KR20220031181A - Fabricating Method of Metal Nano Catalyst using Ionic Liquid - Google Patents
Fabricating Method of Metal Nano Catalyst using Ionic Liquid Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 90
- 239000002184 metal Substances 0.000 title claims abstract description 90
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 65
- 239000011943 nanocatalyst Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims description 38
- 239000002243 precursor Substances 0.000 claims abstract description 56
- 239000002798 polar solvent Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 230000001678 irradiating effect Effects 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims description 20
- 239000012876 carrier material Substances 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- -1 pyridizinium Chemical compound 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- WTKZEGDFNFYCGP-UHFFFAOYSA-O Pyrazolium Chemical compound C1=CN[NH+]=C1 WTKZEGDFNFYCGP-UHFFFAOYSA-O 0.000 claims description 3
- RWRDLPDLKQPQOW-UHFFFAOYSA-O Pyrrolidinium ion Chemical compound C1CC[NH2+]C1 RWRDLPDLKQPQOW-UHFFFAOYSA-O 0.000 claims description 3
- 125000001931 aliphatic group Chemical group 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910021482 group 13 metal Inorganic materials 0.000 claims description 3
- ZCQWOFVYLHDMMC-UHFFFAOYSA-O hydron;1,3-oxazole Chemical compound C1=COC=[NH+]1 ZCQWOFVYLHDMMC-UHFFFAOYSA-O 0.000 claims description 3
- CZPWVGJYEJSRLH-UHFFFAOYSA-O hydron;pyrimidine Chemical compound C1=CN=C[NH+]=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-O 0.000 claims description 3
- 150000002602 lanthanoids Chemical group 0.000 claims description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical compound C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 claims description 3
- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- 150000003624 transition metals Chemical class 0.000 claims description 3
- 125000001425 triazolyl group Chemical group 0.000 claims description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000002082 metal nanoparticle Substances 0.000 description 31
- 230000008569 process Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 239000002105 nanoparticle Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
Description
본 발명은 이온성 액체를 이용한 금속 나노 촉매 제조방법에 관한 것으로, 특히 균일한 크기의 금속 나노입자 제조가 가능하고, 이온성 액체에 잘 분산되지 않은 난용성 금속 전구체를 사용하더라도 금속 나노입자를 제조할 수 있는 이온성 액체를 이용한 금속 나노 촉매 제조방법에 관한 것이다.The present invention relates to a method for manufacturing a metal nanocatalyst using an ionic liquid, in particular, it is possible to prepare metal nanoparticles of a uniform size, and even if a sparingly soluble metal precursor that is not well dispersed in an ionic liquid is used, the metal nanoparticles are prepared It relates to a method for preparing a metal nano-catalyst using an ionic liquid that can do this.
나노입자란 한 차원이 100㎚ 이하인 입자로, 분자나 원자를 조작하여 새로운 소재, 구조, 기계, 기구, 소자를 제작하고, 그 구조를 연구하는 나노기술의 영역에 속하는 입자다.Nanoparticles are particles with a dimension of 100 nm or less, which belong to the field of nanotechnology, which manipulates molecules or atoms to manufacture new materials, structures, machines, instruments, and devices, and to study the structures.
이러한, 나노입자 물질들은 동일한 화학적 조성임에도 불구하고 급격하게 늘어난 비표면적과 양자역학적 효과에 의해 벌크 상태와는 전혀 다른 광학적, 전자기적 성질을 갖는다.Although these nanoparticle materials have the same chemical composition, they have optical and electromagnetic properties completely different from those in the bulk state due to a sharply increased specific surface area and quantum mechanical effect.
나노입자 중 금속 나노입자는 종류가 다양한 만큼 응용범위도 매우 넓은데, 벌크 입자와는 다른 독특한 광학적, 자기적, 전기적, 화학적 특성 때문에 촉매, 센서, 연마제, 항균, 사진 필름용 감광제, 페인트, 디스플레이 분야 등 여러 산업분야에 이용되고 있으며, 입자의 크기와 분포에 따라 커다란 성능 차이를 갖게 된다.Among nanoparticles, metal nanoparticles have a wide range of applications as there are many different types. Because of their unique optical, magnetic, electrical, and chemical properties different from bulk particles, they are used as catalysts, sensors, abrasives, antibacterial agents, photoresists for photographic films, paints, displays. It is used in various industrial fields, such as the field, and has a large performance difference depending on the size and distribution of particles.
