CN105694810A - Method for preparing CuO/porous carbon composite wave-absorbing material with ZIF-67 as template - Google Patents
Method for preparing CuO/porous carbon composite wave-absorbing material with ZIF-67 as template Download PDFInfo
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Abstract
The invention discloses a method for preparing a CuO/porous carbon composite wave-absorbing material with ZIF-67 as a template.The method comprises the steps of synthesizing metal organic framework ZIF-67 powder with the precipitation method; calcining the ZIF-67 powder in the presence of nitrogen, dissolving substances generated after calcination in HF solution to obtain a product with metal Co removed, and marking the product as NPC; dissolving NPC in Cu(NO3)2 solution, removing upper solution after reaction, driving the obtained solid substance, and then conducting calcination at 300-600 DEG C in the presence of nitrogen, so that the CuO inlaid porous carbon composite wave-absorbing material is obtained.The preparing method has the advantages that the process is simple, production cost is low, follow-up treatment is easy, and complicated synthesis equipment is not needed, and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to and a kind of prepare the CuO method inlaying the composite wave-suction material of porous carbon with metallic organic framework ZIF-67 for template, belong to microwave absorbing material technical field。
Background technology
Development along with electromagnetic wave technology, novel wave-absorbing material develops to lightweight, minimal thickness, broadband, the strong direction that absorbs gradually, in recent years, due to advantages such as material with carbon element density are little, electromagnetic attenuation ability is strong, carbon-based material obtains the extensive concern of people as lightweight absorbing material。Cobalt-based imidazate metal-organic framework materials (ZIF-67) has higher heat stability, additionally also there is the advantages such as specific surface area is big, porosity is high, preparation technology is simple, be suitable to batch production, adopting it is that predecessor gained material with carbon element has higher graphitization character, has possessed the essential condition developing into lightweight microwave absorbing material。
Copper oxide (CuO) is a kind of P-type semiconductor, there is narrower energy gap (1.2eV), due to performance and the potential application widely thereof of its uniqueness, get the attention in the application such as photoswitch, anode material, catalysis, optoelectronic pole and gas sensor。In recent years, the composite of CuO as microwave absorbing material by big quantity research。Such as, Zen et al. is prepared for CuO-carbon fibre composite by calcining the method for Cu-carbon fiber in atmosphere, find that this complex is 1.8mm in matching thickness, during 7.8GHz, its reflection loss reaches optimal value for-29.6dB (ZengJ, XuJ, TaoP, etal.Ferromagneticandmicrowaveabsorptionpropertiesofcopp eroxide-carbonfibercomposites.JournalofAlloysandCompound s, 2009,487 (1): 304-308.)。Zhao et al. is prepared for Ni-CuO core-shell structure by two-step hydrothermal route method, and this composite construction is under relatively low matching thickness (1.7mm), and reflection loss RL value reaches optimum for-62.2dB。Test proves that CuO has relatively low dielectric constant values, the interface existed between Ni and CuO in Ni-CuO complex enhances interfacial polarization, improve the microwave absorbing property (BiaoZhao of material, GangShao, BingbingFan, WanyuZhaoandRuiZhang, Facilesynthesisandenhancedmicrowaveabsorptionpropertieso fnovelhierarchicalheterostructuresbasedonaNimicrosphere-CuOnano-ricecore-shellcomposite.Phys.Chem.Chem.Phys., 2015, 17, 6044-6052)。In addition relatively low for CuO dielectric constant (ε ' ≈ 4) also improves the impedance matching of composite。Therefore, CuO also can improve the impedance matching property of material with carbon element as a kind of impedance matching agent。
Summary of the invention
Goal of the invention: the technical problem to be solved is to provide a kind of prepares the CuO method inlaying porous carbon composite wave-suction material with metallic organic framework ZIF-67 for template, and preparation method technique is simple, production cost is low for this。
