TW201325721A - 儲氫複材與其形成方法 - Google Patents
儲氫複材與其形成方法 Download PDFInfo
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- TW201325721A TW201325721A TW100148816A TW100148816A TW201325721A TW 201325721 A TW201325721 A TW 201325721A TW 100148816 A TW100148816 A TW 100148816A TW 100148816 A TW100148816 A TW 100148816A TW 201325721 A TW201325721 A TW 201325721A
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- hydrogen storage
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 133
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 133
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000002131 composite material Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title 1
- 239000003054 catalyst Substances 0.000 claims abstract description 89
- 239000002245 particle Substances 0.000 claims abstract description 35
- 239000011232 storage material Substances 0.000 claims abstract description 34
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 20
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 17
- 239000000956 alloy Substances 0.000 claims description 13
- 229910045601 alloy Inorganic materials 0.000 claims description 12
- 229910012375 magnesium hydride Inorganic materials 0.000 claims description 12
- 238000007772 electroless plating Methods 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052763 palladium Inorganic materials 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 239000011651 chromium Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 3
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 3
- 238000000713 high-energy ball milling Methods 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims 2
- 239000003575 carbonaceous material Substances 0.000 claims 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 23
- 239000000843 powder Substances 0.000 description 19
- 238000010521 absorption reaction Methods 0.000 description 17
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000000227 grinding Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 238000000498 ball milling Methods 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 8
