hours at room temperature. The product obtained is washed with water and dried in air and then placed in a quartz tube with carbon monoxide and heated to 100-200 degrees Celsius for 12-24 hours. The obtained product was gradually raised to 600 degrees and left at 600 degrees for 24 hours to burn off the silk thread to obtain an iron tube.

실시예 6Example 6

폴리에스터 원사 0.1g을 pH 11의 물 5 mL에 넣고 여기에 철(III) 아세틸 아세테이트 10% 아세톤 용액 0.5 mL를 가한 후 상온에서 4시간 내지 24시간 방치한다. 얻어진 생성물을 물로 세척한 후, 공기 중에서 말리고 이를 튜브형 로에서 섭씨 600도까지 온도를 서서히 올린 후 600도에서 24시간 방치하여 폴리에스터 원사를 태워 없앤 후 산화철 튜브를 얻어낸다. 생성된 산화철 튜브를 쿼르츠 튜브에 넣고 일산화 탄소가 흐르게 하여 섭씨 100도에서 200도에서 12-24시간 가열하여 철 튜브를 얻어낸다.0.1 g of polyester yarn is added to 5 mL of water at pH 11, and 0.5 mL of iron (III) acetyl acetate 10% acetone solution is added thereto and left at room temperature for 4 to 24 hours. The obtained product was washed with water, dried in air and gradually heated to 600 degrees Celsius in a tubular furnace and left at 600 degrees for 24 hours to burn off the polyester yarn to obtain an iron oxide tube. The resulting iron oxide tube was placed in a quartz tube and carbon monoxide was flowed and heated at 100 ° C. to 200 ° C. for 12-24 hours to obtain an iron tube.

본 발명은 산화철로 된 속이 빈 구 및 튜브를 제조할 수 있어 일산화 탄소 및 산화질소를 처리하는 촉매로 사용할 수 있으며, 이들을 환원시키면 철로된 미세 전공구와 튜브를 제조할 수 있어 여러 가지 자성 물질로 응용할 수 있다.The present invention can be used to produce hollow spheres and tubes made of iron oxide can be used as a catalyst for treating carbon monoxide and nitric oxide, reducing them can produce a fine electric tool and tube made of iron to various magnetic materials It can be applied.

Claims (7)

철(III) 아세토아세테이트를 구형 템플레이트 및 선형 템플레이트가 들어 있는 pH 8-12의 물 혼합물에 가하여 템플레이트를 산화철로 코팅하는 방법.The iron (III) acetoacetate is added to a water mixture of pH 8-12 containing spherical and linear templates to coat the template with iron oxide. 1항으로부터 얻어진 물질Substances obtained from paragraph 1 1항에 있어 구형 템플레이트로는 톨루엔, 벤젠, 폴리스타이렌이 녹아 있는 톨루엔 및 벤젠, 헥산, 미네랄 오일, 파라핀 오일 등을 그대로 사용하거나 TWEEN 및 세틸암모니윰 브로마이드와 같은 계면 활성제를 첨가하여 안정화 시킨 방울을 사용하는 방법.As for the spherical template, toluene, benzene, toluene dissolved in polystyrene and benzene, hexane, mineral oil, paraffin oil, etc. are used as it is or stabilized by adding a surfactant such as TWEEN and cetyl ammonium bromide. How to. 1항에 있어 선형 템플레이트로는 동물의 털, 명주 실, 무명 실, PET실, 폴리락테이트 실 등을 사용하는 방법.The method of claim 1, wherein the linear template is animal hair, silk yarn, cotton yarn, PET yarn, polylactate yarn, or the like. 1항으로부터 얻어진 물질을 일산화탄소, 수소, 및 불완전산화질소 (NOx)와 환원 반응시켜 얻어지는 철이 성분중 하나인 구조물.A structure wherein iron obtained by the reduction reaction of the material obtained from claim 1 with carbon monoxide, hydrogen, and incomplete nitrogen oxide (NOx) is one of the components. 1항으로부터 얻어진 물질을 섭씨 600도에서 가열하거나 섭씨 150도 이하에서 산 혹은 염기로 처리하여 템플레이트를 제거하여 얻어지는 구 및 튜브형태의 산화철이 성분 중 하나인 구조물.A structure in which the iron oxide in the form of a sphere and a tube obtained by removing a template by heating a material obtained from paragraph 1 at 600 degrees Celsius or treating it with an acid or a base at 150 degrees Celsius or less. 5항으로부터 얻어진 물질을 섭씨 600도에서 가열하거나 섭씨 150도 이하에서 산 혹은 염기로 처리하여 템플레이트를 제거하여 얻어지는 구 및 튜브형태의 철 구조물.A steel structure in the form of spheres and tubes obtained by removing the template by heating the material obtained from paragraph 5 at 600 degrees Celsius or treating it with acid or base at 150 degrees Celsius or less.
KR1020020012080A 2002-03-07 2002-03-07 Fabrication of hollow spheres and tubes of iron(III) oxide KR20030072836A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108374163A (en) * 2016-12-22 2018-08-07 中国航空制造技术研究院 A kind of preparation method of microarray structure
CN112608403A (en) * 2020-11-20 2021-04-06 西安交通大学 Preparation method and application of high-stability polymer microsphere @ all-inorganic lead-halogen perovskite quantum dot

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108374163A (en) * 2016-12-22 2018-08-07 中国航空制造技术研究院 A kind of preparation method of microarray structure
CN112608403A (en) * 2020-11-20 2021-04-06 西安交通大学 Preparation method and application of high-stability polymer microsphere @ all-inorganic lead-halogen perovskite quantum dot

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