CN109112341A - Layer stephanoporate nickel cobalt (alloy)-carbon composite block material preparation method with electromagnetic wave absorption performance - Google Patents
Layer stephanoporate nickel cobalt (alloy)-carbon composite block material preparation method with electromagnetic wave absorption performance Download PDFInfo
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- CN109112341A CN109112341A CN201810850825.0A CN201810850825A CN109112341A CN 109112341 A CN109112341 A CN 109112341A CN 201810850825 A CN201810850825 A CN 201810850825A CN 109112341 A CN109112341 A CN 109112341A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
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Abstract
Layer stephanoporate nickel cobalt (alloy)-carbon composite block material preparation method with electromagnetic wave absorption performance that the invention discloses a kind of, include the following steps: for deionized water, glycerol to be uniformly mixed, addition polyacrylic acid is stirred well to polyacrylic acid and is completely dispersed dissolution, it is added and is hydrolyzed as nickel source, the cobalt source of presoma, add the stirring of gel promotor；Gelation is handled after resulting colloidal sol sealing, and resulting block xerogel is placed in inert atmosphere tube furnace by resulting block gel drying, is warming up to 400~1000 DEG C of 100~300min of heat preservation, layer stephanoporate nickel cobalt (alloy)-carbon composite block material is made.Resulting layer stephanoporate nickel cobalt (alloy)-carbon composite block material is prepared using the method for the present invention, there is stable absorbing property.
Description
Technical field
Layer stephanoporate nickel cobalt (alloy)-carbon composite block material system with electromagnetic wave absorption performance that the present invention relates to a kind of
Preparation Method.
Background technique
Development and electronic product during the progress of the mankind and the development of society, along with electronic information technology
Popularization and application, the living standard of the mankind is greatly improved, quality of life has and is obviously improved.These electronic products are very big
While facilitating people's daily life, the also many trouble of band.This is because with the electronic products such as mobile phone, computer and electricity
Device equipment is widely applied, we will receive the radiation of the electromagnetic wave of various frequencies and energy in usual living environment.Electromagnetism spoke
Range, which spends height, to form electromagnetic pollution beyond the degree that body and environment are able to bear.Electromagnetic pollution is due to its seriousness
Have become the big pollution sources of emerging one for threatening human lives.A large amount of medicine case shows that excessive electromagenetic wave radiation can be right
Human health threatens, and will affect the normal operation of the nervous system, endocrine system, repeats itself system of people.Therefore
The electromagnetism wave material that development can absorb the daily frequency range that can be touched has a wide range of applications in civil field.Inhale wave material
Material becomes anti-because that efficient absorption electromagnetic radiation and can have the characteristics that more efficient and pervasive compared with electromagnetic shielding material
Control the main means of electromagnetic pollution.
Nanometer nickel-cobalt alloy material has special surface magnetism and catalytic performance, in high density magnetic memory materials, high-quality
The fields such as amount magnetic fluid material, electromagnetic shielding and absorbing material tool has been widely used.
Nickel cobalt (alloy) absorbing property and its chemical composition, institutional framework and granularity and pattern are closely related.Material is brilliant
The particle size of grain is smaller, and specific surface area is bigger, higher to the absorption of electromagnetic wave.
The method for preparing nickel cobalt (alloy) traditional at present mainly has machine-alloying, oxalates pyrolysismethod, Ultrasonic Radiation
The methods of method, hydrothermal reduction method, electro-deposition, the nickel cobalt (alloy) particle size of traditional preparation method preparation is big, impurity is more, pattern
It is difficult to obtain stability contorting, inhales wave stability and be difficult to solve.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of layer stephanoporate nickel cobalt (alloy)-with electromagnetic wave absorption performance
The preparation method of carbon composite block material can be used for inhaling wave field.