- 239000003638 chemical reducing agent Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000011324 bead Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000003795 desorption Methods 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000006356 dehydrogenation reaction Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- -1 diffusion Chemical class 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 230000008313 sensitization Effects 0.000 description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 101150003085 Pdcl gene Proteins 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- B01J23/24—Chromium, molybdenum or tungsten
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Abstract
本發明提供之儲氫複材之形成方法，包括：將觸媒粒子均勻披覆於載體之表面上，以形成複合觸媒；以及將複合觸媒鑲嵌至儲氫材料之表面上，以形成儲氫複材。
Description
本發明係關於儲氫材料，更特別關於其採用的觸媒態樣。
氫能為潔淨的能源選擇，其關鍵技術之一就是安全且低成本地儲存與輸送氫氣。由於鋼瓶高壓氫氣儲運以及液態氫儲運的方式存在著儲氫密度低、安全性差、耗能、及成本高的問題，因此最具潛力的儲氫方式乃是以金屬或合金材料儲存氫。儲氫合金的原理是利用外界環境的溫度、及/或壓力改變，使合金吸收氫氣而形成合金氫化物。當需要利用氫氣時，再由合金氫化物釋放氫氣。儲放氫氣的過程如擴散、相變、及化合等階段，均受到熱效應與速度的限制而不易爆炸。
利用金屬氫化物作為儲氫媒介的優點為貯氫密度高、安全程度高、以及氫氣釋放純度高。然而目前儲氫合金的缺點在於高儲氫量的合金如鎂基合金，其吸放氫動力差，放氫操作溫度仍過高(鎂基合金一般需要300℃以上才能放氫)，大幅降低其實用性。綜上所述，目前亟需可在較低的溫度下吸放氫的儲氫複材，以利未來氫能源之運用。
本發明一實施例提供一種儲氫複材，包括：複合觸媒，包括觸媒粒子均勻披覆於載體之表面上；以及儲氫材料；其中複合觸媒鑲嵌於儲氫材料之表面上。
本發明一實施例提供一種儲氫複材之形成方法，包括：將觸媒粒子均勻披覆於載體之表面上，以形成複合觸媒；以及將複合觸媒鑲嵌至儲氫材料之表面上，以形成儲氫複材。
本發明提供之儲氫複材之形成方法如下。首先，將觸媒粒子11均勻披覆於載體13表面上，以形成複合觸媒15，如第1圖所示。在本發明一實施例中，觸媒粒子11可為銀、鈀、鎳、鉻、金、鉑或銅，且觸媒粒子之尺寸介於10nm至100nm之間。若觸媒粒子11之尺寸過大，則催化活性較低。若觸媒粒子11之尺寸過小，則無法於合成的過程中穩定形成。在本發明一實施例中，載體13可為氧化鋁、氧化鈦、氧化鈮、氧化鈷或多孔碳材，且載體13之尺寸介於100nm至1μm之間。若載體13之尺寸過大，則披覆上去的金屬觸媒粒子較粗而降低催化活性。若載體13之尺寸過小，則不容易將金屬觸媒粒子披覆於載體表面。在本發明一實施例中，觸媒粒子11與載體13之重量比介於1:100至1:10之間。若觸媒粒子之比例過高，則觸媒顆粒不易均勻分散於載體表面而形成團聚、粗化。若觸媒粒子之比例過低，則催化活性較差。
將觸媒粒子11均勻披覆於載體13表面上，以形成複合觸媒15的方法可為無電鍍法。舉例來說，可先調配觸媒鹽類溶液作為化學鍍液，接著將表面已進行敏化處理後的載體含浸於化學鍍液中。之後加入還原劑使觸媒鹽類還原成金屬觸媒並披覆於載體表面上。藉由調整還原劑濃度、反應酸鹼值、反應時間、以及反應溫度，可控制披覆於載體表面的觸媒粒子之數量與尺寸，進而得到複合觸媒。敏化載體表面之敏化劑可為SnCl2。觸媒的鹽類溶液可為銀、鈀、鎳、鉻、金、鉑或銅之化合物(可能為鹵化物或錯合物)。還原劑可為葡萄糖、次磷酸鈉、或聯氨。還原劑濃度介於0.05M至0.5M之間。若還原劑之濃度過高，則會造成金屬觸媒粒子生成過快而導致其粒徑粗化或顆粒團聚。若還原劑之濃度過低，則還原能力不足，會造成金屬觸媒粒子的生成量過低。上述無電鍍的反應時間介於5分鐘至30分鐘之間。若無電鍍的反應時間過長，則生成的金屬觸媒數量太多而容易造成顆粒團聚或粗化。若無電鍍的反應時間過短，則生成的金屬觸媒數量過少，而造成催化活性不佳。上述無電鍍的反應溫度介於15℃至75℃之間。若無電鍍的反應溫度過高，則導致金屬觸媒生成速率過於劇烈而使生成量過高。若無電鍍的反應溫度過低，則造成反應速率過慢而不易生成觸媒粒子。在本發明一實施例中，可採用SnCl2之酸性溶液敏化氧化鋁載體，使Sn2+離子吸附至載體表面。接著將敏化後之氧化鋁載體加入由NaOH、NH4OH和AgNO3所形成的銀氨水溶液中，使Sn2+氧化成Sn4+而Ag+還原成Ag。接著可再加入還原劑葡萄糖，則使更多的Ag+還原並披覆於氧化鋁載體的表面上。以無電鍍法使離子還原為奈米等級的金屬粒子於載體表面上，可避免奈米觸媒於高溫熱處理下產生凝聚的問題。藉由均勻分散於載體表面的方式可維持觸媒的高比表面積，進而增加其反應活性。
