CN106882844B - Nucleocapsid NiO/Ni3The preparation method of N materials - Google Patents
Nucleocapsid NiO/Ni3The preparation method of N materials Download PDFInfo
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- CN106882844B CN106882844B CN201510933741.XA CN201510933741A CN106882844B CN 106882844 B CN106882844 B CN 106882844B CN 201510933741 A CN201510933741 A CN 201510933741A CN 106882844 B CN106882844 B CN 106882844B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
The present invention relates to a kind of nano material NiO/Ni with mesoporous nucleocapsid3The preparation method of N, the preparation method use solvent thermal process, and water or ethyl alcohol are solvent, and the two adds in varing proportions；Using urea and nickel sulfate as raw material, the two is respectively with 2:1~5:1 different mol ratio example adds in；After being heated 4~24 hours at 100 DEG C~200 DEG C, presoma is carried out at 400 DEG C~600 DEG C to the calcining of 2~6 hours.The NiO of generation is nitrogenized again, then NiO materials are nitrogenized 2~6 hours at 350 DEG C~450 DEG C.The NiO/Ni with mesoporous nucleocapsid can be obtained3N materials.The method of the present invention has the advantages that simple synthetic method, reaction temperature are low etc..
Description
Technical field
The present invention relates to a kind of NiO/Ni3The preparation method of N compounds.
Background technology
Transition metal nitride is because with high-melting-point, high rigidity, highly thermally conductive property, excellent electric conductivity, good chemical stabilization
Property, the excellent characteristic such as corrosion-resistant and eka-platinium catalytic performance become focus of concern.Be widely used in cutting element,
The numerous areas such as wear parts, coating material is more in terms of the research of nitridation nickel composite metal, as nickel oxide tungsten adds hydrogen to make
Catalyst；Or the magnetism and microwave property of Fe-Ni-N compounds are studied, a series of Fe- of different Fe/Ni atomic ratios
Ni-N compounds are respectively provided with higher saturation magnetization and smaller coercivity, show typical soft ferromagnetic feature.With
This simultaneously, Fe-Ni-N compound samples show good absorbing property；Relative to nickel oxide, nickel oxide is then relatively applied
In terms of capacitor.Such as NiO with meso-hole structure can largely be used for making electrochemical capacitor electrode, and keep higher
Specific capacitance and good capacitive property.The preparation method of NiO has very much, such as Guo Wei, Xie Zhongwei et al. collosol and gel legal system
Standby NiO, (uses nickel sulfate (NiSO4·H2O alkoxide obtained in distilled water and ethyl alcohol) is dissolved in, and alkalinity is carried out to solution with NaOH
Hydrolysis, NiO electrochomeric films are deposited after being sufficiently stirred with dip-coating-czochralski method again.) for another example K.C.Min, Y.H.You et al.
Once NiO was prepared using mocvd method, for another example L.Cattin, B.A.Reguig, A.KheLi et al. were once prepared using spray pyrolysis
NiO, using different precursor solutions, using glass as substrate, in deposition, underlayer temperature is 350 DEG C, is selected respectively
NiCl2·6H2O、Ni(NO3)2·6H2O、NiSO4·4H2O is dissolved in acid salt solution as presoma, and spraying forms NiO.Again
If radio-frequency magnetron sputter method prepares NiO films, with silicon chip and quartzy two kinds of materials respectively as bottom liner, target is sintered
NiO solid targets are passed through argon gas and oxygen in coating process in reative cell.
Invention content
The purpose of the present invention is that providing a kind of raw material is easy to get, and technical process simply prepares mesoporous nucleocapsid
NiO/Ni3The preparation method of N.
The purpose of the present invention is what is reached by following proposal.
1. respectively with 2:1~5:The urea and nickel sulfate of 1 molar ratio are material.
2. the solvent thermal reaction 4~for 24 hours at 100 DEG C~200 DEG C, after carry out suction filtration drying.
3. calcining 2~6h at 400 DEG C~600 DEG C, black NiO materials are obtained.
4. ammonia gas of the NiO materials with nucleocapsid at 350 DEG C~450 DEG C is nitrogenized into 2~6h.