In order to solve the above technical problem, the present invention provides a kind of, and the layer stephanoporate nickel cobalt with electromagnetic wave absorption performance is closed
Gold-carbon composite block material preparation method, includes the following steps:
A), 1.0~4.0mL deionized water is weighed to be added in the glycerol of 1.0~3.0mL, magnetic agitation to be uniformly mixed；
B), the polyacrylic acid of 1.0~4.0g is added into liquid obtained by step A), is stirred well to polyacrylic acid and is completely dispersed
Dissolution；
C), it is added into the uniform solution that step B) is obtained as 0.5~3.0g of nickel source of presoma, as presoma
0.5~4.0g of cobalt source, is hydrolyzed with stirring, hydrolysis time be 3~5h (at this point, forerunner's physical efficiency by complete hydrolysis, generate with
Corresponding hydroxide)；
D), be added into liquid (clear transparent solutions) obtained by step C) 1.0~2.5ml of gel promotor stirring 20~
30min；
E), the colloidal sol sealing that step D) is obtained is placed on 40~60 DEG C of 48 ± 2h of (in baking oven) gelation；
F), the resulting block gel of step E) is placed in 50~60 DEG C (in baking oven) dry 48 ± 2h；
G), the resulting block xerogel of step F) is placed in inert atmosphere tube furnace, is heated up with 0.5~5 DEG C/min fast
Rate is warming up to 400~1000 DEG C, keeps the temperature 100~300min, and layer stephanoporate nickel cobalt (alloy)-carbon composite block material is made.
Improvement as layer stephanoporate nickel cobalt (alloy)-carbon composite block material preparation method of the invention:
Step B) used by polyacrylic acid molecular weight be 3000,5000,50000,10000；
Step C) nickel source be NiCl2·6H2O、Ni(NO3)2·6H2O, cobalt source CoCl2·6H2O、Co(NO3)2·
6H2O；
Step D) used in gel promotor be propylene oxide, propylene oxide, formamide.
Further improvement as layer stephanoporate nickel cobalt (alloy)-carbon composite block material preparation method of the invention: step
Rapid D) in, gel promotor is added in the form being added dropwise, and the temperature of control system is no more than 60 DEG C during dropwise addition.
The present invention is by originals such as phase separation agent (polyacrylic acid), solvent (deionized water, glycerol), presoma, gel promotors
The porous blocks of nickel cobalt complex hydroxide are prepared by synthesis in material；By being heat-treated under inert atmosphere, organic matter high temperature
Carbon is resolved under effect, hydroxide is cleaved the carbon to be formed and is reduced into metal, and it is multiple to finally obtain layer stephanoporate nickel cobalt (alloy)-carbon
Close block materials.
Compared with the existing technology, the present invention has following technical advantage:
1), phase separation agent introduces micron-sized macropore, and nickel cobalt (alloy) can be made to keep certain apparent size, convenient for storage
And transport；Gel promotor can slowly improve the pH value of system, control the formation of skeleton；
2) change of component of nickel cobalt arbitrary proportion, may be implemented under the premise of guaranteeing alloy block；
3) it, is heat-treated under different temperatures in an inert atmosphere, can rationally control the particle size of alloy；
4) micropore that, is formed after Overheating Treatment, mesoporous combination mutually separate generated macroporous structure, form macropore-
Mesoporous-micropore layer stephanoporate nickel cobalt (alloy) block materials；
5), production technology, equipment are simple, are easy to industrialization；
6), production process does not generate harmful substance.
In conclusion guaranteeing the equal of nickel cobalt alloy material with the wet chemistry method of mutually separation using collosol and gel in the present invention
The size of even property, nickel cobalt (alloy) can control it by the temperature of heat treatment, and pore-size distribution, specific surface area depend on
The proportion of beginning raw material.Therefore the nickel cobalt (alloy) being prepared has stable absorbing property.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 is the appearance pictorial diagram (a) and scanning electron microscope (SEM) photograph (b of porous silica silicon bulk aeroge prepared by embodiment 1
~f)；(b)~(f) is after porous nickel cobalt (alloy) block is heat-treated at a temperature of 400 DEG C, 500 DEG C, 600 DEG C, 800 DEG C, 1000 DEG C
Scanning electron microscope (under 50000 times) picture, it can be seen that there is the macropore (about 1 μm) that continuously penetrates through in block.
Fig. 2 is the absorbing property of porous nickel cobalt (alloy) prepared by embodiment 1, wherein 800 degree of heat treatment absorbing properties are best,
Minimal reflection loss is -19dB, effectively absorbs (dB is less than -10dB) bandwidth and reaches 2GHz.
