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1 Journal of Korean Powder Metallurgy Institute Vol 18 No DOI: 10150/KPMI e x 5Mg(OH) MgSO 3H O x w MgO NH OH w a báv y aá½xk aá½ aá½ cá½ bá½ a * aw» l bš w œw ck Effect of MgO and NH OH on Formation of 5Mg(OH) MgSO 3H O Whiskers Ri Yu a b Jae-Hwan Pee a Hyung Tae Kim a Kyung Ja Kim a Young-Woong Kim c Woong Kim b and YooJin Kim a * a Engineering ceramic center Korea Institute of Ceramic Engineering & Technology Icheon Korea b Department of Materials Science and Engineering Korea University Seoul Korea c TAEJIN GnS Co LTD 68- Gojan-Dong Namdong-Gu Incheon Korea (Received April 5 011; Revised May 1 011; Accepted May ) Abstract Magnesium hydroxide sulfate hydrate whiskers (5Mg(OH) MgSO 3H O abbreviated ) were prepared using hydrothermal reaction with magnesium oxide (MgO) and magnesium sulfate (MgSO 7H O) as the starting materials The effects of the molar ratio of MgSO /MgO and amount of NH OH were studied As a result whiskers co-existed with hexagonal plate Mg(OH) at low concentration of SO The molar ratio of MgSO 7H O/MgO was 7:1 uniform whiskers were formed without impurity such as Mg(OH) Appropriate amount of NH OH has affected to formation of high quality Their morphologies and structures were determined by powder X-ray diffraction (XRD) scanning electron microscopy (SEM) and thermo-gravimetric analyzer (TGA) Keywords : Magnesium hydroxide sulfate hydrate whiskers MgO NH OH Hydrothermal reaction Whisker 1 v p ³ šƒ ƒœ z š s» w w e x Magnesium Hydroxide Sulfate Hydrate (5Mg(OH) MgSO 3H O abbreviated )ƒ š ( Magnesium Hydroxide Sulfate Hydrate ) e x üy š k v ù š ƒ w [1 ] *Corresponding Author : [Tel : ; 83 Mg(OH) MgCl MgSO w w ƒ w e x (5Mg(OH) MgSO 3H O) 51 (5Mg(OH) MgSO sh O) w xk w [3] e ¼ ph SO ƒ w [] w EDTA (Ethylenediaminetetraacetic acid) w ù dropping temperature w y y g x w p y sww yw ƒw y k y ù» ù [-6] ù w w ³ w x j ÿw

2 8 Áv yá½xká½ Á½ Á½ Á½ Table 1 Reaction condition of Sample Starting materials Mole ratio NH OH ƒ (ml) Reaction time (h) ReactionG temperature ( o C) 1 3: 1:3 MgO MgSO 3 1: :7 5 6 MgO MgSO 1: MgSO ƒ OH š + Mg w q Mg(OH) ƒ x» Mg(OH) ƒ w ù w» w w x Mg(OH) w v p w Mg(OH) ww x w j e yw w w [6] w» w MgSO 7H O MgO w MgSO 7H O NH OH w w wš w MgO w MgO MgSO 7H O w ù w š š w w MgSO 7H O w ƒ w x 1 e x (5Mg(OH) MgSO 3H O) w y (MgSO 7H O) y (MgO) (NH OH) w ƒ» y yw () w w w» w ƒƒ x t 1 w t v y y w y (16~8 g/1~3 mol) y (1968~6888 g/~7 mol) 80 ml yww 10 z lv» z 170 C w t v y w ƒ w w w w» N g w M y 0 ml N(Normality) (5~33 ml) ƒw z 10 z 1-7 v w 170 C þ óù z þƒ z» w e e w w 80 C» w z p sƒ w x y w» w x (SEM Model JSM-6390 JEOL Japan) w w X-ray z (XRD Model D/Max 500 Rigaku Japan)»» w»»(tga Model SDT Q600 TA instruments USA) w sƒw Journal of Korean Powder Metallurgy Institute