接著將複合觸媒15鑲嵌至儲氫材料17之表面上，以形成儲氫複材19，如第2圖所示。儲氫材料17可為鎂、氫化鎂、或鎂基合金如Mg1-xAx，A係Li、Ca、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Al、Y、Zr、Nb、Mo、In、Sn、Si、B、C、或Be，且0<x0.3。在本發明一實施例中，複合觸媒15與儲氫材料17之重量比介於1:100至1:10。若複合觸媒15之比例過高，則會佔據整體材料系統中太多的重量而損失一些儲氫量。若複合觸媒15之比例過低，則對於儲放氫反應的催化活性不足。
將複合觸媒15鑲嵌至儲氫材料17之表面上，以形成儲氫複材19的方法可為高能球磨法。舉例來說，可將複合觸媒15與儲氫材料17置於球磨罐中，於氬氣下進行球磨製程以形成儲氫複材19。球磨珠可為碳化鎢或不鏽鋼，其直徑介於1mm至5mm之間。若球磨珠之直徑過小，則研磨能量較低而機械嵌合的效率較差。若球磨珠之直徑過大，則容易在研磨珠與研磨罐之間的空隙產生死角，而使部分粉體無法充分被磨珠撞擊而嵌合。球磨珠與複合觸媒15及儲氫材料17之重量比介於10:1至50:1之間。若複合觸媒15及儲氫材料17之比例過高，則研磨、嵌合的效率較差。若複合觸媒15及儲氫材料17之比例過低，則容易造成研磨珠的磨耗。球磨方式可為行星式旋轉、攪拌或振盪，且球磨製程歷時0.25至1.5小時。若球磨製程歷時過短，則機械嵌合的效果較差。若球磨製程歷時過長，則可能造成觸媒金屬從載體表面脫落，並與儲氫材料產生合金化。利用機械力研磨的撞擊方式，可將複合觸媒15直接鑲嵌於儲氫材料17的表面上，使觸媒可以發揮催化活性，讓儲氫材料17在較低的溫度下有效地進行放氫。由於已先行將觸媒粒子11披覆於載體13表面，除了有助於均勻分散觸媒粒子11外，更可形成保護界面，降低觸媒粒子11在高能球磨中與儲氫材料17合金化的可能性。此外，可進一步選用堅硬的奈米陶瓷粉體作為載體13，在球磨製程中可以充當助磨劑來撞擊儲氫合金，使儲氫複材19產生晶界與缺陷而有利氫原子擴散。當複合觸媒15透過機械力的方式與儲氫材料17的表面達成固相接合時，即可於兩相的交界處提供氫原子擴散的路徑，而有助於降低吸放氫的活化能能障。另一方面，鑲嵌於儲氫材料17表面的載體13之氧離子亦有機會在表面形成微弱的氫鍵吸引力，來幫助儲氫材料17儲存的氫由內部釋放出來。
為了讓本發明之上述和其他目的、特徵、和優點能更明顯易懂，下文特舉數實施例配合所附圖示，作詳細說明如下：
首先將α-Al2O3粉體進行敏化處理(Sensitization Processing)。敏化劑的調配是取0.4g的SnCl2溶解於34 ml的去離子水中，此時SnCl2會水解產生Sn(OH2)Cl白色沉澱，再滴入3ml之1N的HCl水溶液直至整體溶液澄清即可使用。而後將2g之α-Al2O3粉體(大明株式會社，TM-DAR)浸入上述調配好的敏化劑中，於室溫下攪拌5分鐘，使Sn2+離子吸附在α-Al2O3粉體表面上，再利用離心方式去除濾液以得敏化之α-Al2O3粉體。將敏化後的α-Al2O3粉體浸入由30mL之0.9N的NaOH( l )、35mL之2N的NH4OH( l )以及30mL之0.3N的AgNO3( l )所形成的銀氨水溶液中，並加入含有C6H12O6的還原劑溶液。這時粉體表面上的Sn2+離子會將銀離子還原而吸附在α-Al2O3粉體表面，而含C6H12O6的溶液則強化銀的還原反應，待反應5分鐘的時間後，將粉體以離心方式收集，則得到複合觸媒α-Al2O3/Ag，其X光繞射圖譜如第3A圖所示，且其TEM影像如第3B圖所示。
將上述複合觸媒α-Al2O3/Ag以機械力的方式，將其鑲嵌於氫化鎂的儲氫材料上。首先將氫化鎂與複合觸媒α-Al2O3/Ag以重量百分比92:8的比例混合後，再將混合後的粉體與碳化鎢磨球以球粉重量比32:1的方式填入碳化鎢研磨罐體中，並充填氬氣。將研磨罐置入震盪球磨機(SPEX CertiPrep,Inc.,8000M)中以30分鐘的時間進行球磨撞擊，進而將複合觸媒α-Al2O3/Ag鑲嵌於氫化鎂的表面上，形成儲氫複材。上述儲氫複材於140℃下之吸氫/放氫量對時間的曲線如第4圖所示。上述吸放氫測試採用Sievert系統，在密閉且固定的容積內放入儲氫材料，藉由量測充放氫過程中氣體壓力的變化量來推知儲放氫量。吸氫測試所採用的氫氣壓力為20 atm，放氫測試所採用的氫氣壓力低於1atm。由於本實驗的Sievert系統僅能量得吸氫曲線，故放氫的量測則是由材料於第一次吸氫後，讓材料於<1atm的壓力環境下充分放氫一天，而後量測其第二次吸氫曲線來判斷該材料的放氫量。