Nucleocapsid NiO/Ni is prepared the present invention provides a kind of3The method of N, its main feature is that：
1. preparation flow and equipment are simple.
2. nitrogen source used in is industrial ammonia, safer compared to hydrogen and nitrogen mixed gas.
3. the reaction process temperature of the present invention is low, the time is relatively short, is easy to control.
4. this method is easy to operate.
Description of the drawings
Fig. 1 is Ni (HCO3)2XRD diagram.
Fig. 2 is the XRD diagram of NiO.
Fig. 3 is NiO/Ni3The XRD diagram of N.
Fig. 4 is Ni3The XRD diagram of N.
Fig. 5 is Ni (OH)2XRD diagram.
Fig. 6 is Ni (OH)2SEM figure.
Fig. 7 is Ni (HCO3)2SEM figure.
Fig. 8 is NiO/Ni3The SEM figures of N.
Specific embodiment
In order to further illustrate the present invention, following embodiment is enumerated.
Embodiment 1
Nickel salt NiSO4·6H2O and urea are with 1:5 molar ratios mix, and add 50ml water and 30ml ethyl alcohol progress solvent heat anti-
Should, it is put into Muffle furnace and is warming up to 160 DEG C with 4 DEG C/min rates, cool down after keeping 18h.It is cooled to room temperature taking-up, through XRD characterization,
Ni (HCO can be obtained3)2(Fig. 1), after SEM is scanned, it can be seen that Ni (HCO3)2External morphology (Fig. 7).It is put by primary product
It is placed in tube furnace, 500 DEG C is warming up to 4 DEG C/min, be down to room temperature taking-up after calcining 2h, NiO (Fig. 2) can be obtained, then put
Enter in nitriding furnace and vacuumize, lead to ammonia, be warming up to 400 DEG C, nitrogenize 2 hours, through XRD characterization, can obtain NiO/Ni3N materials (figure
3) it, is characterized through SEM, it can be seen that NiO/Ni3N materials have nucleocapsid (Fig. 8).
Embodiment 2
Nickel salt NiSO4·6H2O and urea are with 1:5 molar ratios mix, and add 50ml water and 30ml ethyl alcohol progress solvent heat anti-
Should, it is put into Muffle furnace and is warming up to 160 DEG C with 4 DEG C/min rates, cool down after keeping 18h.It is cooled to room temperature taking-up, through XRD characterization,
Ni (HCO can be obtained3)2, it is positioned in tube furnace by primary product, is warming up to 500 DEG C with 4 DEG C/min, room temperature is down to after calcining 2h
It takes out, NiO can be obtained, then put it into nitriding furnace and vacuumize, lead to ammonia, be warming up to 350 DEG C, nitrogenize 4 hours, through XRD characterization,
It can obtain Ni3N materials (Fig. 4).
Embodiment 3
Nickel salt NiSO4·6H2O and urea are with 1:2 molar ratios mix, and add 50ml water and 30ml ethyl alcohol progress solvent heat anti-
Should, it is put into Muffle furnace and is warming up to 160 DEG C with 4 DEG C/min rates, cool down after keeping 4h.It is cooled to room temperature taking-up, through XRD characterization,
Ni (OH) can be obtained2(Fig. 5), after SEM is characterized, it can be seen that Ni (OH)2External morphology (such as Fig. 6).It is placed by primary product
In tube furnace, 600 DEG C are warming up to 4 DEG C/min, room temperature taking-up is down to after calcining 2h, NiO can be obtained, then put it into nitriding furnace
In vacuumize, lead to ammonia, be warming up to 350 DEG C, nitrogenize 3 hours, through XRD characterization, can obtain NiO materials.
Embodiment 4
Nickel salt NiSO4·6H2O and urea are with 1:5 molar ratios mix, and add 50ml water and 30ml ethyl alcohol progress solvent heat anti-
Should, it is put into Muffle furnace and is warming up to 100 DEG C with 4 DEG C/min rates, cool down after keeping 18h.It is cooled to room temperature taking-up, through XRD characterization,
Ni (OH) can be obtained2, it is positioned in tube furnace by primary product, is warming up to 450 DEG C with 4 DEG C/min, room temperature is down to after calcining 2h
It takes out, NiO can be obtained, then put it into nitriding furnace and vacuumize, lead to ammonia, be warming up to 450 DEG C, nitrogenize 2 hours, through XRD characterization,
It can obtain Ni3N materials.
