A novel strategy for the simultaneous reduction and functionalization of graphene oxide (G-O) was developed using polyallylamine hydrochloride (PAAH) as a multi-functional agent. The G-O functionalization by PAAH was carried out under basic conditions to catalyze the epoxide ring opening reaction of G-O with abundant amine groups of PAAH. We found that G-O was not only functionalized with PAAH but also reduced under the reaction condition. Moreover, the synthesized PAAH-functionalized G-O sheets were soluble in water and applicable to the synthesis of nanocomposites with gold nanoparticles.

The present study focused on the synthesis of Bi-Te-Se-based powder by an oxide-reduction process, and analysis of the thermoelectric properties of the synthesized powder. The phase structure, chemical composition, and morphology of the synthesized powder were analyzed by XRD, EPMA and SEM. The synthesized powder was sintered by spark plasma sintering. The thermoelectric properties of the sintered body were evaluated by measuring its Seebeck coefficient, electrical resistivity, and thermal conductivity. powder was synthesized from a mixture of , , and powders by mechanical milling, calcination, and reduction. The sintered body of the synthesized powder exhibited n-type thermoelectric characteristics. The thermoelectric properties of the sintered bodies depend on the reduction temperature. The Seebeck coefficient and electrical resistivity of the sintered body were increased with increasing reduction temperature. The sintered body of the powder synthesized at showed about 0.5 of the figure of merit (ZT) at room temperature.

The present study focused on the synthesis of Bi-Sb-Te-based thermoelectric powder by an oxidereduction process. The phase structure, particle size of the synthesized powders were analyzed using XRD and SEM. The synthesized powder was sintered by the spark plasma sintering method. The thermoelectric property of the sintered body was evaluated by measuring the Seebeck coefficient and specific electric resistivity. The powder had been synthesized by a combination of mechanical milling, calcination and reduction processes using mixture of , and powders. The sintered body of the powder synthesized by an oxide-reduction process showed p-type thermoelectric characteristics, even though it had lower thermoelectric properties than the sintered body of the thermoelectric powder synthesized by the conventional melting-crushing method.

상용원자로에서 발생하는 산화물 사용후핵연료의 부피감용과 재활용을 위하여 산화물을 금속으로 환원시 키는 공정에 대한 연구가 수행되어 왔다. 다양한 환원법 중에서, 한국원자력연구원은 LiCl-Li2O 용융염을 반 응매질로 사용하는 전해환원공정을 현재 개발 중이다. 파이로 공정의 전단부에 해당하는 전해환원 공정은 PWR 산화물 연료 주기를 소듐냉각 고속로의 금속연료 주기에 연결시켜 준다. 이 논문은 금속전환 공정을 개 발/개선하고, 용량 증대를 수행한 한국원자력연구원의 노력을 요약한다.

경막결정화를 이용한 산화물 사용후연료의 전해환원 공정에서 발생하는 LiCl 염폐기물 내 포함되어 있는 Cs 및 Sr을 분리(농축)에 대한 실험을 수행하였다. 결정화 공정에서 Cs 및 Sr과 같은 불순물들은 불순물들의 용융염 상 및 결정상에 대한 용해도이 차리로 분리되어 최종적으로 작은 양의 LiCl 용융염내에 농축된다. 본 연구에서는 LiCl-CsCl-SrCl2 계에대한 고체-액체 상평형도를 통해 결정화를 통한 분리가능성을 파악하였으며 열전달방정식 의 계산을 통해 경막결정화 운전중 LiCl 용융염상의 온도분포를 예측할 수 있었다. 경막결정화 공정에서 결정성 장 속도는 분리효율에 큰 영향을 미쳤으며 90%의 LiCl 재생율을 가정할 경우 20-25 l/min의 냉각속도 그리고 0.2 g/min·cm2보다 작은 결정성장 속도조건에서 각각의 Cs 및 Sr에 대하여 90% 정도의 분리효율을 나타내었다.

고온 용융염 전해환원 공정은 후행핵연료 주기의 대안 공정인 파이로공정의 산화물 사용후핵연료의 확대 를 위해 필수적인 공정이다. 사용후핵연료는 다성분 산화물로 이루어져 있으며 각 산화물은 전해환원 공정 에서 화학적 특성에 따라 산소를 잃게 된다. 본 연구에서는 건식분말화 공정 이후 전해환원 반응기에 도입되 는 사용후핵연료 조성을 기준으로 각 금속-산소 시스템을 독립적인 이상고용체로 가정하여 전해환원 반응거동을 계산하였다. 전해환원을 Li의 환원과 이어지는 Li과의 화학반응의 결합으로 산정하여 U을 비롯한 금 속 환원 거동을 계산하였다. 계산결과 대부분의 산화물들은 전해환원 공정에 의해 금속으로 전환되는 것으 로 예상되었다. 란타나이드 원소들의 경우 Li2O의 농도가 낮아지면 금속 전환율이 높아지나 대부분 산화물로 존재하는 것으로 나타났다. 추가적으로 U3O8의 전해환원 거동에 대해 Li의 확산과 Li과의 화학반응을 고려하 여 반실험적 모델이 제시되었다. 실험데이터를 활용하여 매개변수를 결정하였으며 시간에 대한 환원율 및 전류에 대한 99.9% 환원 시간을 계산하였다.

