CN106702198A - 一种铝介孔材料及其制备方法 - Google Patents
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 29
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000013335 mesoporous material Substances 0.000 title claims abstract description 25
- 239000004411 aluminium Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910020828 NaAlH4 Inorganic materials 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 238000010926 purge Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 238000009489 vacuum treatment Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 12
- 239000001257 hydrogen Substances 0.000 abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 12
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- 238000003860 storage Methods 0.000 abstract description 6
- 239000011232 storage material Substances 0.000 abstract description 6
- 238000004146 energy storage Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
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- 238000002441 X-ray diffraction Methods 0.000 description 4
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- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
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- 229910010277 boron hydride Inorganic materials 0.000 description 3
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- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- 239000012448 Lithium borohydride Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
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Abstract
本发明公开了一种铝介孔材料及其制备方法。所述铝介孔材料的孔径分布集中在5‑15nm。所述制备方法,包括:惰性气体气氛下,对原料NaAlH4进行焙烧,焙烧结束后冷却。本发明制备的铝介孔材料,制备方法较为简单易行。孔径分布集中在5‑15nm之间,可以作为一种新型结构催化剂对储氢/储能材料进行纳米限域。
Description
技术领域
本发明涉及介孔材料,尤其涉及一种孔径分布集中在5-15nm左右的铝介孔材料,还涉及该材料的制备方法和应用。
背景技术
1992年Mobil的科学家Kresge等人首次成功制备出了孔径可调的介孔SiO2,命名为MCM-41。2001年Jonah Erlebacher采用去合金技术成功制备出尺寸约为40nm、相对密度为30%的金纳米多孔网状结构。在纳米多孔材料中按照孔径大小分布可以划分为微孔(孔径小于2nm)、介孔(2-50nm)、大孔(大于50nm)。由于材料的多孔化赋予原来材料崭新的优异性能,扩大了材料的应用范围,多孔材料的低密度、高比表面积、低热导率、高比强度、良好的吸能等使其在分离、传感器、催化、减震缓冲、消声等方面得到广泛应用,尤其在储能材料领域有很好的应用。近年来制备出的纳米多孔结构的碳材料由于具有大比表面积、独特的孔结构以及丰富的纳米孔,使其在储能领域应用潜力巨大,也引起了人们的高度重视。然而,对于多孔材料在纳米尺度上,面向不同储能需求的多功能组合和调控仍是目前材料领域的一个难点问题。
在储氢材料目前面临诸多难题的同时,研究者们提出了通过纳米限域技术提高材料的储氢性能,而一种性能优异的纳米多孔材料对储氢材料领域具有重大意义,目前迫切需要研发出一种良好的有序纳米多孔材料来促进储氢材料的进一步发展。
发明内容
发明目的:为了弥补现有材料的不足,本发明提供了一种新的铝介孔材料,孔径分布无序集中。本发明还提供了所述铝介孔材料的制备方法及应用。
技术方案:
本发明所述的铝介孔材料,其孔径分布集中在5-15nm。
所述铝介孔材料的平均孔直径10-13nm。
本发明还提供了所述的铝介孔材料的制备方法,包括:惰性气体气氛下,对原料NaAlH4进行焙烧,焙烧结束后冷却。
所述的惰性气体可以为氩气。
焙烧前,可先对原料NaAlH4进行压制成型。压制时压力值为10-12MPa,保持时间为10-12min。
焙烧时,焙烧温度为450-650℃,保温时间为5-10小时,升温速率为1-20℃/min。优选的,焙烧温度为550℃,保温时间为7小时,升温速率为5-10℃/min。
升温时,可采用分段升温的方式,加热第一段以8~10℃/min的升温速率从室温加热到X℃,第二阶段以5~7℃/min的升温速率从X℃加热到焙烧温度Y℃,其中X与Y的温度差为30-50℃。
焙烧过程中用高纯氩气气流吹扫样品,流量为60-120sccm,同时采用机械泵进行动态真空处理。优选的,流量为90-100sccm。