Embodiment 5
Nickel salt NiSO4·6H2O and urea are with 1:5 molar ratios mix, and add 50ml water and 30ml ethyl alcohol progress solvent heat anti-
Should, it is put into Muffle furnace and is warming up to 200 DEG C with 4 DEG C/min rates, cool down after keeping 4.It is cooled to room temperature taking-up, it, can through XRD characterization
Obtain Ni (OH)2, it is positioned in tube furnace by primary product, is warming up to 600 DEG C with 4 DEG C/min, being down to room temperature after calcining 2h takes
Go out, NiO can be obtained, then put it into nitriding furnace and vacuumize, lead to ammonia, be warming up to 450 DEG C, nitrogenize 2 hours, it, can through XRD characterization
Obtain Ni3N materials.
Embodiment 6
Nickel salt NiSO4·6H2O and urea are with 1:2 molar ratios mix, and add 50ml water and 30ml ethyl alcohol progress solvent heat anti-
Should, it is put into Muffle furnace and is warming up to 100 DEG C with 4 DEG C/min rates, cool down after keeping 18h.It is cooled to room temperature taking-up, through XRD characterization,
Ni (OH) can be obtained2, it is positioned in tube furnace by primary product, is warming up to 400 DEG C with 4 DEG C/min, room temperature is down to after calcining 2h
It takes out, NiO can be obtained, then put it into nitriding furnace and vacuumize, lead to ammonia, be warming up to 450 DEG C, nitrogenize 2 hours, through XRD characterization,
It can obtain Ni3N materials.
Embodiment 7
Nickel salt NiSO4·6H2O and urea are with 1:5 molar ratios mix, and 80ml water is added to carry out solvent thermal reaction, is put into Muffle
160 DEG C are warming up to 4 DEG C/min rates in stove, is cooled down after keeping 20h.It is cooled to room temperature taking-up, through XRD characterization, Ni can be obtained
(HCO3)2, it is positioned in tube furnace by primary product, 500 DEG C is warming up to 4 DEG C/min, room temperature taking-up is down to after calcining 2h,
NiO can be obtained, then puts it into nitriding furnace and vacuumizes, leads to ammonia, is warming up to 375 DEG C, nitrogenizes 2 hours, through XRD characterization, can obtain
To NiO materials.
Embodiment 8
Nickel salt NiSO4·6H2O and urea are with 1:2 molar ratios mix, and 80ml water is added to carry out solvent thermal reaction, is put into Muffle
170 DEG C are warming up to 4 DEG C/min rates in stove, holding cools down afterwards for 24 hours.It is cooled to room temperature taking-up, through XRD characterization, Ni can be obtained
(OH)2, it is positioned in tube furnace by primary product, 600 DEG C is warming up to 4 DEG C/min, room temperature taking-up is down to after calcining 2h, it can
NiO is obtained, then puts it into nitriding furnace and vacuumizes, leads to ammonia, is warming up to 400 DEG C, is nitrogenized 2 hours, through XRD characterization, can obtain
NiO/Ni3N materials.
Embodiment 9
Nickel salt NiSO4·6H2O and urea are with 1:5 molar ratios mix, and 80ml water is added to carry out solvent thermal reaction, is put into Muffle
160 DEG C are warming up to 4 DEG C/min rates in stove, holding cools down afterwards for 24 hours.It is cooled to room temperature taking-up, through XRD characterization, Ni can be obtained
(HCO3)2, it is positioned in tube furnace by primary product, 600 DEG C is warming up to 4 DEG C/min, room temperature taking-up is down to after calcining 2h,
NiO can be obtained, then puts it into nitriding furnace and vacuumizes, leads to ammonia, is warming up to 400 DEG C, nitrogenizes 3 hours, through XRD characterization, can obtain
To NiO/Ni3N materials.