이러한, 금속 나노입자를 제조하는 방법으로는 크게 물리적 제조법과 화학적 합성법이 있는데, 물리적 제조법의 경우에는 기상에서의 균질 핵 생성과 응축을 통해 제조하는 가스 응축법과 벌크 금속을 분쇄하여 나노화하는 기계적 분쇄법이 있으나, 기계적 분쇄법의 경우 분쇄하는 입자의 크기에 한계가 있고, 입자의 입도 분포와 입자의 크기가 크며, 입자를 분쇄하기 위해 많은 에너지와 설비비용이 들지만 그에 비해 제조되는 양이 매우 작은 문제가 있다.Methods for manufacturing such metal nanoparticles include a physical manufacturing method and a chemical synthesis method. In the case of the physical manufacturing method, a gas condensation method prepared through homogeneous nucleation and condensation in the gas phase and a mechanical crushing method of pulverizing bulk metal into nanoparticles However, in the case of mechanical grinding, there is a limit to the size of the particles to be pulverized, the particle size distribution and the size of the particles are large, and a lot of energy and equipment cost to pulverize the particles, but the quantity produced is very small compared to that. there is
한편, 화학적 합성법은 최근 가장 많이 사용되는 방법으로 반응이 일어나는 영역에 따라 기상반응, 액상반응, 고상반응으로 분류되고, 화학반응에서는 반응에 수반되는 에너지를 활용할 수 있으므로 적은 양의 에너지 투입으로 합성이 가능하며 합성반응의 속도가 빠르고 균일한 반응 제어가 가능하다는 장점이 있으나, 불순물 제거가 어려운 문제가 있다.On the other hand, chemical synthesis method is the most recently used method and is classified into gas phase reaction, liquid phase reaction, and solid phase reaction depending on the area where the reaction takes place. It is possible and has the advantage that the speed of the synthesis reaction is fast and uniform reaction control is possible, but there is a problem in that it is difficult to remove impurities.
즉, 화학적 합성법에서는 환원이 완료된 나노입자 용액에서 환원제를 다시 제거할 때 환원제가 확실히 제거되지 않을 뿐만 아니라 제거 공정 또한 매우 복잡하고, 환원제 제거 후 나노입자를 다시 용매에 분산시키는 과정이 필요한데, 이 과정 또한 완벽히 이루어지지 않아 침전현상이 생기는 문제가 있다.That is, in the chemical synthesis method, when the reducing agent is removed again from the reduced nanoparticle solution, the reducing agent is not reliably removed, and the removal process is also very complicated. In addition, there is a problem that the precipitation phenomenon occurs because it is not done completely.
이러한 문제를 해결하기 위해 최근에는 일본 공개특허 제2015-117395호에 개시된 바와 같이 이온성 액체를 이용한 금속 나노입자 제조방법이 이용되고 있다. 이때, 이온성 액체는 양이온과 음이온만으로 구성되는 염(salt)임에도 불구하고 상온에서 액체 상태를 유지하는 화합물을 말하며, 고온 안정성이 높고, 액체 온도 범위가 넓으며, 점성이 높고, 증기압이 매우 낮으며, 높은 산화·환원 내성을 갖는 특성을 지니고 있어 환원제 등과 같은 불순물 없이 금속 나노입자를 제조할 수 있다.In order to solve this problem, recently, as disclosed in Japanese Patent Application Laid-Open No. 2015-117395, a method for manufacturing metal nanoparticles using an ionic liquid has been used. At this time, the ionic liquid refers to a compound that maintains a liquid state at room temperature despite being a salt composed of only positive and negative ions, has high high temperature stability, wide liquid temperature range, high viscosity, and very low vapor pressure. and has high oxidation/reduction resistance, it is possible to manufacture metal nanoparticles without impurities such as reducing agents.
그러나, 상기의 일본 공개특허에서는 금속 타겟에 대해 레이저 절삭(laser ablation)을 행하여 금속 나노입자를 제조하기 때문에 균일한 크기의 금속 나노입자 제조가 용이하지 않고, 레이저 조사에 의해 생성된 미립자가 이온성 액체에서 성장하기 위해서는 미립자가 이온성 액체 내에 분산되어야 하나, 이온성 액체와 금속의 특성에 따라 이온성 액체 내에 분산되지 않은 경우 금속 나노입자 제조가 불가능한 문제가 있다.However, in the above Japanese Laid-Open Patent Publication, it is not easy to manufacture metal nanoparticles of a uniform size because metal nanoparticles are manufactured by laser ablation on a metal target, and fine particles generated by laser irradiation are ionic. In order to grow in a liquid, the fine particles must be dispersed in the ionic liquid, but depending on the properties of the ionic liquid and the metal, if not dispersed in the ionic liquid, there is a problem in that metal nanoparticles cannot be manufactured.