首先將α-Al2O3粉體進行敏化處理(Sensitization Processing)。敏化劑的調配是取5g的SnCl2溶解於7.5 mL之37%的HCl( l )中，再將整體溶液以去離子水稀釋至50mL後即可使用。而後將2g之α-Al2O3粉體(大明株式會社，TM-DAR)浸入上述調配好的敏化劑中，於室溫下攪拌5分鐘，使Sn2+離子吸附在α-Al2O3粉體表面上，再利用離心方式去除濾液以得敏化之α-Al2O3粉體。將敏化後的α-Al2O3粉體浸入45mL的氯化鈀水溶液中，該溶液的調配乃是取1g的PdCl2溶解於30 ml之37%的HCl( l )中，再將整體溶液以去離子水稀釋至100mL後即可使用。這時粉體表面上的Sn2+離子會將鈀離子還原而吸附在α-Al2O3粉體表面，待反應5分鐘的時間後，將粉體以離心方式收集，則得到複合觸媒α-Al2O3/Pd，其X光繞射圖譜如第5A圖所示；其TEM分析影像則如第5B圖所示。在第5B圖中，虛線框51標示的深色部份為還原後的鈀金屬，而其餘淺色的部份為α-Al2O3粉體。
將上述複合觸媒α-Al2O3/Pd以機械力的方式，將其鑲嵌於氫化鎂的儲氫材料上。首先將氫化鎂與複合觸媒α-Al2O3/Pd以重量百分比92:8的比例混合後，再將混合後的粉體與碳化鎢磨球以球粉重量比32:1的方式填入碳化鎢研磨罐體中，並充填氬氣。將研磨罐置入震盪球磨機(SPEX CertiPrep,Inc.,8000M)中以30分鐘的時間進行球磨撞擊，進而將複合觸媒α-Al2O3/Pd鑲嵌於氫化鎂的表面上，形成儲氫複材。上述儲氫複材於140℃下之吸氫/放氫量對時間的曲線如第6圖所示。上述吸放氫測試採用Sievert系統，在密閉且固定的容積內放入儲氫材料，藉由量測充放氫過程中氣體壓力的變化量來推知儲放氫量。吸氫測試所採用的氫氣壓力為20 atm，放氫測試所採用的氫氣壓力低於1atm。放氫的量測是讓材料於第一次吸氫後，使材料於<1atm的壓力環境下充分放氫一天，而後量測其第二次吸氫曲線來判斷該材料的放氫量。
取100重量份的氫化鎂置於140℃下，其吸氫/放氫量對時間的曲線如第4及6圖所示。由第4及6圖可知，未添加觸媒的氫化鎂在140℃下幾乎無法放氫，而表面鑲嵌有複合觸媒之氫化鎂則維持穩定的放氫量。上述吸放氫測試採用Sievert系統，在密閉且固定的容積內放入儲氫材料，藉由量測充放氫過程中氣體壓力的變化量來推知儲放氫量。吸氫測試所採用的氫氣壓力為20 atm，放氫測試所採用的氫氣壓力低於1atm。放氫的量測是讓材料於第一次吸氫後，使材料於<1atm的壓力環境下充分放氫一天，而後量測其第二次吸氫曲線來判斷該材料的放氫量。
雖然本發明已以數個較佳實施例揭露如上，然其並非用以限定本發明，任何熟習此技藝者，在不脫離本發明之精神和範圍內，當可作任意之更動與潤飾，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。
11．．．觸媒粒子
13．．．載體
15．．．複合觸媒
17．．．儲氫材料
19．．．儲氫複材
51．．．虛線框
第1圖係本發明一實施例中，複合觸媒的示意圖；
第2圖係本發明一實施例中，儲氫複材的示意圖；
第3A圖係本發明一實施例中，複合觸媒α-Al2O3/Ag之X光繞射圖譜；
第3B圖係本發明一實施例中，複合觸媒α-Al2O3/Ag之TEM影像；
第4圖係本發明之實施例與比較例之觸媒的吸氫/放氫量對時間的曲線圖；
第5A圖係本發明一實施例中，複合觸媒α-Al2O3/Pd之X光繞射圖譜；
第5B圖係本發明一實施例中，複合觸媒α-Al2O3/Pd之TEM影像；以及
第6圖係本發明之實施例與比較例之觸媒的吸氫/放氫量對時間的曲線圖。
Claims (14)
- 一種儲氫複材，包括：一複合觸媒，包括一觸媒粒子均勻披覆於一載體之表面上；以及一儲氫材料；其中該複合觸媒鑲嵌於該儲氫材料之表面上。
- 如申請專利範圍第1項所述之儲氫複材，其中該觸媒粒子包括銀、鈀、鎳、鉻、金、鉑、或銅，且該觸媒粒子之尺寸介於10nm至100nm之間。
- 如申請專利範圍第1項所述之儲氫複材，其中該載體包括氧化鋁、氧化鈦、氧化鈮、氧化鈷、或多孔碳材，且該載體之尺寸介於100nm至1μm之間。
- 如申請專利範圍第1項所述之儲氫複材，其中該複合觸媒中，該觸媒粒子與該載體之重量比介於1:100至1:10之間。
- 如申請專利範圍第1項所述之儲氫複材，其中該儲氫材料包括鎂、氫化鎂、或鎂基合金。
- 如申請專利範圍第1項所述之儲氫複材，其中該複合觸媒與該儲氫材料之重量比介於1:100至1:10之間。
- 一種儲氫複材之形成方法，包括：將一觸媒粒子均勻披覆於一載體之表面上，以形成一複合觸媒；以及將該複合觸媒鑲嵌至一儲氫材料之表面上，以形成一儲氫複材。
- 如申請專利範圍第7項所述之儲氫複材之形成方法，其中該觸媒粒子包括銀、鈀、鎳、鉻、金、鉑、或銅，且該觸媒粒子之尺寸介於10nm至100nm之間。
- 如申請專利範圍第7項所述之儲氫複材之形成方法，其中該複合觸媒中，該觸媒粒子與該載體之重量比介於1:100至1:10之間。
- 如申請專利範圍第7項所述之儲氫複材之形成方法，其中該載體包括氧化鋁、氧化鈦、氧化鈮、或氧化鈷，且該載體之尺寸介於100nm至1μm之間。
- 如申請專利範圍第7項所述之儲氫複材之形成方法，其中該複合觸媒與該儲氫材料之重量比介於1:100至1:10之間。
- 如申請專利範圍第7項所述之儲氫複材之形成方法，其中該儲氫材料包括鎂、氫化鎂、或鎂基合金。
- 如申請專利範圍第7項所述之儲氫複材之形成方法，其中將該觸媒粒子均勻披覆於該載體之表面上，以形成該複合觸媒之步驟係一無電鍍法。