Embodiment 10
Nickel salt NiSO4·6H2O and urea are with 1:5 molar ratios mix, and 80ml water is added to carry out solvent thermal reaction, is put into Muffle
160 DEG C are warming up to 4 DEG C/min rates in stove, holding cools down afterwards for 24 hours.It is cooled to room temperature taking-up, through XRD characterization, Ni can be obtained
(HCO3)2, it is positioned in tube furnace by primary product, 600 DEG C is warming up to 4 DEG C/min, room temperature taking-up is down to after calcining 2h,
NiO can be obtained, then puts it into nitriding furnace and vacuumizes, leads to ammonia, is warming up to 400 DEG C, nitrogenizes 2 hours, through XRD characterization, can obtain
To NiO/Ni3N materials.
Claims (7)
1. nucleocapsid NiO/Ni3The preparation method of N materials, it is characterized in that：Nickel source with urea is mixed and is dissolved in solvent, is carried out
The persursor material of generation is sintered by solvent thermal reaction, then the NiO materials of generation are carried out nitrogen treatment, can prepare Jie
Hole nucleocapsid NiO/Ni3N materials；
The temperature of the solvent thermal reaction is 100 DEG C~200 DEG C, and the time of reaction is 4~24 hours；
The nitriding temperature of the nitrogen treatment is 350 DEG C~450 DEG C, and nitridation time is 2~6 hours.
2. preparation method described in accordance with the claim 1, it is characterized in that：The nickel source is NiSO4·6H2O；Control nickel source with
The molar ratio of urea is 1:2~1:5.
3. preparation method described in accordance with the claim 1, it is characterized in that：The solvent is water or ethyl alcohol or the two with arbitrary
Ratio mixes.
4. preparation method described in accordance with the claim 1, it is characterized in that：The persursor material that solvent thermal reaction is generated is Ni
(HCO3)2Or Ni (OH)2。
5. preparation method described in accordance with the claim 1, it is characterized in that：The sintering temperature is controlled at 400 DEG C~600 DEG C.
6. preparation method described in accordance with the claim 1, it is characterized in that：Described sintering time control was at 2~6 hours, product
For NiO.
7. preparation method described in accordance with the claim 1, it is characterized in that：Nitrogen source used is ammonia during the nitrogen treatment.
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| CN109055974B (en) * | 2018-07-23 | 2020-03-27 | 电子科技大学 | Porous Ni-N-O nano-particle material and preparation method and application thereof |
| CN110171807A (en) * | 2019-06-10 | 2019-08-27 | 陕西师范大学 | A method of preparing three nickel by powder of nano silicon nitride |
| CN112058299B (en) * | 2020-09-10 | 2021-11-16 | 中山大学 | Multi-shell nickel-based nitride nano composite material and preparation method and application thereof |
| CN114214663A (en) * | 2022-01-06 | 2022-03-22 | 武汉工程大学 | Nitrogen vacancy modified nickel nitride electrocatalytic material and preparation method and application thereof |
| CN114573028B (en) * | 2022-04-28 | 2022-08-12 | 华中科技大学 | Transition metal compound with heterojunction structure, preparation method thereof and composite lithium-supplementing material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1251351A (en) * | 1998-10-21 | 2000-04-26 | 中国科学院金属腐蚀与防护研究所 | Method for producing spheroidal nickelous hydroxide series powder |
| CN1861528A (en) * | 2005-05-13 | 2006-11-15 | 黄石理工学院 | Process for preparing nano NiO by ammonia water single phase precipitation |
| CN103946146A (en) * | 2011-10-24 | 2014-07-23 | 康奈尔大学 | Mesoporous metal nitride materials and methods |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1251351A (en) * | 1998-10-21 | 2000-04-26 | 中国科学院金属腐蚀与防护研究所 | Method for producing spheroidal nickelous hydroxide series powder |
| CN1861528A (en) * | 2005-05-13 | 2006-11-15 | 黄石理工学院 | Process for preparing nano NiO by ammonia water single phase precipitation |
| CN103946146A (en) * | 2011-10-24 | 2014-07-23 | 康奈尔大学 | Mesoporous metal nitride materials and methods |
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