따라서, 본 발명은 상기와 같은 문제를 해결하기 위한 것으로, 균일한 크기의 금속 나노입자 제조가 가능하고, 이온성 액체에 잘 분산되지 않은 난용성 금속전구체를 사용하더라도 금속 나노입자를 제조할 수 있는 이온성 액체를 이용한 금속 나노 촉매 제조방법에 관한 것이다.Therefore, the present invention is to solve the above problems, and it is possible to manufacture metal nanoparticles of a uniform size, It relates to a method for preparing a metal nano-catalyst using an ionic liquid.
상술한 목적을 이루기 위해, 본 발명에 따르면, 금속 전구체를 극성 용매에 용해시키는 단계; 상기 금속 전구체가 용해된 용해액과 이온성 액체가 혼합된 혼합물을 제조하는 단계; 및 상기 혼합물에 마이크로웨이브를 조사하는 단계를 포함한다.In order to achieve the above object, according to the present invention, the step of dissolving a metal precursor in a polar solvent; preparing a mixture in which a solution in which the metal precursor is dissolved and an ionic liquid are mixed; and irradiating the mixture with microwaves.
본 발명에 따르면, 상기 금속 전구체와 극성 용매는 1:1 ~ 1:10의 농도 비율로 혼합되는 것을 특징으로 한다.According to the present invention, the metal precursor and the polar solvent are mixed in a concentration ratio of 1:1 to 1:10.
본 발명에 따르면, 상기 금속 전구체는 상기 이온성 액체에 0.1mM/L ~ 50mM/L 농도로 혼합되는 것을 특징으로 한다.According to the present invention, the metal precursor is characterized in that the ionic liquid is mixed at a concentration of 0.1mM / L ~ 50mM / L.
본 발명에 따르면, 상기 금속 전구체의 금속은 2족 금속, 3족 금속, 12족 금속, 13족 금속, 전이 금속, 란타넘족 및 이들의 조합물로 이루어진 군으로부터 선택되는 것을 특징으로 한다.According to the present invention, the metal of the metal precursor is selected from the group consisting of a Group 2 metal, a Group 3 metal, a Group 12 metal, a Group 13 metal, a transition metal, a lanthanide, and combinations thereof.
본 발명에 따르면, 상기 극성 용매에는 2개의 서로 다른 금속 전구체가 용해되는 것을 특징으로 한다.According to the present invention, it is characterized in that two different metal precursors are dissolved in the polar solvent.
본 발명에 따르면, 상기 이온성 액체는 지방족계, 피라졸륨계, 트리아졸륨계, 티아졸륨계, 옥사졸륨계, 피리디지늄계, 피리미디늄계, 암모늄계, 포스포늄계, 설포늄계, 피리디늄계, 피롤리디늄계, 및 이들의 조합물로 이루어진 군에서 선택되는 것을 특징으로 한다.According to the present invention, the ionic liquid is aliphatic, pyrazolium, triazolium, thiazolium, oxazolium, pyridizinium, pyrimidinium, ammonium, phosphonium, sulfonium, pyridinium , pyrrolidinium-based, and characterized in that it is selected from the group consisting of combinations thereof.
본 발명에 따르면, 상기 혼합물을 제조하는 단계는, 상기 금속 전구체가 용해된 용해액과 함께 담체 소재가 이온성 액체에 혼합되는 단계를 더 포함하는 것을 특징으로 한다.According to the present invention, the step of preparing the mixture is characterized in that it further comprises the step of mixing the carrier material with the dissolved solution in which the metal precursor is dissolved in the ionic liquid.
본 발명에 따르면, 상기 담체 소재는 그래핀, 그라파이트, 카본 블랙, 카본 나노튜브, 전도성 산화물 중 어느 하나인 것을 특징으로 한다.According to the present invention, the carrier material is characterized in that any one of graphene, graphite, carbon black, carbon nanotubes, and conductive oxides.
본 발명에 따르면, 상기 담체 소재는 상기 금속 전구체에 비해 1 ~ 10배 정도의 농도로 이온성 액체에 혼합되는 것을 특징으로 한다.According to the present invention, the carrier material is characterized in that it is mixed with the ionic liquid at a concentration of about 1 to 10 times that of the metal precursor.
본 발명에 따르면, 상기 혼합물을 제조하는 단계는, 상기 혼합물에 초음파를 조사하는 단계를 더 포함하는 것을 특징으로 한다.According to the present invention, the step of preparing the mixture is characterized in that it further comprises the step of irradiating ultrasonic waves to the mixture.
본 발명에 따르면, 이온성 액체 내에 균일하게 분산된 금속 전구체에 마이크로웨이브를 조사하여 균일한 에너지를 공급하기 때문에 균일한 크기의 금속 나노입자 제조가 가능하고, 금속 전구체를 극성 용매에 용해시킨 후 이온성 액체와 혼합하기 때문에 이온성 액체에 분산이 이루어지지 않는 난용성 금속 전구체를 사용하더라도 금속 나노입자 제조가 가능하다.According to the present invention, it is possible to manufacture metal nanoparticles of uniform size by irradiating microwaves to a metal precursor uniformly dispersed in an ionic liquid to supply uniform energy, and after dissolving the metal precursor in a polar solvent, ions Since it is mixed with an ionic liquid, it is possible to manufacture metal nanoparticles even if a poorly soluble metal precursor that is not dispersed in the ionic liquid is used.