To produce alloy powders with only SmFe single phase by reduction-diffusion (R-D) method, the effect of excess samarium oxide on the preparation of Sm-Fe alloy powder during R-D heat treatment was studied. The quantity of samarium oxide was varied from 5% to 50% whereas iron and calcium were taken 0% and 200% in excess of chemical equivalent, respectively. The pellet type mixture of samarium, iron powders and calcium granulars was subjected to heat treatment at 1100 for 5 hours. The R-D treated pellet was moved into deionized water and agitated to separate Sm-Fe alloy powders. After washing them in deionized water several times, the powders were washed with acetic acid to remove the undesired reaction products such as CaO. By these washing and acid cleaning treatment, only 0.03 wt% calcium remained in Sm-Fe alloy powders. It was also confirmed that the content of unreacted -Fe in SmFe matrix gradually decreased as the percentage of samarium oxide is increased. However, there was no significant change above 40% excess samarium oxide.

Aluminum nitride (AlN) nanopowders with low degree of agglomeration and uniform particle size were synthesized by carbothermal reduction of alumina and subsequent direct nitridization. Boehmite powder was homogeneously admixed with carbon black nanopowders by ball milling. The powder mixture was treated under ammonia atmosphere to synthesize AlN powder at lour temperature. The effect of process variables such as boehmite/carbon black powder ratio, reaction temperature and reaction time on the synthesis of AlN nanopowder was investigated.

Ultrasonic-milling of metal oxide nanopowders for the preparation of tungsten heavy alloys was investigated. Milling time was selected as a process variable. XRD results of metal oxide nanopowders ultrasonic-milled for 50 and 100h showed that mean crystallite size reduced with increasing milling time and there was no evidence of contamination or change of composition by impurities. It was found that nanocomposite powders reduced at in atmosphere had a composition of 93.1W-4.9Ni-2.0Fe by EDX analysis. Hardness of sintered samples of 50 and 100h was 390 and 463 Hv, respectively, which corresponds to the hardness of commercial products.

In the present study, the focus is on the effect of cobalt oxide powder in the carbothermal reduction of the titanium-cobalt-oxygen based oxide powder by solid carbon for the optimizing synthesis process of ultra fine TiC/Co composite powder. The titanium-cobalt-oxygen based oxide powder was prepared by the combination of the spray drying and desalting processes using the titanium dioxide powder and cobalt nitrate as the raw materials. The titanium-cobalt-oxygen based oxide powder was mixed with carbon black, and then this mixture was carbothermally reduced under flowing argon atmosphere. Changes in the phase structure and thermal gravity of the mixture during carbothermal reduction were analysed using XRD and TGA. Titanium-cobalt-oxygen based oxide powder desalted at had a mixture of . And the one desalted at had a mixture of . In the case of the former powder, the reduction of cobalt oxide powder in the titanium-cobalt-oxygen based oxide powder occurred at lower temperature than the latter one. However, the carbothermal reduction of titanium dioxide powder in the titanium-cobalt-oxygen based oxide powder with a mixture of occurred at higher temperature than the one with a mixture of . And also, the former powder showed a lower TiC formation ability than the latter one.

650의 LiCl-LiO 용융염계에서 10 g UO/batch 규모의 장치를 이용해서 우라늄산화물의 전해환원 특성에 대한 평가를 수행하였다. 일체형 음극은 고체전극, 우라늄산화물과 우라늄산화물을 담아주는 다공성 용기(멤브레인)로 구성된다. 멤브레인 재료로는 325-mesh 스테인레스강막과 다공성 마그네시아 도가니를 사용하였다. 일체형 음극의 재질에 따른 LiCl-3 wt LiO계와 UO-LiCl-3 wt LiO계의 순환 전압측정법 결과로부터 전해환원 반웅 메커니즘을 규명하였다. 일체형 음극의 재질에 따른 우라늄산화물의 직접 및 간접 전해환원에 대한 실험을 수행하였다. 그 결과, 325-mesh스테인레스강막을 사용하여 직접 및 간접 전해환원으로 금속전환을 수행하였을 때 낮은 전류효율로 인해 우라늄산화물을 금속우라늄으로 환원시키지 못했으며, 마그네시아 다공성 도가니를 사용하여 간접 전해환원으로 금속전환을 수행하였을 때는 높은 전류효율로 인해 우라늄산화물을 금속우라늄으로 환원시킬 수 있었다