3 3 5Mg(OH) MgSO 3H O 형성에 관한 와 MgO NH OH 영향 85 결과 및 고찰 반응물에 따른 형성의 영향 일반적으로 는 를 이용하여 합 성하지만 본 연구에서는 산화마그네슘과 황산마그네 슘을 이용하였다 그림 과 그림 는 산화마그네슘과 황산마그네슘의 몰비율을 조절하여 합성한 의 분석 결과와 이미지이다 시험조건으로 반응 온도는 이며 반응시간은 시간으로 동일한 조건에서 합성되었다 황산마그네슘 과 산화마그네슘의 몰비율이 인 경우엔 가 생성되는 것을 가 생성되기보다는 그림 의 패턴을 통해서 확인할 수 있으며 가 응집체 형태로 존재함을 판상 형태의 그림 의 이미지를 통해 확인할 수 있다 이는 산화마그네슘의 농도가 황산마그네슘의 농도보 다 높을 경우 상대적으로 농도가 낮아져 가 합성되기 때문이다 보다는 의 농도가 더 높을 경우에는 수열반응이 진행되 는 동안 생성되는 중간생성물인 가 이온과 반응하기보다는 이온과 반응하여 가 형성한다 이처럼 의 양은 중 쉽게 31 1 XRD SEM 170 C :3 1(a) XRD (a) SEM SO MgO + Mg SO OH OH + MgOH Fig 1 XRD patterns of the as-prepared products synthesized at the molar ratio of MgSO 7HO/MgO: (a) :3 (b) 3:1 and (c) 7:1 Fig SEM images of the as-prepared products synthesized at the molar ratio of MgSO 7HO/MgO: (a) :3 (b) 3:1 and (c) 7:1 Vol 18 No 3 011

4 유 리 피재환 김형태 김경자 김영웅 김 웅 김유진 86 간생성물인 와 의 형성에 영향을 주기 때문에 는 중요한 요소 이다 반면에 황 산마그네슘의 농도가 산화마그네슘의 농도보다 높은 경우엔 대부분 가 형성되는 것을 볼 수 있다 그림 황산마그네슘과 산화마그네슘의 가 여전 몰비율이 인 경우엔 적은 양의 히 불순물로써 존재하는 것을 그림 를 통해 확인 할 수 있었다 그림 와 그림 에서 확인 할 수 있듯이 황산마그네슘과 산화마그네슘의 몰비율이 형성 없이 의 인 경우에 가 형성되는 것을 볼 수 있었다 즉 황산마그 네슘과 산화마그네슘의 비율에서도 알 수 있듯이 의 농도가 을 형성하는데 있어 중요 한 성장 요소로써 작용한다는 것을 알 수 있었다 + + Mg MgOH ph [ 7-8] ( 1(b)~(c)) 3:1 1(b) 7:1 1(c) (c) SO [ 7-8] 반응시간 조절에 의한 의 영향 황산마그네슘과 산화마그네슘의 몰비율이 일 경우에는 이미 앞서 확인한 바와 같이 순수한 을 얻을 수 있었다 따라서 이번 실험에서는 반응시간에 따른 생성을 확인하기 위하여 황 산마그네슘과 산화마그네슘의 몰비율이 일 경우를 3 7:1 Fig 3 XRD patterns of the as-prepared products synthesized at different reaction time: (a) hour (b) hour and (c) 8 hour Fig SEM images of the as-prepared products synthesized at different reaction time: (a) hour (b) hour and (c) 8 hour Journal of Korean Powder Metallurgy Institute

