CN110155985A - A kind of preparation method of high orientation flaky carbon nanomaterials - Google Patents
A kind of preparation method of high orientation flaky carbon nanomaterials Download PDFInfo
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- CN110155985A CN110155985A CN201910524005.7A CN201910524005A CN110155985A CN 110155985 A CN110155985 A CN 110155985A CN 201910524005 A CN201910524005 A CN 201910524005A CN 110155985 A CN110155985 A CN 110155985A
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- cellulose nanocrystal
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- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
A kind of method that the present invention discloses low temperature preparation high orientation flaky carbon nanomaterials, belongs to carbon material field.The preparation method of the high orientation flaky carbon nanomaterials, it is that Cellulose nanocrystal colloid is evenly dispersed, the self assembly direction of crystal in static several weeks control Cellulose nanocrystal, then the growth using ice crystal in vacuum freeze drying control Cellulose nanocrystal and distillation direction, obtain Cellulose nanocrystal flaky material.Further starvation carries out pyrolysis carbonization to product at 600~1000 DEG C, removes hydrogen, oxygen element in Cellulose nanocrystal molecular structure, and the carbon nanomaterial of highly crystalline is prepared, and yield is 28%~35%.The material has high-graphitized structure, and piece interlamellar spacing is 0.388~0.408nm, and crystallinity is 77.7%~92.8%.Conductive material is made in the material, conductivity is 0.043~6.2S/m.This method preparation manipulation is simple, energy saving.
Description
Technical field
The present invention relates to carbon material fields, and in particular to a kind of side of low temperature preparation high orientation flaky carbon nanomaterials
Method.
Background technique
Two-dimentional carbon nanomaterial such as graphene, carbon nanosheet, carbon nanocapsule thin film etc. has big lateral dimension, ultra-thin
Thickness, excellent conductivity and high chemical stability, can be widely applied to catalysis, energy stores, electronics etc..Current two
The common preparation method of dimension carbon nanomaterial has chemical vapour deposition technique, template, stripping method etc..Wherein, before being with polymer
Body has big production scale, broad applicability and economic benefit height etc. excellent by the method that pyrolysis prepares two-dimentional carbon nanomaterial
Point.Cellulose is a kind of common carbon precursor as a kind of natural polymer, usually in 400 DEG C or more starvation pyrolysis systems
Obtain biomass carbon.Since its carbon yield is lower (yield is 17%~19% within the scope of 550~850 DEG C), mechanical performance is poor, and
It is hardly formed carbonization structure at 1000 DEG C or less, the application requirement for making it be difficult to meet New Two Dimensional carbon nanomaterial.
Nano-cellulose (nanocellulose) be diameter be 1~100nm, length be tens nanometers to several microns surpass
The general designation of microfibre.Currently, according to the size and form of preparation, nano-cellulose can be divided into Cellulose nanocrystal and fiber
Plain nanofibrils.Wherein, Cellulose nanocrystal (Cellulose nanocrystal, CNC) is cellulose by processing (such as acid
Hydrolysis), after the crystal region of amorphous region and low-crystallinity in cellulose is abolished, a kind of rigid rod fiber for extracting
Plain crystalline solid, 2~20nm of diameter, 100~500nm of length.CNC has high-crystallinity, high-modulus (130~250GPa), height
Specific surface area (150-1000m2/ g) etc. characteristics, be expected to be applied to the preparation of two-dimentional carbon nanomaterial.
Summary of the invention
The purpose of the present invention: a kind of preparation method of high orientation flaky carbon nanomaterials is provided.
Technical solution of the invention: Cellulose nanocrystal colloid is evenly dispersed, and static several weeks control cellulose is received
The self assembly direction of meter Jing Zhong crystal, then using the growth and distillation of ice crystal in vacuum freeze drying control Cellulose nanocrystal
Direction obtains Cellulose nanocrystal flaky material.Further starvation carries out pyrolysis carbonization to product at a certain temperature,
Hydrogen, the oxygen element in Cellulose nanocrystal molecular structure are removed, the carbon nanomaterial of highly crystalline is prepared.
