• Resources Recycling
• /
• v.31 no.2
• /
• pp.63-69
• /
• 2022

In this study, mechanical grinding using a planetary ball mill was performed under various conditions to evaluate its effect on the crystal structure of vanadium titanium magnetite (VTM) ore from the Kwain Mine in South Korea. The crystal structure of the activated product was also evaluated. Magnetite and ilmenite were identified as the main types of VTM ore used in the Kwain Mine, and the main types of gangue minerals were iron-based silicate minerals. According to the mechanical activation results, the crystallinity and crystal size decreased as the size of the grinding media (balls) decreased, and the amorphization of the sample/ball filling was significant as the amount of the sample was reduced. In addition, as the grinding speed and time increased, the crystal structure significantly changed, proving that these two parameters had a greater effect on the crystal structure than the ball size and sample/ball filling ratio.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 1997.10a
• /
• pp.81-85
• /
• 1997

철질화물 및 Mo-Si계 규화물을 합성하기 위하여 실온 메카노케미칼 공정을 적용하였다. 메카노케미칼 처리는 고에너지 유성형 볼밀장치를 사용하였고 용기는 진공배기 후 암모니아 혹은 아르곤 가스로 충전시킨 후 벌밀처리를 행하였다. 분말의 특성평가는 XRD, DTA/DSC, SEM 및 EPMA 등에 의하여 행하였다. 철질화물의 경우 실온에서 최대 23.3 at.%N의 $\varepsilon$상 질화물을 얻을 수 있었다. 또한 Mo-SirP의 경우 100시간 메카노케미칼 처리시킴으로서 MiSi$_2$규화물을 합성할 수 있었으며 얻어진 분말의 결정립은 25cm로 매우 미세한 결정립의 분말재료임이 확인되었다.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.21 no.6
• /
• pp.246-252
• /
• 2011

The semiconducting $MnSi_{1.73}$ compound has been recognized as a thermoelectric material with excellent oxidation resistance and stable characteristics at elevated temperature. In the present work, we applied mechanical alloying (MA) technique to produce $MnSi_{1.73}$ compound using a mixture of elemental manganese and silicon powders. The mechanical alloying was carried out using a Fritsch P-5 planetary mill under Ar gas atmosphere. The MA powders were characterized by the X-ray diffraction with Cu-$K{\alpha}$ radiation, thermal analysis and scanning electron microscopy. Due to the observed larger loss of Si relative to Mn during mechanical alloying of $MnSi_{1.73}$, the starting composition of a mixture Mn-Si was modified to $MnSi_{1.83}$ and then $MnSi_{1.88}$. The single $MnSi_{1.73}$ phase has been obtained by mechanical alloying of $MnSi_{1.88}$ mixture powders for 200 hours. It is also found that the grain size of $MnSi_{1.73}$ compound powders analyzed by Hall plot method is reduced to 40 nm after 200 hours of milling.

• Proceedings of the Korean Powder Metallurgy Institute Conference
• /
• 2002.11a
• /
• pp.63-63
• /
• 2002