5 5Mg(OH) MgSO 3H O 선택하여 실험을 진행하였다 그림 과 그림 에서는 황산마그네슘과 산화마그네슘의 몰비율이 일 때 반응시간을 조절한 경우의 결정상 분석결과와 미세 조직 결과이다 그림 와 그림 처럼 반응 시 간이 시간 미만인 경우엔 응집된 판상형 결정 이 확인되지만 그림 와 그림 에서 볼 수 있듯이 반응시간이 증가할수록 판 상형 의 결정상은 점차 사라지고 순수한 침 상형 만 존재하는 것을 볼 수 있다 이온들이 와 반응하여 가 되더 라도 반응시간이 길어질수록 이온과 배위되어 을 얻을 수 있다 즉 황산마그네 슘과 산화마그네슘의 몰비율이 인 경우에는 반응 시간 시간일 때 고순도의 를얻 을 수 있었다 출발물질의 몰비율이 인 경우에는 반 응시간이 시간일 때 이미 순수한 를 얻을 수 있었으며 몰비율이 인 경우의 시간 반응결과와 비교가 될 수 있다 형성에 미치는 의 영향 그림 와 그림 은 암모니아 함량변화에 따라 제 조된 의 결정분석 결과와 이미지이다 반응에 사용된 암모니아는 로 3 형성에 관한 와 MgO NH OH 영향 87 3(a) (a) peak 3(b)~(c) (b)~(c) + Mg + OH MgOH SO 8 7: SEM NHOH XRD N Fig 5 XRD patterns of the as-prepared products synthesized at different ammonia solution: (a) 5 ml (b) 10 ml (c) 15 ml and (d) 33 ml 희석 하여 사용하였다 암모니아의 농도가 낮을 경우 에는 형성 없이 고순도의 만 Fig 6 SEM images of the as-prepared products synthesized at different ammonia solution: (a) 5 ml (b) 10 ml (c) 15 ml and (d) 33 ml Vol 18 No 3 011

6 88 Áv yá½xká½ Á½ Á½ Á½ x ( 5(a)~(c)) 5 ml ƒw 10 ml ƒ y w mw ƒ w w ƒ Mg(OH) q x ù w j ƒ +ƒ SO w» Mg + MgOH OH w Mg(OH) x w» w 6(a)~(c) m 0 µm 0~50 µm ¼ ƒ 33 ml q x Mg(OH) y 5(d) 6(d) mw y w H O 5MgSO + NH OH 5Mg(OH) H O MgSO + 5Mg(OH) 5Mg(OH) MgSO 3H O MgSO»» Mg(OH) ƒ x Mg(OH) + MgOH OH w w ww e x x w 3 e x p sƒ y mw w e x p sƒ w 7 e x p w TGA e x M y N 10 ml ƒw 170 C mw w w w š 150 C k y ù w 50~300 C 370~00 C w 3 H Oƒ wš 5Mg(OH) ƒ 5 w» e w 11% 17% y w 900 C SO ƒ SO 3»y» w 1050 C e x MgO w ƒ w e x w w y y mw y ƒ š e x ƒ w y w š e x y y ƒ 7:1 170 C mw w Mg(OH) ƒ y ƒ j q x Mg(OH) š w e x w y w y w 5~15 ml ƒw ³ w e x» w»» x w š x Fig 7 TG/DTA results for whisker [1] H Iwanaga T Iwasaki K Reizen T Matsunami M Ichihara and S Takeuchi: J Am Ceram Soc 75 (199) 197 [] H Lu Y Hu J Xiao Z Wang Z Chen and W Fan: Journal of Korean Powder Metallurgy Institute

7 e x 5Mg(OH) MgSO 3H O x w MgO NH OH w 89 J Mater Sci 1 (006) 363 [3] C Gao X Li L Feng Z Xiang and D Zhang: Chem Eng J 150 (009) 551 [] X Yan D Xu and D Xue: Acta Mater 55 (007) 577 [5] X T Sun W T Shi and W C Zhu: Nanoscale Res Lett 3 (008) 386 [6] J Li L Xiang and Y Jin: J Mater Sci 1 (006) 135 [7] J Lv L Qiu and B Qu: Nanotechnology 15 (00) 1576 [8] C Yan and D Sue: J Phys Chem B 110 (006) 1581 Vol 18 No 3 011

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