For solving above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of with the ZIF-67 method preparing CuO/ porous carbon composite wave-suction material for template, comprise the steps:
Step 1, sedimentation method synthesis metallic organic framework ZIF-67 powder;
Step 2, is placed in the ZIF-67 powder of step 1 under nitrogen and calcines, and by organic macromolecule carbonization, is dissolved in HF solution by the material after calcining, obtains removing the product of metal Co, be marked as NPC;
Step 3, is dissolved in Cu (NO by the product NPC of step 23)2In solution, remove upper solution, the solids dried that will obtain after reaction, be placed under nitrogen after drying again and calcine, namely obtain the CuO porous carbon composite wave-suction material inlayed;Wherein, described calcining heat is 300 DEG C~600 DEG C。
Wherein, in step 2, for every 1mgZIF-67 powder, the volume of required HF solution is 0.5mL。
Wherein, in step 2, the mass percentage concentration of described HF solution is 10%。
Wherein, in step 2, described calcining heat is 700 DEG C, and calcination time is 5h。
Wherein, in step 3, for every 1mgNPC, required Cu (NO3)2The volume of solution is 100mL。
Wherein, in step 3, described Cu (NO3)2The concentration of solution is 0.4mol/L。
Wherein, in step 3, described baking temperature is 60 DEG C, and drying time is 24h。
Wherein, in step 3, described calcination time is 3h。
The principle of preparation method of the present invention: (this porous carbon is pure NPC to impregnate porous carbon by simple copper nitrate, remove the metal Co in CoNPC by HF to obtain) method obtain the mixture of porous carbon load copper nitrate, then mixture is calcined under optimum conditions and obtains the CuO porous carbon complex (CuONPC) inlayed。
Beneficial effect: there is the problems such as preparation method complexity, equipment requirements height and cost are big compared to existing carbon microwave receptor material, preparation method of the present invention has that technique is simple, production cost is low, subsequent treatment is easy and without the advantage of complicated synthesis device, is suitable to industrialization large-scale production。
Accompanying drawing explanation
Fig. 1 is the CuO that the embodiment of the present invention 1,2,3 the prepares X ray diffracting spectrum inlaying porous carbon composite wave-suction material;
Fig. 2 is the SEM picture of the NPC of the embodiment of the present invention 1 gained;
Fig. 3 is the CuO that the embodiment of the present invention 1 the prepares SEM picture inlaying porous carbon composite wave-suction material;
Fig. 4 is the CuO that the embodiment of the present invention 1 the prepares reflection loss collection of illustrative plates inlaying porous carbon composite wave-suction material;
Fig. 5 is the CuO that the embodiment of the present invention 2 the prepares reflection loss collection of illustrative plates inlaying porous carbon composite wave-suction material;
Fig. 6 is the CuO that the embodiment of the present invention 3 the prepares reflection loss collection of illustrative plates inlaying porous carbon composite wave-suction material。
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme is described further, but the scope of protection of present invention is not limited thereto。
Embodiment 1
The present invention prepares the CuO method inlaying porous carbon composite wave-suction material with metallic organic framework ZIF-67 for template, specifically includes following steps:
Step 1, according to bibliographical information (NagyL.Torad, MingHu, ShinsukeIshihara, HiroakiSukegawa, AlexisA.Belik, MasatakaImura, KatsuhikoAriga, YoshioSakka, andYusukeYamauchi, DirectSynthesisofMOF-DerivedNanoporousCarbonwithMagnetic CoNanoparticlestowardEfficientWaterTreatment.Small, 2014, 10, 2096-2107) sedimentation method synthesis metallic organic framework ZIF-67 powder: weigh 2.63g methylimidazole and be placed in 100mLA beaker, 30mL methanol and 10mL distilled water it is sequentially added into again in A beaker, stirring to material is completely dissolved;600mg polyvinylpyrrolidone and 520mgCoCl is added in 100mLB beaker2·6H2O, then in B beaker, add 40mL methanol, stirring 5min is completely dissolved to material, seals ageing 24h with preservative film;By the mixing of materials in A beaker and B beaker, after reaction 24h, the precipitation bottom mixed material is put into after centrifugation and methanol are washed vacuum drying oven dry 5h at 60 DEG C, grinds to obtain purple ZIF-67 powder after drying;
