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pH = 3 —oª¥„¦—°³Ž¸˜·„ ‹³Å—o µ¦¨³¨µ¥š¸É ¤¸ o¤ ‹µ„œ´ÊœÁšÄnĜ Teflon-lined stainless steel autoclave (bomb)
(»—űצÁš°¦r ¤´¨) œÎµÁ oµÁ˜µ° ˜´ÊŠ°»–®£¼¤·Åªoš¸É 180 oC Áž} œÁª¨µ 72 ´ÉªÃ¤Š (3 ª´œ) ¨oµŠ—oª¥œÊÎ µ„¨´Éœ ¨³Á°šµœ°¨
®¨µ¥Ç ‡¦´ÊŠ šÎµµ¦š¸É ´ŠÁ‡¦µ³®rŗoÄ®o®oŠ Á¡ºÉ°Á˜¦¸ ¥¤ª·Á‡¦µ³®r ¤´˜·š´Ê ŠšµŠ„µ¥£µ¡Â¨³šµŠÁ‡¤¸˜n°Åž
„µ¦«¹„¬µ¤´˜·°Šµ¦ž¦³„°ªµÁœÁ—¸¥¤°°„ÅŽ—rš¸É ´ŠÁ‡¦µ³®rŗo
1. Powder X-ray diffractometer (PXRD)
´œš¹„×¥Á‡¦ºÉ°Š JEOL ¦»nœ JDX-3530 X-ray diffractometer „´ graphite monochromator čo
¦´Š¸Á°„Žr Cu KĮ (O = 1.541 0
$ ) ĜnªŠ¤»¤¦³®ªnµŠ 5 o ” 2T ” 60o
2. Fourier Transform Infrared Spectrometer (FTIR)
¥¸É®o ° Perkin Elmer ץčo KBr pellet nªŠ‡ªµ¤¥µª‡¨ºÉœ 400 – 4000 cm-1
3. Scanning Electron Microscope (SEM)
JSM-5800 LV, JEOL Áš‡œ·‡„µ¦š—°™nµ¥£µ¡°·Á¨È„˜¦°œÅ¤Ã‡¦„¦µ¢
4. Thermal Gravity Analysis (TGA)
¥¸É®o ° Perkin Elmer, TGA 7 nªŠ°»–®£¼¤·„µ¦š—° 50 oC ™¹ Š 1,000 oC š¸É°´˜¦µ 10 oC/min ×¥
čo N2
Ÿ¨„µ¦ª·‹´¥Â¨³°£· ž¦µ¥Ÿ¨
1. „µ¦«¹„¬µ„µ¦Áž¨¸É¥œÂž¨Š °ŠÂ™„µ¦—¼—„¨ºœ FT-IR
‹µ„Áž„˜¦´¤Â™„µ¦—¼ —„¨ºœ‹³¤¸Â™„µ¦—¼ —„¨ºœ °Š®¤¼n¢{ Š„r´œš¸É ε‡´ —´Šœ¸Ê Á¨ ‡¨ºÉœ 1411 cm-1 Áž}œ
™„µ¦—¼—„¨ºœ °Š®¤¼n¢{ Š„r´œ NH ¤¸ „µ¦´ÉœÂŠ° (Bending) Á¨ ‡¨ºÉœ 996 cm -1 Áž}œÂ™„µ¦—¼—„¨ºœ °Š V5+= O
š¸É¤¸Á¨ °°„Ž· Á—´œÁšnµ„´ +5 Á¨ ‡¨ºÉœ 893 ¨³ 996 cm-1 Áž}œÂ™„µ¦—¼—„¨ºœ °Š®¤¼n¢{ Š„r´œ V-O ¨³ V-O-V
˜µ¤¨Îµ—´ ¨³Á¨ ‡¨ºÉœ 470 Áž}œÂ™„µ¦—¼ —„¨ºœ °Š Zn-O —Š—´ Š˜µ¦µŠ
˜µ¦µŠš¸É 1 —Š o°¤¼¨Â™„µ¦—¼ —„¨ºœš¸É ε‡´ °Šµ¦ž¦³„°ªµÁœÁ—¸¥¤°°„ÅŽ—r
µ¦ž¦³„° ž¦³Á£š„µ¦´Éœ/Á¨ ‡¨ºÉœ (cm-1)
Qas NH V5+ = O V-O V-O-V Zn-O
1 1411 996 893 996 470
2. „µ¦«¹„¬µ„µ¦Áž¨¸É¥œÂž¨Š¦³®ªnµŠ°»–®£¼¤·„´„µ¦¼Á¸¥œÊ宜´„—oª¥ TGA
Ĝ„µ¦ª·Á‡¦µ³®r„µ¦¼Á¸¥œÊ宜´„ °Šµ¦ž¦³„°ªµÁœÁ—¸¥¤°°„ÅŽ—r ‹³ÂnŠÁž}œ 2 nªŠ°»–®£¼¤· ‡º°nªŠ
°»–®£¼¤· 176-308 °Š«µÁŽ¨ÁŽ¸¥ Áž}œ„µ¦¼Á¸¥œÊ宜´„ °Š®¤¼n¢{ Š„r´œ ¨³n ªŠš¸É 2 °»–®£¼¤· 377 °Š«µÁŽ¨ÁŽ¸¥
Áž}œ„µ¦¼Á¸¥ °Š®¤¼n¢{Š„r´œ VxOy