도 1은 본 발명의 실시 예에 따른 이온성 액체를 이용한 금속 나노 촉매 제조방법을 나타내는 공정도이다.
도 2는 본 발명의 실시 예 1의 TEM 이미지를 나타내는 도면이다.
도 3은 본 발명의 실시 예 2의 TEM 이미지를 나타내는 도면이다.
도 4는 본 발명의 실시 예 3의 TEM 이미지를 나타내는 도면이다.
도 5는 본 발명의 실시 예 1의 Diffraction pattern 이미지를 나타내는 도면이다.
도 6은 본 발명의 실시 예 2의 Diffraction pattern 이미지를 나타내는 도면이다.
도 7은 본 발명의 실시 예 3의 Diffraction pattern 이미지를 나타내는 도면이다.
도 8은 본 발명의 실시 예 1의 격자간격 이미지를 나타내는 도면이다.
도 9는 본 발명의 실시 예 2의 격자간격이미지를 나타내는 도면이다.
도 10은 본 발명의 실시 예 3의 격자간격 이미지를 나타내는 도면이다.1 is a process diagram showing a method for manufacturing a metal nano-catalyst using an ionic liquid according to an embodiment of the present invention.
2 is a view showing a TEM image of Example 1 of the present invention.
3 is a view showing a TEM image of Example 2 of the present invention.
4 is a view showing a TEM image of Example 3 of the present invention.
5 is a view showing a diffraction pattern image of Example 1 of the present invention.
6 is a view showing a diffraction pattern image of Example 2 of the present invention.
7 is a view showing a diffraction pattern image of Example 3 of the present invention.
8 is a diagram illustrating a grid-spaced image according to Example 1 of the present invention.
9 is a view showing a grid-spaced image in Example 2 of the present invention.
10 is a diagram illustrating a grid-spaced image according to Example 3 of the present invention.
이하, 첨부된 도면들을 참조하여 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자가 본 발명을 용이하게 실시할 수 있는 바람직한 실시 예를 상세히 설명한다. 다만, 본 발명의 바람직한 실시 예의 동작원리를 상세하게 설명함에 있어 관련된 공지 기능 또는 구성에 대한 구체적인 설명이 본 발명의 요지를 불필요하게 흐릴 수 있다고 판단되는 경우에는 그 상세한 설명을 생략한다.Hereinafter, with reference to the accompanying drawings, a preferred embodiment in which a person of ordinary skill in the art to which the present invention pertains can easily practice the present invention will be described in detail. However, in the detailed description of the operating principle of the preferred embodiment of the present invention, if it is determined that a detailed description of a related known function or configuration may unnecessarily obscure the gist of the present invention, the detailed description thereof will be omitted.
본 발명의 일 실시 예에 따른 이온성 액체를 이용한 금속 나노 촉매 제조방법은 도 1에 도시된 바와 같이 금속 전구체를 극성 용매에 용해시키는 단계(S100); 금속 전구체가 용해된 용해액을 이온성 액체에 혼합시키는 단계(S200); 및 이온성 액체 혼합물에 마이크로웨이브를 조사하여 금속 나노입자를 제조하는 단계(300)를 포함한다.A method for preparing a metal nano-catalyst using an ionic liquid according to an embodiment of the present invention includes dissolving a metal precursor in a polar solvent as shown in FIG. 1 (S100); mixing the dissolved solution in which the metal precursor is dissolved in the ionic liquid (S200); And irradiating a microwave to the ionic liquid mixture comprises a step 300 to prepare metal nanoparticles.
먼저, 금속 전구체를 극성 용매에 용해시킨다. 이렇게 금속 전구체를 극성 용매에 용해시키는 이유는 많은 종류의 금속 전구체가 이온성 액체에 직접 분산(또는 용해)되지 않기 때문에 금속 전구체를 이온성 액체에 균일하게 분산시키기 위한 전처리 공정을 수행하는 것이다. 이때, 금속 전구체가 극성 용매에 완전히 용해되고, 후속 공정에서 극성 용매의 제거가 용이하도록 금속 전구체와 극성 용매는 1:1 ~ 1:10의 농도 비율로 혼합되는 게 바람직하다.First, a metal precursor is dissolved in a polar solvent. The reason for dissolving the metal precursor in the polar solvent is to perform a pretreatment process for uniformly dispersing the metal precursor in the ionic liquid because many kinds of metal precursors are not directly dispersed (or dissolved) in the ionic liquid. At this time, it is preferable that the metal precursor and the polar solvent are mixed in a concentration ratio of 1:1 to 1:10 so that the metal precursor is completely dissolved in the polar solvent, and the polar solvent is easily removed in a subsequent process.