In the present study, the focus is on the analysis of carbothermal reduction of oxide powder prepared from waste WC/Co hardmetal by solid carbon under a stream of argon for the recycling of the WC/Co hard-metal. The oxide powder was prepared by the combination of the oxidation and crushing processes using the waste hardmetal as the raw material. This oxide powder was mixed with carbon black, and then this mixture was carbothermally reduced under a flowing argon atmosphere. The changes in the phase structure and gases discharge of the mixture during carbothermal reduction was analysed using XRD and gas analyzer. The oxide powder prepared from waste hardmetal has a mixture of . This oxide powder reduced at about , formed tungsten carbides at about , and then fully transformed to a mixed state of tungsten carbide (WC) and cobalt at about by solid carbon under a stream of argon. The WC/Co composite powder synthesized at for 6 hours from oxide powder of waste hardmetal has an average particle size of .

We report a carbothermal reduction process for massive synthesis of monolithic WO phase from tungsten oxide in the presence of carbon source. Carbon black powder was used as a carbon source and added to WO by 40 weight percent. Bundles of WO rods were formed over the temperature range of 80 to 90. Pure WO bundles could be separated from the mixture of WO and residual carbon black powder. Field emission character of WO phase was determined using the extracted WO rods. Flat lamp fabricated from the WO rods showed the turn-on field of 9.3 V/

In the present study, the focus is on the analysis of carbothermal reduction of the titanium-cobalt-oxygen based oxide powder by solid carbon for the optimizing synthesis process of ultra fined TiC/Co composite powder. The titanium-cobalt-oxygen based oxide powder was prepared by the combination of the spray drying and desalting processes using the titanium dioxide powder and cobalt nitrate as the raw materials. The titanium-cobalt-oxygen based oxide powder was mixed with carbon black, and then this mixture was carbothermally reduced under a flowing argon atmosphere. The changes in the phase structure and thermal gravity of the mixture during carbothermal reduction were analysed using XRD and TGA. The synthesized titanium-cobalt-oxygen based oxide powder has a mixture of and . This oxide powder was transformed to a mixed state of titanium car-bide and cobalt by solid carbon through four steps of carbothermal reduction steps with increasing temperature; reduction of to and Co, reduction of , to the magneli phase(, n>3), reduction of the mag-neli phase(, n>3) to the (2n3) phases, and reduction and carburization of the (2n3) phases to titanium carbide.

The reduction mechanism of the composite powders mixed with and CuO has been studied by using thermogravimetry (TG), X-ray diffraction, and microstructure analyses. The composite powders were made by simple Turbula mixing, spray drying, and ball-milling in a stainless steel jar with the ball to powder ratio of 32 to 1 at 80 rpm for 1 h without process controlling agents. It is observed that all the oxide composite powders are converted to W-coated Cu composite powder after reducing treatment under hydrogen atmosphere. For the formation mechanism of W-coated Cu composite powder, the sequential reduction steps are proposed as follows: CuO contained in the ball-milled composite powder is initially reduced to Cu at the temperature range from 20 to 30. Then, powder is reduced to W via W and W at higher temperature region. Finally, the gaseous phase of formed by reaction of with water vapour migrates to previously reduced Cu and deposits on it as W reduced by hydrogen. The proposed mechanism has been proved through the model experiment which was performed by using Cu plate and powder.der.

본 연구에서는 고온의 LiCl-LlO 용융염계에서 우라늄 산화물의 금속전환과 LiO의 전해반응이 동시에 진행되는 통합 반응 메카니즘을 기초로 한 전기화학적 금속전환기술을 제안하였다. 본 실험에서는 전기화학적 환원반응에 의해 생성된 Li 금속이온이 음극에 전착과 동시에 우라늄 산화물과 반응하여 금속전환율 99 % 이상의 우라늄 감속을 생성하는 통합 반응 메카니즘을 확인할 수 있었다. 또한 전기화학적 금속전환기술의 공정 적용성 평가 일환으로 우라늄 산화물의 금속전환성, 반응 메카니즘 규명, LiO의 closed recycle rate 및 물질전달 특성 등의 기초 데이터를 확보하였다 향후 전기화학적 금속전환기술은 LiCl-Li 용융염계의 금속전환공정의 반응조건 제한성 해소, 금속전환율 향상 및 공정의 단순화 등의 기술성과 경제성 향상 측면에서 획기적인 방안으로 고려될 수 있을 것으로 판단된다.