Step 2, takes 100mgZIF-67 powder and puts in tube furnace and to calcine 5h in 700 DEG C under nitrogen atmosphere, be dissolved in the HF solution of 50mL10wt% by the material after calcining, and agitator treating more than 3 times obtains removing the product of metal Co, is marked as NPC;Wherein, tube furnace heating rate is 1 DEG C/min;
Step 3, takes 100mgNPC powder and is dissolved in the Cu (N0 that 100mL concentration is 0.4mol/L3)2Solution stirs 3h, stands and treat powder drop, go upper solution, the solids vacuum drying 24h at 60 DEG C that will obtain, obtain the porous carbon of load copper nitrate in mesopore orbit, by load, the porous carbon powder of copper nitrate puts into N in tube furnace2Calcine 3h in 300 DEG C under atmosphere, namely obtain the CuO porous carbon composite wave-suction material inlayed, be S-300 by the Product Labeling of gained。
Embodiment 2
Step 1, with embodiment 1;
Step 2, with embodiment 1;
Step 3, takes 100mgNPC powder and is dissolved in the Cu (NO that 100mL concentration is 0.4mol/L3)2Solution stirs 3h, stands and treat powder drop, go upper solution, the solids vacuum drying 24h at 60 DEG C that will obtain, obtain the porous carbon of load copper nitrate in mesopore orbit, by load, the porous carbon powder of copper nitrate puts into N in tube furnace2Calcine 3h in 450 DEG C under atmosphere, namely obtain the CuO porous carbon composite wave-suction material inlayed, be S-450 by the Product Labeling of gained。
Embodiment 3
Step 1, with embodiment 1;
Step 2, with embodiment 1;
Step 3, taking 100mgNPC powder, to be dissolved in 100mL concentration be 0.4mol/LCu (NO3)2Solution stirs 3h, stands and treat powder drop, go upper solution, the solids vacuum drying 24h at 60 DEG C that will obtain, obtain the porous carbon of load copper nitrate in mesopore orbit, by load, the porous carbon powder of copper nitrate puts into N in tube furnace2Calcine 3h in 600 DEG C under atmosphere, namely obtain the CuO porous carbon composite wave-suction material inlayed, be S-600 by the Product Labeling of gained。
Fig. 1 is the CuO that embodiment 1,2,3 the prepares X ray diffracting spectrum inlaying porous carbon composite wave-suction material, as can be seen from Figure 1, all there is graphitized carbon (002) crystallographic plane diffraction peak at 2 θ=30.55 ° places in the NPC that embodiment 1,2,3 obtains, the product S-300 principal phase that 1300 DEG C of calcinings of embodiment obtain is CuO, the product S-450 principal phase that 2450 DEG C of calcinings of embodiment obtain is Cu, in addition with Cu2The diffraction maximum of O and CuO exists, when calcining heat is 600 DEG C, in the product S-600 sample that 3600 DEG C of calcinings of embodiment obtain, the oxide diffraction maximum of copper is very weak, the diffraction maximum of basic only surplus Cu, and the valence state of Cu based products raises with calcining heat and is gradually lowered。
Fig. 2 is the SEM photograph of the NPC of embodiment 1 gained, figure it is seen that the NPC granule-morphology prepared by embodiment 1 is granatohedron。
Fig. 3 is the CuO that embodiment 1 the prepares SEM photograph inlaying porous carbon composite wave-suction material, from figure 3, it can be seen that the pattern compared to Fig. 2 NPC, CuO inlays the granatohedron of porous carbon composite wave-suction material certain contraction, and overall morphology change is little。
Fig. 4 is the reflection loss collection of illustrative plates of the product S-300 that embodiment 1 prepares, as can be seen from Figure 4, product S-300 shows the microwave absorbing property of excellence, it is 11GHz in frequency, when matching thickness is 2mm, it is 3.5GHz that optimum RL value can reach-27dB, the RL bandwidth less than-10dB, when matching thickness is 1-5mm, the RL value frequency less than-10dB can cover 3-13GHz。
Fig. 5 is the reflection loss collection of illustrative plates of the product S-450 that embodiment 2 prepares, from fig. 5, it can be seen that product S-450 is at best match frequency 16.5GHz, under best matching thickness 1mm, best RL value can only achieve-7dB。