여기서, 금속 전구체로는 2족 금속, 3족 금속, 12족 금속, 13족 금속, 전이금속, 란타넘족 및 이들의 조합물로 이루어진 군으로부터 선택되고, 적어도 1개 이상의 금속 전구체가 극성 용매에 용해되며, 극성 용매로는 물, 아세톤, 에탄올 등이 사용된다.Here, the metal precursor is selected from the group consisting of a group 2 metal, a group 3 metal, a group 12 metal, a group 13 metal, a transition metal, a lanthanide group, and combinations thereof, and at least one metal precursor is dissolved in a polar solvent and water, acetone, ethanol, etc. are used as the polar solvent.
한편, 2종류의 서로 다른 금속 전구체가 극성 용매에 혼합될 때 제1 금속 전구체와 제2 금속 전구체는 1:99~99:1의 농도 비율을 갖도록 혼합되고, 금속 전구체를 극성 용매에 용해시키는 용해 공정에서는 금속 전구체가 극성 용매에 쉽게 용해될 수 있도록 극성 용매를 교반하는 교반 공정이 추가될 수 있다.On the other hand, when two different metal precursors are mixed in a polar solvent, the first metal precursor and the second metal precursor are mixed to have a concentration ratio of 1:99 to 99:1, and the metal precursor is dissolved in the polar solvent. In the process, a stirring process of stirring the polar solvent may be added so that the metal precursor can be easily dissolved in the polar solvent.
금속 전구체를 극성 용매에 용해시킨 후에는 금속 전구체가 용해된 극성 용매 용해액을 이온성 액체와 혼합시킨다.After the metal precursor is dissolved in the polar solvent, the polar solvent solution in which the metal precursor is dissolved is mixed with the ionic liquid.
이때, 이온성 액체 혼합되는 금속 전구체 농도가 너무 낮으면, 원하는 크기의 금속 나노입자 제조가 어렵고, 너무 높은 농도로 혼합되면, 균일한 금속 나노입자 제조가 어렵기 때문에 0.1mM/L ~ 50mM/L의 농도로 이온성 액체에 혼합되는 게 바람직하다.At this time, if the concentration of the metal precursor to be mixed with the ionic liquid is too low, it is difficult to manufacture metal nanoparticles of a desired size, and if the concentration is too high, it is difficult to produce uniform metal nanoparticles, so 0.1mM/L ~ 50mM/L It is preferable to be mixed with the ionic liquid at a concentration of
여기서, 이온성 액체는 양이온과 음이온만으로 구성되는 염(salt)임에도 불구하고 상온에서 액체 상태를 유지하는 화합물을 말하며, 고온 안정성이 높고, 액체 온도 범위가 넓으며, 점성이 높고, 증기압이 매우 낮으며, 높은 산화·환원 내성을 갖는 특성을 가지고 있다.Here, the ionic liquid refers to a compound that maintains a liquid state at room temperature despite being a salt composed of only cations and anions, high temperature stability, wide liquid temperature range, high viscosity, and very low vapor pressure and has high oxidation/reduction resistance.
이러한, 이온성 액체는 친수성이거나 소수성일 수 있으며, 특별히 제한되는 것은 아니나 지방족계, 피라졸륨계, 트리아졸륨계, 티아졸륨계, 옥사졸륨계, 피리디지늄계, 피리미디늄계, 암모늄계, 포스포늄계, 설포늄계, 피리디늄계, 피롤리디늄계, 및 이들의 조합물로 이루어진 군에서 선택될 수 있으나, 이에 한정되지는 않는다.These ionic liquids may be hydrophilic or hydrophobic, and although not particularly limited, aliphatic, pyrazolium, triazolium, thiazolium, oxazolium, pyridizinium, pyrimidinium, ammonium, phospho It may be selected from the group consisting of nium-based, sulfonium-based, pyridinium-based, pyrrolidinium-based, and combinations thereof, but is not limited thereto.
한편, 금속 전구체가 용해된 용해액을 이온성 액체와 혼합시킬 때 용해액에 용해된 금속 전구체들이 이온성 액체 내에 균일하게 분포되도록 이온성 액체를 교반하거나 초음파를 조사하는 공정이 추가될 수 있다.On the other hand, when mixing the solution in which the metal precursor is dissolved with the ionic liquid, a process of stirring the ionic liquid or irradiating ultrasonic waves may be added so that the metal precursors dissolved in the solution are uniformly distributed in the ionic liquid.