현재 기계적 합금화법에서는 주로 합금을 구성하는 성분원소 분말을 불활성분위기에서 볼밀처리 함으로써 함금화를 시키거나 모합금에 산화물을 분산시켜 복합화시키는 공정을 통하여 각종 화합물, 비정질상 및 과포화고용체등의 준안정상의 합성 뿐만이 아니라 초미세조직의 생성에 관한 폭 넓은 분야의 연구가 행하여지고 있다. 한편 MA에서는 볼멀처리중 기계적 에너지의 투여에 의하여 실제 반응온도보다 낮은 온도에서 발생하는 특이한 화학반응 즉 Mechanochemical 반응을 일으키 기도 한다. 본 연구에서는 헤마타이트($Fe_20_3$)와 금속윈소인 Ti의 MA처리에 의하여 고상환원반응 을 유기시켜 $Fe-TiO_2$계 nanocomposite 분말재료를 제조하고자 한다. 특히 MA 공정에 있어서 자기 물성의 변화와 X선 회절을 통하여 고상환원반응에 의한 복합분말의 생성과정을 조사하였다. 출발원료는 $Fe_20_3$(고순도화학제,99.9%, 평균입경 0.1$\mu\textrm{m}$)와 금속원소인 Ti(99.9%, 명균업경 150$\mu\textrm{m}$)을 몰비 2:3의 조성이 되도록 하여 MA를 실시하였다. 볼멀은 고에너지 유성형 볼밀장치(독일 제, Fritsch P-5)를 이용하였으며 진공치환형 용기에 원료분말을 장입하여 2회정도 진공배기한 후 아르곤 가스를 충전하여 볼밀을 행하였다. 얻어진 분말시료에 대하여 x-선 회절장치, 전자현미경 (SEM) 및 진동시료형자력계(VSM)를 통하여 결정구조, 미셰조직 빛 자기특성을 조사하였다. $Fe_2O_3-Ti$ 혼합분말의 MA처리 에 의하여 초기단계부터 환원반응과 함께 $Fe_3TIO_{lO}$ 중간상이 관찰 되었으나 30hrs의 MA처리 후 Fe와 산화물 $TiO_2$로 모두 환원되어 $Fe-TiO_2$계 나노복합분말이 얻어짐을 알 수 있었다. 이 때 X션 회절피크의 line broadening으로부터 복합분말의 Fe 명균 결정립 크기는 24nm로 초미세 결정럽의 분말합금이었다. 포화자화값은 볼밀처리에 따라 점점 증가하여 MA 30시간에는 20.3emu/g로 포화됨을 알 수 있었다. 또한 보자력 Hc는 MA초기단계에 350e로 매우 낮으나 30시간 후에는 Hc값이 2600e로 매우 큰 값을 나타내었다. 이것은 환원반응결과 초기에 생성된 Fe의 결정립이 비교적 크고 결정결함이 적으나 볼밀처리를 30시간까지 행하면 Fe 결정렵의 미세화 빛 strain 증가로 magnetic hardening이 일어나기 때문인 것으로 사료된다.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.10 no.4
• /
• pp.292-296
• /
• 2000

Mechenochemical reaction by planetary type ball mill is applied to prepare $Sm_2$$Fe_{17}$$N_{x}$ permanent magnet powders. Starting from pure samarium and iron powders, the formation process of hard magnetic $Sm_2$$Fe_{17}$$N_{x}$ phase by ball milling and a subsequent solid state reaction were studied. At as-milled stage powders were found to consist of amorphous Sm-Fe and $\alpha$-Fe phases in all composition of $Sm_2$$Fe_{100-x}$(x = 11, 13, 15). The dependence of starting composition of elemental powder on the formation of Sm-Fe intermetallic compound was investigated by heat treatment of as-milled powders. When Sm concentration was 15 at%, heat-treated powder consists of mostly $Sm_2$$Fe_{17}$$N_{x}$single phase. For synthesizing of hard magnetic $Sm_2$$Fe_{17}$$N_{x}$ compound, additional nitriding treatment was carried out under $N_2$gas atmosphere at $450^{\circ}C$. The increase in the coercivity and remanence was parallel to the nitrogen content which increased drastically at first and then gradually as the nitriding time was extended. The ball-milled Sm-Fe-N powders were expected to be prospective materials for synthesizing of permanent magnet with high performance.

• 한국신재생에너지학회:학술대회논문집
• /
• 2007.11a
• /
• pp.101-104
• /
• 2007

700 $^{\circ}C$이상의 온도에서 실시되는 고온수전해는 다가오는 수소경제시대의 주요한 수소제조기 술로 주목되고 있다. 이 연구에서는 Ni보다 전기전도도가 우수하고 가격이 저렴한 Cu를 사용하여 고온수 전해 수소극용 Cu/YSZ 복합체를 기계적합금법에 의해 제조하여 미세구조를 관찰하였고 Cu/YSZ를 수소전극으로 한 반전지를 제조하여 수조제조 실험을 실시하였다. Cu/YSZ 복합체는 Cu와 YSZ를 6:4(vol%)의 조성비로 유성밀을 사용하여 400 rpm으로 24시간 동안 실시하여 제조하였다. 고에너지 볼밀 후 500 nm이하의 나노크기의 복합체가 제조되었으며 Cu입자에 YSZ가 고르게 분포되어 있었다. 수은압입법으로 측정한 기공률은 70%이고 기공크기는 평균 0.5 ${\mu}m$으로 미세한 기공으로 이루어져 있었다. 제조된 Cu/YSZ 복합체를 수소전극으로 한 반전지를 제조하여 수소제조 실험을 실시한 결과 Ni/YSZ 전극보다 수소제조 성능이 우수한 것으로 나타났다. Cu의 높은 열팽창계수와 낮은 녹는점을 보완하면 우수한 고온수전해용 전극재료로 사용될 것으로 판단된다.