It is specific the preparation method is as follows:
(1) in mass ratio 1.0~2.0: 100 Cellulose nanocrystal, deionized water are weighed, be sufficiently mixed, in ice-water bath
Ultrasonic disperse is carried out, the Cellulose nanocrystal colloid that mass fraction is 1.0~2.0% is obtained；
(2) the Cellulose nanocrystal colloid for obtaining step (1) is placed 1~2 week at 4~10 DEG C, obtains high orientation
Cellulose nanocrystal colloid；
(3) the Cellulose nanocrystal colloid of step (2) freezes to 12 at -40~-25 DEG C~for 24 hours, it is dry to be put into vacuum refrigeration
Dry 24~the 48h of dry machine, obtains Cellulose nanocrystal flaky material；
(4) the Cellulose nanocrystal flaky material for obtaining step (3), is placed in tube furnace, keeps at 600~1000 DEG C
Flaky carbon nanomaterials are made in 2~4h.
Advantages of the present invention:
Cellulose nanocrystal has the crystallinity of height, makes it that melt-flow not occur when being pyrolyzed carbonization, can still keep
Its pattern and structure, in addition, the cellulose molecular chain of proper alignment form it can at low temperature in Cellulose nanocrystal
The carbonization structure orderly oriented.This method prepares that flaky carbon nanomaterials are easy to operate, energy saving.Performance test shows:
The freeze-dried combination low temperature pyrogenation carbonization treatment of CNC has been made flaky carbon nanomaterials, and yield is 28%~
35%, the material have high-graphitized structure, piece interlamellar spacing be 0.388~0.408nm, crystallinity be 77.7%~
92.8%.Conductive material is made in the material, after tested, conductivity is 0.043~6.3S/m.
Detailed description of the invention
Attached drawing 1 is the SEM figure of the flaky carbon nanomaterials of embodiment 2.
Attached drawing 2 is the HR-TEM figure of the flaky carbon nanomaterials of embodiment 2.
Specific embodiment
Embodiment 1,
(1) in mass ratio 1.0: 100 Cellulose nanocrystal, deionized water are weighed, is sufficiently mixed, is surpassed in ice-water bath
Sound dispersion obtains the Cellulose nanocrystal colloid that mass fraction is 1.0%；
(2) the Cellulose nanocrystal colloid for obtaining step (1) is placed 1~2 week at 4~10 DEG C, obtains high orientation
Cellulose nanocrystal colloid；
(3) the Cellulose nanocrystal colloid of step (2) freezes to 12 at -40~-25 DEG C~for 24 hours, it is dry to be put into vacuum refrigeration
Dry 24~the 48h of dry machine, obtains Cellulose nanocrystal flaky material；
(4) the Cellulose nanocrystal flaky material for obtaining step (3), is placed in tube furnace, keeps at 600~1000 DEG C
Flaky carbon nanomaterials are made in 2~4h.
Performance test shows: the yield of flaky carbon nanomaterials is 28%, and piece interlamellar spacing is 0.388nm, and crystallinity is
77.7%.After conductive material is made in the material, conductivity 0.043S/m.
Embodiment 2,
(1) in mass ratio 1.8: 100 Cellulose nanocrystal, deionized water are weighed, is sufficiently mixed, is surpassed in ice-water bath
Sound dispersion obtains the Cellulose nanocrystal colloid that mass fraction is 1.8%；
(2) the Cellulose nanocrystal colloid for obtaining step (1) is placed 1~2 week at 4~10 DEG C, obtains high orientation
Cellulose nanocrystal colloid；
(3) the Cellulose nanocrystal colloid of step (2) freezes to 12 at -40~-25 DEG C~for 24 hours, it is dry to be put into vacuum refrigeration
Dry 24~the 48h of dry machine, obtains Cellulose nanocrystal flaky material；
(4) the Cellulose nanocrystal flaky material for obtaining step (3), is placed in tube furnace, keeps at 600~1000 DEG C
Flaky carbon nanomaterials are made in 2~4h.
Performance test shows: the yield of flaky carbon nanomaterials is 30%, and piece interlamellar spacing is 0.402nm, and crystallinity is
85.5%.After conductive material is made in the material, conductivity 5.2S/m.