Fig. 3 is adsorption desorption curve (above) and the aperture BJH point of the nitrogen of porous nickel cobalt (alloy) block prepared by embodiment 2
Cloth curve (following figure).Show that the specific surface area that porous nickel cobalt (alloy) block is heat-treated at a temperature of 600 DEG C can by BET calculated result
Up to 167m2·g-1。
Fig. 4 is the XRD spectrum of porous nickel cobalt (alloy) block prepared by embodiment 3, the peak position of (111) crystal face of nickel cobalt (alloy)
Between pure cobalt and pure nickel, show that nickel cobalt (alloy) can be formed under 800 DEG C of heat treatment.In figure, it is followed successively by from top to bottom
pure Co、Ni-Co、pure Ni。
Specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited in
This.
The step D of following case) in, propylene oxide is added in the form of dropwise addition, the temperature of control system during dropwise addition
Degree is no more than 60 DEG C.
Embodiment 1, a kind of layer stephanoporate nickel cobalt (alloy)-carbon composite block material preparation method, are successively walked as follows
It is rapid:
A), weigh 1.2mL deionized water to be added in the glycerol of 2.4mL, magnetic agitation to 2 is mixed thoroughly；
B), the polyacrylic acid (50000) of 4.0g is added into liquid obtained by step A), is stirred well to polyacrylic acid and divides completely
Dissipate dissolution；
C), the nickel source (NiCl as presoma is added into the uniform solution that step B) is obtained2·6H2O) 0.713g, cobalt
Source (CoCl2·6H2O 5h is hydrolyzed, at this time presoma complete hydrolysis in) 1.426g under stirring.
D), propylene oxide 1.76ml is added into the clear transparent solutions that step C) is obtained and stirs 20~30min；
E), the colloidal sol sealing that step D) is obtained is placed in gelation 48h in 40~60 DEG C of baking ovens；
F), block gel obtained by step E) is placed in 50~60 DEG C of baking ovens dry 48h；
G), by block xerogel obtained by step F), it is placed in inert atmosphere tube furnace, with 2.5 DEG C/min heating rate point
It is not warming up to following 5 temperature spots: 400 DEG C, 500 DEG C, 600 DEG C, 800 DEG C or 1000 DEG C, 100min is kept the temperature, to make accordingly
Obtain 5 kinds of layer stephanoporate nickel cobalt (alloy)-carbon composites.
Embodiment 2, a kind of layer stephanoporate nickel cobalt (alloy)-carbon composite block material preparation method, are successively walked as follows
It is rapid:
A), weigh 2.4mL deionized water to be added in the glycerol of 1.2mL, magnetic agitation to solution is mixed thoroughly；
B), into liquid obtained by step A), the polyacrylic acid (50000) of 4.0g is added, it is complete to be stirred well to polyacrylic acid
Dispersing and dissolving；
C), presoma nickel source (NiCl is added into the uniform solution that step B) is obtained2·6H2O) 0.713g, cobalt source
(CoCl2·6H2O) 1.426g, stirring 5h to presoma complete hydrolysis；
D), propylene oxide 1.76ml is added into the clear transparent solutions that step C) is obtained and stirs 20~30min；
E), the colloidal sol sealing that step D) is obtained is placed in gelation 48h in 40~60 DEG C of baking ovens；
F), block gel obtained by step E) is placed in 50~60 DEG C of baking ovens dry 48h；
G), block xerogel obtained by step F) is placed in inert atmosphere tube furnace, with the heating of 2.5 DEG C/min heating rate
To following 4 temperature spots: 400 DEG C, 600 DEG C, 800 DEG C or 1000 DEG C, keeping the temperature 100min, be made so that 4 kinds be made accordingly
Layer stephanoporate nickel cobalt (alloy)-carbon composite.