• Resources Recycling
• /
• v.23 no.6
• /
• pp.3-11
• /
• 2014

Bottom ash from coal fired power plants is not widely used due to a broad range of particle sizes and a high carbon content for producing geopolymers. The effect of mechanical activation on compressive strength of bottom ash- based geopolymers was examined by rod and planetary-ball milling to encourage full-fledged recycling of bottom ash, the main component of pond ash. The amount of amorphous component in the milled ash samples did not change significantly after the mechanical activation. It is presumably because needle-shaped mullite crystals, which is a major crystalline phase and grown in a glassy matrix, possess high strength and toughness, and therefore, they could endure external shocks and remain almost intact. Milling operation, however, decreased the particle size and improved the homogeneity of ash, thereby leading to increase reactivity of milled ash with alkali activators. Rod milling produced a relatively narrow particle size distribution of the milled ash particles; however, it was less effective in reducing the particle size. Nevertheless, it was interesting to observe that rod milling had equal effect on improving the compressive strength of geopolymers up to about 37%, as that of planetary ball milling. Rod milling is believed to be suitable process for enhancing the reactivity of bottom ash for large-scale recycling of bottom ash and producing geopolymers.

• Applied Chemistry for Engineering
• /
• v.8 no.5
• /
• pp.811-815
• /
• 1997

The present work describes the effect of dry grinding of a mixture composed of $Y_2O_3$, $BaCO_3$ and CuO powders with a planetary ball mill before heat treatment on crystal structure and superconductivity in the $YBa_2Cu_3O_{7-y}$. The specific surface area of the ground product of mixture decreased with an increase in the grinding time, after showing an upward trend up to 60 minutes of grinding. The critical current density, which was influenced by the grinding time of mixture, indicates the maximum value of about $150A/cm^2$ in the case of 60 minutes grinding, while the critical temperature, which were around 90K, for the sintered bodies were almost independent of the grinding time.

• Journal of Powder Materials
• /
• v.22 no.3
• /
• pp.208-215
• /
• 2015

Fe-TiC composite powders were fabricated by planetary ball mill processing. Two kinds of powder mixtures were prepared from the starting materials of (a) (Fe, TiC) powders and (b) (Fe, $TiH_2$, Carbon) powders, respectively. Milling speed (300, 500 and 700 rpm) and time (1, 2, and 3 h) were varied. For (Fe, $TiH_2$, Carbon) powders, an in situ reaction synthesis of TiC after the planetary ball mill processing was added to obtain a homogeneous distribution of ultrafine TiC particulates in Fe matrix. Powder characteristics such as particle size, size distribution, shape, and mixing homogeneity were investigated.

• Journal of Powder Materials
• /
• v.17 no.4
• /
• pp.281-288
• /
• 2010

A carbon doped $TiO_2$ (C-$TiO_2$) photocatalyst, which shows good photocatalytic activity to Ultraviolet irradiation and visible irradiation, was successfully prepared by co-grinding of $TiO_2$ with ethanol or Activated Carbon(C), followed by heat treatment at $200^{\circ}C$ in air for 60 min. Ethanol and C were used as a representative agent of liquid and solid for carbon doping. Their influence on improving photocatalytic ability and carbon doping degree was studied with degradation of methyl orange and XPS analysis. The product prepared by co-grinding of $TiO_2$ with Ethanol had Ti-C and C-O chemical bonds and showed higher photocatalytic activity than the product prepared by co-grinding of $TiO_2$ with C, where just C-O chemical bond existed. As a result, mechanochemical route is useful to prepare a carbon doped $TiO_2$ photocatalyst activating to visible irradiation, where the solid-liquid operation is more effective than solid-solid operation to obtain a carbon doped $TiO_2$.