Embodiment 3,
(1) in mass ratio 2.0: 100 Cellulose nanocrystal, deionized water are weighed, is sufficiently mixed, is surpassed in ice-water bath
Sound dispersion obtains the Cellulose nanocrystal colloid that mass fraction is 2.0%；
(2) the Cellulose nanocrystal colloid for obtaining step (1) is placed 1~2 week at 4~10 DEG C, obtains high orientation
Cellulose nanocrystal colloid；
(3) the Cellulose nanocrystal colloid of step (2) freezes to 12 at -40~-25 DEG C~for 24 hours, it is dry to be put into vacuum refrigeration
Dry 24~the 48h of dry machine, obtains Cellulose nanocrystal flaky material；
(4) the Cellulose nanocrystal flaky material for obtaining step (3), is placed in tube furnace, keeps at 600~1000 DEG C
Flaky carbon nanomaterials are made in 2~4h.
Performance test shows: the yield of flaky carbon nanomaterials is 35%, and piece interlamellar spacing is 0.408nm, and crystallinity is
92.8%.After conductive material is made in the material, conductivity 6.3S/m.
Claims (2)
1. a kind of preparation method of high orientation flaky carbon nanomaterials, it is characterised in that be made as follows:
(1) in mass ratio 1.0~2.0: 100 Cellulose nanocrystal, deionized water are weighed, be sufficiently mixed, carried out in ice-water bath
Ultrasonic disperse obtains the Cellulose nanocrystal colloid that mass fraction is 1.0~2.0%；
(2) the Cellulose nanocrystal colloid for obtaining step (1) is placed 1~2 week at 4~10 DEG C, obtains the fiber of high orientation
Plain nanocrystalline colloid；
(3) the highly oriented fibre element nanocrystalline colloid for obtaining step (2) freeze 12 at -40~-25 DEG C~for 24 hours, be put into true
Vacuum freecing-dry machine dries 24~48h, obtains Cellulose nanocrystal flaky material；
(4) the Cellulose nanocrystal flaky material for obtaining step (3), is placed in tube furnace, starvation, 600~1000
DEG C keep 2~4h, be made high orientation flaky carbon nanomaterials.
2. a kind of preparation method of high orientation flaky carbon nanomaterials according to claim 1, it is characterised in that described
10~20nm of Cellulose nanocrystal diameter, 200~400nm of length.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113248958A (en) * | 2021-06-16 | 2021-08-13 | 廊坊中电熊猫晶体科技有限公司 | Heat dissipation electrostatic adsorption powder and preparation method thereof |
| CN113522315A (en) * | 2021-08-26 | 2021-10-22 | 南京林业大学 | Sulfur-doped carbon nanosheet and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587006A (en) * | 2016-11-18 | 2017-04-26 | 浙江理工大学 | Method for preparing carbon nano bar based on cellulose nanocrystals |
| CN108043399A (en) * | 2017-12-13 | 2018-05-18 | 南京林业大学 | A kind of method that nanocrystalline cellulose template prepares photochemical catalyst |
-
2019
- 2019-06-17 CN CN201910524005.7A patent/CN110155985A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587006A (en) * | 2016-11-18 | 2017-04-26 | 浙江理工大学 | Method for preparing carbon nano bar based on cellulose nanocrystals |
| CN108043399A (en) * | 2017-12-13 | 2018-05-18 | 南京林业大学 | A kind of method that nanocrystalline cellulose template prepares photochemical catalyst |
Non-Patent Citations (4)
| Title |
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| HONGLI ZHU等: "Low temperature carbonization of cellulose nanocrystals for high performance carbon anode of sodium-ion batteries", 《NANO ENERGY》 * |
| JIA DING等: "Exceptional energy and new insight with a sodium–selenium battery based on a carbon nanosheet cathode and a pseudographite anode", 《ENERGY & ENVIRONMENTAL SCIENCE》 * |
| SEULBEE LEE等: "Morphologies and surface properties of cellulose-based activated carbon nanoplates", 《CARBON LETTERS》 * |
| 赵国敏等: "CNC基手性向列液晶衍生材料制备及应用研究进展", 《高分子通报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113248958A (en) * | 2021-06-16 | 2021-08-13 | 廊坊中电熊猫晶体科技有限公司 | Heat dissipation electrostatic adsorption powder and preparation method thereof |
| CN113522315A (en) * | 2021-08-26 | 2021-10-22 | 南京林业大学 | Sulfur-doped carbon nanosheet and preparation method and application thereof |
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Application publication date: 20190823 |