용해액을 이온성 액체와 혼합한 이후에는 혼합물에 마이크로웨이브를 조사한다. 이로 인해, 이온성 액체 내에 금속 나노입자가 생성된다. 이때, 금속 나노입자는 균일한 크기로 형성되는 데, 이러한 이유는 이온성 액체 내에 균일하게 분포되는 금속 전구체들에 균일한 열이 가해지기 때문에 인접한 금속 전구체들이 서로 결합하여 금속 나노입자로 생성될 때 그 크기가 균일해지게 된다.After mixing the solution with the ionic liquid, the mixture is irradiated with microwaves. Due to this, metal nanoparticles are generated in the ionic liquid. At this time, the metal nanoparticles are formed in a uniform size, because uniform heat is applied to the metal precursors uniformly distributed in the ionic liquid, so when adjacent metal precursors combine with each other to form metal nanoparticles Its size becomes uniform.
이렇게, 이온성 액체를 이용하여 금속 나노입자를 제조하게 되면, 금속 나노입자의 표면이 화학적으로 변성되지 않기 때문에 고활성도를 갖는 금속 나노입자(즉, 금속 나노촉매) 제조가 가능해진다.In this way, when metal nanoparticles are prepared using an ionic liquid, metal nanoparticles having high activity (ie, metal nanocatalysts) can be manufactured because the surface of the metal nanoparticles is not chemically modified.
한편, 이온성 액체 내에 금속 나노입자를 생성한 후에는 이온성 액체와 금속 나노입자를 분리시킨 후 분리된 금속 나노입자를 세정하여 금속 나노입자에 잔류하는 이온성 액체를 제거한다.On the other hand, after generating the metal nanoparticles in the ionic liquid, the ionic liquid and the metal nanoparticles are separated, and then the separated metal nanoparticles are washed to remove the ionic liquid remaining in the metal nanoparticles.
이와 같은 본 발명의 금속 나노 촉매 제조방법은 금속 전구체 용해액과 이온성 액체를 혼합할 때 금속 전구체 용해액과 함께 담체 소재를 이온성 액체에 혼합하는 단계를 더 포함할 수 있다.The method for preparing a metal nanocatalyst of the present invention may further include mixing a carrier material together with the metal precursor solution into the ionic liquid when mixing the metal precursor solution and the ionic liquid.
이때, 담체 소재로는 그래핀, 그라파이트, 카본 블랙, 카본 나노튜브, 전도성 산화물 등이 사용된다.In this case, as the carrier material, graphene, graphite, carbon black, carbon nanotubes, conductive oxides, and the like are used.
이러한, 담체 소재는 금속 전구체에 비해 1 ~ 10배 정도의 농도로 이온성 액체에 혼합(즉, 이온성 액체에 1mM/L ~ 100mM/L의 농도로 혼합)되는데, 이러한 이유는 담체 소재 농도가 너무 낮을 경우 금속 전구체가 담체 소재에 담지가 되기 어렵고, 담체 소재의 농도가 너무 높을 경우 금속 나노입자가 담지된 담지체가 촉매로서의 기능이 저하되기 때문이다.Such a carrier material is mixed with the ionic liquid at a concentration of 1 to 10 times that of the metal precursor (that is, mixed with the ionic liquid at a concentration of 1 mM/L to 100 mM/L), for this reason, the carrier material concentration is If it is too low, it is difficult for the metal precursor to be supported on the carrier material, and if the concentration of the carrier material is too high, the function of the carrier on which the metal nanoparticles are supported as a catalyst is reduced.
이렇게 금속 전구체 용해액과 담체 소재를 이온성 액체와 혼합한 후 혼합물에 마이크로웨이브를 조사하면, 이온성 액체에 분산된 금속 전구체에 균일한 마이크로웨이브 에너지가 전달되기 때문에 이온성 액체 내에 균일한 크기의 금속 나노입자가 생성되어 담체에 부착된다.In this way, when the metal precursor solution and the carrier material are mixed with the ionic liquid and then microwave is irradiated to the mixture, the uniform microwave energy is transmitted to the metal precursor dispersed in the ionic liquid. Metal nanoparticles are generated and attached to the carrier.
[실시 예 1][Example 1]
H2O(1mL)에 AgNO3 0.035g을 넣어 1분 동안 300rpm으로 교반하여 금속 전구체 용액을 제조한다. 금속 전구체 용해액을 제조한 후에는 금속 전구체 용해액을 9ml의 BMIM BF4에 넣은 후 금속 전구체가 이온성 액체 내에 균일하게 분산되도록 3시간 동안 300rpm으로 교반한다.Add 0.035 g of AgNO 3 to H 2 O (1 mL) and stir at 300 rpm for 1 minute to prepare a metal precursor solution. After preparing the metal precursor solution, the metal precursor solution is put in 9 ml of BMIM BF 4 and stirred at 300 rpm for 3 hours so that the metal precursor is uniformly dispersed in the ionic liquid.