焙烧结束后冷却,冷却速率为1-50℃/min,冷却过程处于动态真空状态。
制备原理:本发明提供的介孔铝材料的制备原理,是通过NaAlH4原位反应产生气体(氢气)以及金属钠的挥发而造孔,具体涉及如下反应:
(1)3NaAlH4→Na3AlH6+2Al+3H2;
(2)Na3AlH6→3NaH+Al+3/2H2;
(3)NaH→Na+1/2H2。
与现有技术相比,本发明的有益效果为:
本发明制备的铝介孔材料孔径分布无序,主要集中在5-15nm之间,同时该材料孔隙率较高,合成产物纯度高,制备工艺简单易行,适用于大批量商业生产。可以作为一种新型结构催化剂广泛应用于储氢/储能等材料领域的纳米限域和结构催化。
根据近年来的研究表明,对储氢材料通过纳米多孔材料进行纳米限域取得了很好的效果,尤其对于反应复合硼氢化物来说,能够明显降低其脱氢温度,使硼氢化物在纳米级空间进行脱氢所需的热力学条件较为温和,并且对其吸氢动力学也有所提高。
将纯度为95%的LiBH4粉末和纯度为99%的Al粉以摩尔比为2:1的比例混合,通过行星式高能球磨机进行球磨,球料比50:1,球磨时间20h,转速设置为500rpm。对最终获得的材料2LiBH4-Al进行储氢性能测试,结果表明,与单纯LiBH4相比,其反应活化能明显降低到94KJ/mol,其初始脱氢温度降到280℃,等温脱氢动力学也有显著提高,本项研究结果已经在The Journal of Physical Chemistry C 113(2009)18424–18430期刊中发表。另外根据Mingxia Gao等人在Journal of Alloys and Compounds 670(2016)135-143发表文章报道,Ca(BH4)2中掺杂Al粉后其初始脱氢温度由350℃降低到230℃,脱氢速率由0.034wt%/min提高至0.286wt%/min,脱氢表观活化能由189KJ/mol降低至153KJ/mol,整体储氢性能大幅提高。所以本发明所制备的铝介孔材料由于崭新的纳米多孔结构具有作为新型结构催化剂进行纳米限域的效果.可将制备好的介孔铝材料可以通过与反应氢化物储氢材料机械球磨后纳米限域进介孔铝材料中以改善材料储氢性能。
附图说明
图1为实施例1中实验组1-2制得材料的X射线衍射(XRD)图谱;
图2为实施例1中实验组1-2制得材料的扫描电镜图(标尺50μm)和能谱图;
图3为实施例1中实验组1-2制得材料的透射电镜图(标尺100nm)和选区电子衍射图;
图4为实施例1中实验组1-2制得材料的氮气物理吸附测试结果图。
具体实施方式
下面结合具体实施方式进一步阐释本发明。
实施例1
一种铝介孔材料的制备步骤如下:
(1)在浓度为99.9999%的氩气气氛保护下称取纯度为98%的NaAlH4粉末采用压片装置进行压制成型,压制时采用的压强为11-13MPa,保压时间为10min。然后将成型的片状材料置于氧化铝坩埚中,并在氧化铝坩埚外层包覆一层铜箔,在铜箔上留孔,以便于后续工艺中通过控制铜箔与坩埚间预留的孔隙以控制气流吹扫量和出气量。
(2)将步骤(1)处理好的样品置于管式炉中,用氩气洗气三遍后调节氩气进气气流,同时用机械泵抽真空达到动态平衡并保持管内负压稳定。设置温度对样品进行焙烧,焙烧过程中用高纯氩气(99.9999%)吹扫样品,流量为90sccm,同时采用机械泵进行动态真空(-0.1bar)处理,全程保证氩气气流和抽真空处于动态平衡且保持负压稳定;
其中,焙烧的升温过程分两段进行,加热第一段以10℃/min的升温速率从室温加热到X℃,第二阶段以5℃/min的升温速率从X℃加热到Y℃,保温时间为7个小时。
本实施例设置不同焙烧温度(Y),考察焙烧温度对最终形成材料的影响。
实验组1-1:X=420℃,Y=450℃;
实验组1-2:X=500℃,Y=550℃;
实验组1-3:X=600℃,Y=650℃。
(3)保温结束后进行冷却,冷却速率为1-50℃/min。冷却过程处于真空状态。
最终所获得的材料即为铝介孔材料,对最终获得的材料分别进行XRD、扫描电镜、透射电镜、电子衍射、氮气物理吸附测试分析。
图1~图4为焙烧温度550℃时获得的铝介孔材料的检测结果。XRD测试及精修表明,样品纯度很高,纯度>98%(图1);扫描电镜分析表明,样品中有极少量微孔存在,EDS能谱同样表明Al的含量很高,Al含量达97.5%(图2),表明所制备的铝介孔材料纯度高,不含杂相;透射电镜形貌和电子衍射图表明,多孔Al样品绝大部分孔径分布为纳米级孔道,孔分布均匀(图3);氮气物理吸附测试分析结果(分别是氮气吸附、脱附曲线和孔径分布曲线)表明,孔径集中范围在5-15nm,平均孔直径12.8nm,可定义为介孔结构的Al材料(图4)。
实验组1-1和实验组1-3获得的材料XRD测试及精修表明,当保温温度为450℃时样品纯度稍微有所降低,当保温温度为650℃时,样品纯度无明显变化,但颗粒粒度增大,这是因为温度过高时所获得的介孔铝材料会发生部分软化并凝结成小球,而温度过低时会导致金属钠挥发不完全而使纯度降低。
实施例2
调节步骤(2)中焙烧过程中吹扫样品的氩气流量,分别设置为60sccm、90sccm、100sccm,其余步骤同实施例1,考察不同流量对最终制得材料的影响。
实验结果表明,当进气流量较低时(60sccm),样品纯度有所降低,当进气流量为90sccm时,样品纯度高,精修表明达98%,当进气流量提高到100sccm时结果和90sccm基本一致。
Claims (6)
1.一种铝介孔材料,其特征在于,孔径分布集中在5-15nm之间。
2.根据权利要求1所述的铝介孔材料的制备方法,其特征在于,包括:惰性气体气氛下,对原料NaAlH4压制成型后进行焙烧,焙烧结束后冷却。
3.根据权利要求2所述的铝介孔材料的制备方法,其特征在于,压制时压力值为10-12MPa,保持时间为10-12min。
4.根据权利要求2所述的铝介孔材料的制备方法,其特征在于,焙烧时,焙烧温度为450-650℃,保温时间为5-10小时,升温速率为1-20℃/min。
5.根据权利要求2所述的铝介孔材料的制备方法,其特征在于,焙烧过程中用高纯氩气气流吹扫样品,流量为60-120sccm,同时采用机械泵进行动态真空处理。
6.根据权利要求2所述的铝介孔材料的制备方法,其特征在于,焙烧结束后冷却,冷却速率为1-50℃/min,冷却过程处于真空状态。
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