Fig. 6 is the reflection loss collection of illustrative plates of the product S-600 that embodiment 3 prepares, as can be seen from Figure 6, product S-600 shows poor absorbent properties, the result shows that the embedding of CuO can be greatly improved the absorbing property of porous carbon microwave absorbing material, and after CuO is reduced to Ni metal, the microwave absorbing property of sample significantly reduces。
It is embedded by electromagnetic wave transparent material inside wave absorbing agent duct that the present invention prepares the method for composite wave-suction material, after the composite wave-suction material obtained and paraffin proportioning under relatively low coating layer thickness, embody the lightweight broad-band microwave absorbing property of excellence, and Granular composite is uniform, do not reunite, can as practical lightweight broad-band electromagnetic wave absorption material。Preparation method of the present invention overcomes tradition and prepares the complicated technology of porous carbon/magnetic nanoparticle material, and preparation method technique of the present invention is simple, production cost is low, it is easy to industrialized production。
Obviously, above-described embodiment is only for clearly demonstrating example of the present invention, and is not the restriction to embodiments of the present invention。For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description。Here without also cannot all of embodiment be given exhaustive。And the apparent change that these spirit belonging to the present invention are extended out or variation are still among protection scope of the present invention。
Claims (8)
1. one kind with the ZIF-67 method preparing CuO/ porous carbon composite wave-suction material for template, it is characterised in that comprise the steps:
Step 1, sedimentation method synthesis metallic organic framework ZIF-67 powder;
Step 2, is placed in the ZIF-67 powder of step 1 under nitrogen and calcines, and is dissolved in HF solution by the material after calcining, obtains removing the product of metal Co, is marked as NPC;
Step 3, is dissolved in Cu (NO by the product NPC of step 23)2In solution, after reaction, remove upper solution, calcine at 300 DEG C~600 DEG C in nitrogen again after the solids dried obtained, namely obtain the CuO porous carbon composite wave-suction material inlayed。
2. according to claim 1 with the ZIF-67 method preparing CuO/ porous carbon composite wave-suction material for template, it is characterised in that: in step 2, for every 1mgZIF-67 powder, the volume of required HF solution is 0.5mL。
3. according to claim 1 with the ZIF-67 method preparing CuO/ porous carbon composite wave-suction material for template, it is characterised in that: in step 2, the mass percentage concentration of described HF solution is 10%。
4. according to claim 1 with the ZIF-67 method preparing CuO/ porous carbon composite wave-suction material for template, it is characterised in that: in step 2, described calcining heat is 700 DEG C, and calcination time is 5h。
5. according to claim 1 with the ZIF-67 method preparing CuO/ porous carbon composite wave-suction material for template, it is characterised in that: in step 3, for every 1mgNPC, required Cu (NO3)2The volume of solution is 100mL。
6. according to claim 1 with the ZIF-67 method preparing CuO/ porous carbon composite wave-suction material for template, it is characterised in that: in step 3, described Cu (NO3)2The concentration of solution is 0.4mol/L。
7. according to claim 1 with the ZIF-67 method preparing CuO/ porous carbon composite wave-suction material for template, it is characterised in that: in step 3, described baking temperature is 60 DEG C, and drying time is 24h。
8. according to claim 1 with the ZIF-67 method preparing CuO/ porous carbon composite wave-suction material for template, it is characterised in that: in step 3, described calcination time is 3h。
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CN106169381A (en) * | 2016-07-26 | 2016-11-30 | 北京工业大学 | A kind of synthetic method constructing the azotized carbon nano pipe with electrochemical capacitance performance based on ZIF 67 |
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