이때, 금속 전구체 용해액 제조 및 금속 전구체 용해액과 이온성 액체 혼합 공정은 모두 상온/상압에서 진행된다.In this case, the metal precursor solution preparation and the metal precursor solution and the ionic liquid mixing process are all carried out at room temperature/atmospheric pressure.
이렇게, AgNO3가 BMIM BF4에 50mM 농도로 혼합된 혼합물이 제조되면, 혼합물에 마이크로웨이브를 조사한다. 이때, 마이크로웨이브의 파워는 15W, 설정온도는 250℃, 유지시간은 600초로 진행하였다.In this way, AgNO 3 When a mixture in which BMIM BF 4 is mixed at a concentration of 50 mM is prepared, the mixture is irradiated with microwaves. At this time, the power of the microwave was 15W, the set temperature was 250°C, and the holding time was 600 seconds.
마이크로웨이브를 조사하여 설정온도에 도달된 후에는 자연 냉각으로 혼합물을 냉각시켰다.After reaching the set temperature by irradiating microwaves, the mixture was cooled by natural cooling.
[실시 예 2][Example 2]
실시 예 2는 마이크로웨이브의 파워를 20W로 설정한 것을 제외한 나머지 모든 공정은 실시 예1과 동일하게 진행하였다.In Example 2, all processes except for setting the microwave power to 20W were the same as in Example 1.
[실시 예3][Example 3]
실시 예 3은 마이크로웨이브의 파워를 30W로 설정하고, 유지시간을 400초로 설정한 것을 제외한 나머지 모든 공정은 실시 예 1과 동일하게 진행하였다.In Example 3, the microwave power was set to 30W, and all other processes were performed in the same manner as in Example 1, except that the holding time was set to 400 seconds.
실시 예 1 내지 실시 예 3에 따라 생성된 이온성 액체 내의 금속 나노입자는 투사 전자현미경(Transmission Electron Microscope; TEM)으로 촬영하였다. 도 2 내지 도 4를 통해 알 수 있듯이, 본 발명의 금속 나노 촉매 제조방법에 의해 제조된 금속 나노입자들은 균일한 크기를 갖도록 형성됨을 알 수 있고, 마이크로웨이브의 파워가 15W, 20W, 30W로 순차적으로 증가할 때 평균 입자 크기는 10㎚, 6.89㎚, 5.44㎚로 감소함을 알 수 있다. 따라서, 금속 나노입자의 사용용도에 따라 마이크로웨이브의 파워를 조절하여 금속 나노입자의 크기를 조절할 수 있음을 알 수 있다.Metal nanoparticles in the ionic liquid produced according to Examples 1 to 3 were photographed with a transmission electron microscope (TEM). As can be seen through FIGS. 2 to 4, it can be seen that the metal nanoparticles prepared by the method for preparing a metal nanocatalyst of the present invention are formed to have a uniform size, and the power of the microwave is 15W, 20W, 30W sequentially. It can be seen that the average particle size decreases to 10 nm, 6.89 nm, and 5.44 nm as it increases. Therefore, it can be seen that the size of the metal nanoparticles can be adjusted by adjusting the power of the microwave according to the purpose of use of the metal nanoparticles.
또한, 도 5 내지 도 10에 도시된 바와 같이, 모두 실버(Ag) 특성을 나타내는 (111), (002), 222) 회절패턴(Diffraction pattern)을 나타내고, 모두 실버(Ag)의 격자간격인 2.35Å을 나타내어 생성된 나노입자가 모두 실버(Ag) 입자로 확인되었다.In addition, as shown in FIGS. 5 to 10 , all of (111), (002), and 222) showing silver (Ag) characteristics show diffraction patterns, all of which are silver (Ag) lattice spacing of 2.35. It was confirmed that all nanoparticles produced by indicating Å were silver (Ag) particles.
이상에서 설명한 바와 같이, 본 발명의 상세한 설명에서는 본 발명의 바람직한 실시 예에 관해서 설명하였으나, 이는 본 발명의 가장 양호한 실시 예를 예시적으로 설명한 것일 뿐, 본 발명을 한정하는 것은 아니다. 또한, 본 발명이 속하는 기술 분야의 통상의 지식을 가진 자라면 누구나 본 발명의 기술사상의 범주를 벗어나지 않는 범위 내에서 다양한 변형과 모방이 가능함을 물론이다. 따라서, 본 발명의 권리범위는 설명된 실시 예에 국한되어 정해져선 안 되며, 후술하는 청구범위뿐만 아니라 이와 균등한 것들에 의해 정해져야 한다.As described above, in the detailed description of the present invention, a preferred embodiment of the present invention has been described, but this is only illustrative of the preferred embodiment of the present invention, and does not limit the present invention. In addition, of course, various modifications and imitations are possible without departing from the scope of the technical idea of the present invention by anyone having ordinary knowledge in the technical field to which the present invention belongs. Accordingly, the scope of the present invention should not be limited to the described embodiments, but should be defined by the following claims as well as equivalents thereof.