Embodiment 3, a kind of layer stephanoporate nickel cobalt (alloy)-carbon composite block material preparation method, are successively walked as follows
It is rapid:
A), weigh 1.2mL deionized water to be added in the glycerol of 2.4mL, magnetic agitation to solution is mixed thoroughly；
B), into liquid obtained by step A), the polyacrylic acid (50000) of 4.0g is added, it is complete to be stirred well to polyacrylic acid
Dispersing and dissolving；
C), presoma nickel source (NiCl is added into the uniform solution that step B) is obtained2·6H2O) 2.16g, nickel source
(NiCl2·6H2O) 0.713g, cobalt source (CoCl2·6H2O) 1.426g, cobalt source (CoCl2·6H2O) 2.16g stirs 5h to forerunner
Body complete hydrolysis；
D), propylene oxide 1.76ml is added into the clear transparent solutions that step C) is obtained and stirs 20~30min；
E), the colloidal sol sealing that step D) is obtained is placed in gelation 48h in 40~60 DEG C of baking ovens；
F), block gel obtained by step E) is placed in 50~60 DEG C of baking ovens dry 48h；
G), step F) gained block xerogel be placed in inert atmosphere tube furnace, be warming up to 2.5 DEG C/min heating rate
800 DEG C, 100min is kept the temperature, layer stephanoporate nickel cobalt (alloy)-carbon composite is made.
The above list is only a few specific embodiments of the present invention for finally, it should also be noted that.Obviously, this hair
Bright to be not limited to above embodiments, acceptable there are many deformations.Those skilled in the art can be from present disclosure
All deformations for directly exporting or associating, are considered as protection scope of the present invention.
Claims (5)
1. layer stephanoporate nickel cobalt (alloy)-carbon composite block material preparation method with electromagnetic wave absorption performance, feature exist
In including the following steps:
A), 1.0~4.0mL deionized water is weighed to be added in the glycerol of 1.0~3.0mL, magnetic agitation to be uniformly mixed；
B), the polyacrylic acid of 1.0~4.0g is added into liquid obtained by step A), be stirred well to polyacrylic acid be completely dispersed it is molten
Solution；
C), it is added into the uniform solution that step B) is obtained as 0.5~3g of nickel source of presoma, as the cobalt source of presoma
0.5~4.0g is hydrolyzed with stirring, and hydrolysis time is 3~5h；
D), 1.0~2.5ml of gel promotor is added into liquid obtained by step C) and stirs 20~30min；
E), the colloidal sol sealing that step D) is obtained is placed on 40~60 DEG C of 48 ± 2h of gelation；
F), the resulting block gel of step E) is placed in 50~60 DEG C of dry 48 ± 2h；
G), the resulting block xerogel of step F) is placed in inert atmosphere tube furnace, with 0.5~5 DEG C/min heating rate liter
Temperature keeps the temperature 100~300min to 400~1000 DEG C, and layer stephanoporate nickel cobalt (alloy)-carbon composite block material is made.
2. the preparation method of layer stephanoporate nickel cobalt (alloy)-carbon composite block material according to claim 1, feature exist
In: the molecular weight of polyacrylic acid used by step B) is 3000,5000,50000,10000.
3. the preparation method of layer stephanoporate nickel cobalt (alloy)-carbon composite block material according to claim 2, feature exist
In: nickel source step C) is NiCl2·6H2O、Ni(NO3)2·6H2O, cobalt source CoCl2·6H2O、Co(NO3)2·6H2O。
4. the preparation method of layer stephanoporate nickel cobalt (alloy)-carbon composite block material according to claim 3, feature exist
In: the gel promotor used in step D) is propylene oxide, propylene oxide, formamide.
5. the preparation method of layer stephanoporate nickel cobalt (alloy)-carbon composite block material according to claim 4, feature exist
In: in step D), gel promotor is added in the form being added dropwise, and the temperature of control system is no more than 60 DEG C during dropwise addition.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114920303A (en) * | 2022-04-30 | 2022-08-19 | 浙江大学杭州国际科创中心 | Iron-nickel hydroxide porous block material for hydrogen production by electrolyzing water and preparation method thereof |
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| CN114920303A (en) * | 2022-04-30 | 2022-08-19 | 浙江大学杭州国际科创中心 | Iron-nickel hydroxide porous block material for hydrogen production by electrolyzing water and preparation method thereof |
| CN114920303B (en) * | 2022-04-30 | 2024-02-27 | 浙江大学杭州国际科创中心 | Porous iron-nickel hydroxide block material for producing hydrogen by water electrolysis and preparation method thereof |
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