- 如申請專利範圍第7所述之儲氫複材之形成方法，其中將該複合觸媒鑲嵌至該儲氫材料之表面上，以形成該儲氫複材之步驟係一高能球磨法。
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| CN201110449945.8A CN103183313B (zh) | 2011-12-27 | 2011-12-29 | 储氢复合材料与其形成方法 |
| US13/553,712 US9174209B2 (en) | 2011-12-27 | 2012-07-19 | Hydrogen storage composites and methods for manufacturing the same |
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| CN111774568B (zh) * | 2020-06-12 | 2022-06-10 | 榆林学院 | 一种气化渣镁镍合金储氢复合材料的工业化生产装置 |
| CN114477082B (zh) * | 2021-12-28 | 2023-07-21 | 桂林电子科技大学 | 一种纳米Ni-Nb-O掺杂氢化镁的储氢材料及其制备方法和应用 |
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| CN1245329C (zh) * | 2003-06-10 | 2006-03-15 | 中国科学院大连化学物理研究所 | 含氢无机化合物水溶液制氢催化剂及制氢方法 |
| JP5095909B2 (ja) * | 2003-06-24 | 2012-12-12 | ローム・アンド・ハース・エレクトロニック・マテリアルズ，エル．エル．シー． | 触媒組成物および析出方法 |
| US7250386B2 (en) | 2003-07-18 | 2007-07-31 | Energy Conversion Devices, Inc. | Quantum limit catalysts and hydrogen storage materials |
| US20050126663A1 (en) | 2003-12-11 | 2005-06-16 | Fetcenko Michael A. | Catalyzed hydrogen desorption in Mg-based hydrogen storage material and methods for production thereof |
| TWI297284B (en) * | 2004-12-06 | 2008-06-01 | Ind Tech Res Inst | Hydrogen storage composite and preparation thereof |
| US7951749B2 (en) | 2005-10-11 | 2011-05-31 | The Regents Of The University Of Michigan | Enhancing hydrogen spillover and storage |
| CN101289161A (zh) * | 2007-04-20 | 2008-10-22 | 中国科学院大连化学物理研究所 | 一种储氢材料的制备方法 |
| CN101671788B (zh) * | 2008-09-12 | 2013-06-19 | 财团法人工业技术研究院 | 镁基储氢材料纳米化方法 |
| US9623393B2 (en) * | 2008-10-31 | 2017-04-18 | Asemblon, Inc. | Dehydrogenation of cyclic thioethers |
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| US20130084474A1 (en) * | 2010-03-18 | 2013-04-04 | Randell L. Mills | Electrochemical hydrogen-catalyst power system |
| WO2012014225A2 (en) * | 2010-07-26 | 2012-02-02 | Council Of Scientific & Industrial Research | An improved process for the storage delivery of hydrogen using catalyst |
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| TWI450764B (zh) | 2014-09-01 |
| US9174209B2 (en) | 2015-11-03 |
| CN103183313B (zh) | 2014-10-15 |
| US20130161559A1 (en) | 2013-06-27 |
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