Claims (10)
상기 금속 전구체가 용해된 용해액과 이온성 액체가 혼합된 혼합물을 제조하는 단계; 및
상기 혼합물에 마이크로웨이브를 조사하는 단계를 포함하는 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.dissolving the metal precursor in a polar solvent;
preparing a mixture in which a solution in which the metal precursor is dissolved and an ionic liquid are mixed; and
Method for producing a metal nano-catalyst using an ionic liquid, characterized in that it comprises the step of irradiating the mixture with microwaves.
상기 금속 전구체와 극성 용매는 1:1 ~ 1:10의 농도 비율로 혼합되는 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.The method according to claim 1,
The metal precursor and the polar solvent are a method for producing a metal nano-catalyst using an ionic liquid, characterized in that mixed in a concentration ratio of 1:1 to 1:10.
상기 금속 전구체는 상기 이온성 액체에 0.1mM/L ~ 50mM/L 농도로 혼합되는 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.The method according to claim 1,
The metal precursor is a metal nano-catalyst manufacturing method using an ionic liquid, characterized in that mixed in the ionic liquid at a concentration of 0.1mM / L ~ 50mM / L.
상기 금속 전구체의 금속은 2족 금속, 3족 금속, 12족 금속, 13족 금속, 전이 금속, 란타넘족 및 이들의 조합물로 이루어진 군으로부터 선택되는 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.The method according to claim 1,
The metal of the metal precursor is a metal nanocatalyst using an ionic liquid, characterized in that selected from the group consisting of a Group 2 metal, a Group 3 metal, a Group 12 metal, a Group 13 metal, a transition metal, a lanthanide group, and combinations thereof manufacturing method.
상기 극성 용매에는 2개의 서로 다른 금속 전구체가 용해되는 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.The method according to claim 1,
A method for preparing a metal nano-catalyst using an ionic liquid, characterized in that two different metal precursors are dissolved in the polar solvent.
상기 이온성 액체는 지방족계, 피라졸륨계, 트리아졸륨계, 티아졸륨계, 옥사졸륨계, 피리디지늄계, 피리미디늄계, 암모늄계, 포스포늄계, 설포늄계, 피리디늄계, 피롤리디늄계, 및 이들의 조합물로 이루어진 군에서 선택되는 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.The method according to claim 1,
The ionic liquid is aliphatic, pyrazolium, triazolium, thiazolium, oxazolium, pyridizinium, pyrimidinium, ammonium, phosphonium, sulfonium, pyridinium, pyrrolidinium , and a method for preparing a metal nano-catalyst using an ionic liquid, characterized in that selected from the group consisting of combinations thereof.
상기 혼합물을 제조하는 단계는,
상기 금속 전구체가 용해된 용해액과 함께 담체 소재가 이온성 액체에 혼합되는 단계를 더 포함하는 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.The method according to claim 1,
The step of preparing the mixture,
Method for producing a metal nano-catalyst using an ionic liquid, characterized in that it further comprises the step of mixing the carrier material with the solution in which the metal precursor is dissolved in the ionic liquid.
상기 담체 소재는 그래핀, 그라파이트, 카본 블랙, 카본 나노튜브, 전도성 산화물 중 어느 하나인 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.8. The method of claim 7,
The method for preparing a metal nano catalyst using an ionic liquid, characterized in that the carrier material is any one of graphene, graphite, carbon black, carbon nanotubes, and conductive oxides.
상기 담체 소재는 상기 금속 전구체에 비해 1 ~ 10배 정도의 농도로 이온성 액체에 혼합되는 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.8. The method of claim 7,
The carrier material is a metal nano-catalyst manufacturing method using an ionic liquid, characterized in that it is mixed with the ionic liquid at a concentration of about 1 to 10 times that of the metal precursor.
상기 혼합물을 제조하는 단계는,
상기 혼합물에 초음파를 조사하는 단계를 더 포함하는 것을 특징으로 하는 이온성 액체를 이용한 금속 나노 촉매 제조방법.The method according to claim 1,
The step of preparing the mixture,
Method for producing a metal nano-catalyst using an ionic liquid, characterized in that it further comprises the step of irradiating ultrasonic waves to the mixture.
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