CN105883732A - Carbon nitride nanotube and preparation method thereof - Google Patents
Carbon nitride nanotube and preparation method thereof Download PDFInfo
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- CN105883732A CN105883732A CN201610219084.7A CN201610219084A CN105883732A CN 105883732 A CN105883732 A CN 105883732A CN 201610219084 A CN201610219084 A CN 201610219084A CN 105883732 A CN105883732 A CN 105883732A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
Abstract
The invention discloses a carbon nitride nanotube and a preparation method thereof. The component of the carbon nitride nanotube is carbon nitride represented by the chemical structural formula of C3N(4+/-x). According to the preparation method, a urea solution is prepared from urea and sodium bicarbonate in a mole ratio, then the solution is cooled to be frozen wholly, and uniform white blocky solids are obtained; the white blocky solids are transferred into a vacuum freeze dryer rapidly and subjected to freeze drying under the conditions of the vacuum lower than or equal to 20 Pa and the freezing temperature lower than or equal to subzero 50 DEG C, solids are obtained through calcination in a nitrogen atmosphere furnace, a yellowish powdery sample is obtained and subjected to dialysis and purification, and the yellowish carbon nitride nanotube is obtained. The method is effective, practical and simple, is applicable to preparation in a laboratory and industrial production and has broad development space and great application prospect.
Description
Technical field
The present invention relates to a kind of azotized carbon nano pipe and preparation method thereof, particularly relate to a kind of azotized carbon nano pipe and there is environment friend
The method that the simplicity that good low cost high yield high-performance can be mass prepares this azotized carbon nano pipe, belongs to field of nanometer material technology.
Background technology
Carbonitride (CN or C3N4) be made up of the two kinds of elemental carbons being widespread in nature and nitrogen, include highly stable
Triazine (Triazine) and three s-triazine (Tri-s-triazine) unit.Perfect carbon nitride material is that a kind of low energy gap is partly led
Body (band gap width is 2.7eV).Meanwhile, carbonitride has the much the most noticeable performance, the most heat-resisting resistance to chemical attack,
Biocompatibility wear-resistant, superhard, waterproof, that density is little, nontoxic, good, and there is the highest electron transfer rate and very
Strong oxidability, this makes carbonitride become a kind of very important functional material without metallic element, as photocatalyst quilt
It is widely used in the fields such as decomposition water, solar energy conversion, contaminant degradation.
Nanotube (Nanotube, NT) refers to that the yardstick in a certain respect of sample is being managed by one or more layers of nanometer (nm) level
The molecular tubular material of the coaxial high score of shape, is found to be the beginning with CNT.There are the most again boron nitride nano-tube, molybdenum sulfide
Nanotube, Sic nanotube, the nano-tube material such as titanium oxide nanotubes.Generally a length of micron (μm) level of nanotube,
And warp or outer through in nano-scale range in it；Also or its pipe thickness is in nano-scale range.Therefore, nanotube
Length/diameter is than very big, for the typical monodimension nanometer material of one.Owing to nanotube has the least size, and have
Bigger specific surface area, the most exclusive special tubular structure, thus it is endowed unusual physical and chemical performance, in sensing
Device, capacitor, thing fix, hydrogen storage, catalysis, battery electrode, before there are great researching value and application in the field such as photoelectricity
Scape.
Azotized carbon nano pipe (CNNT) possess carbon nitride material itself speciality (forbidden band is narrow, water dispersible good, anti-light radiation,
The excellent properties such as corrosion-resistant, biocompatibility), simultaneously because the special construction of its nanotube, be one have huge potential should
Valuable material.
The method preparing nanotube is generally divided into two big classes.One class method is direct synthesis technique, such as chemical method, arc process, changes
Learn vapour deposition process, ion beam irradiation method.Chuanbao Cao seminar1Chemical method is used to prepare the carbonitride of tubulose, sample
The specific surface area of product is relatively big and has higher ratio electric capacity and preferable photocatalysis performance.But the raw material of the method is for have biology
Highly basic used by the tripolycyanamide of evil and preparation process.Mukul Kumar seminar2Chemical gaseous phase is used to deposit and combine mould
Plate is successfully prepared the CNNT of long size, and have studied its field emission performance.K.Suenaga seminar3Propose a kind of magnetic
The method of control sputtering, and use the method to successfully synthesize CNNT.Another kind of method is template, such as, utilize oldered array
Prepare nanotube as template, utilize porous material to prepare nanotube etc. as template.Wei-Guo Song seminar4With porous
Aluminium oxide nano material is template, and polymerization ethylenediamine and carbon tetrachloride prepare CNNT.Prepared material list reveals preferably
Catalytic performance.H.-Jurgen Meyer seminar5Metathesis reaction is carried out for raw material with cyanuryl chloride and multiple solid phase nitrogen source,
And with intermediate product N (C3N3Cl2)3Under the special environment such as vacuum or argon, it is successfully prepared CNNT as template.
Although this two class can being used to prepare azotized carbon nano pipe, but existing method existing a lot of not enough: or preparation work
Sequence is complicated, and apparatus expensive, the production cycle is very long, and productivity is low, is not suitable for large-scale production；Or in raw material and preparation process
Use the material harmful to environment and health；Or the nanotube size of preparation is bad, performance is the best, is unfavorable for practicality.Therefore,
It is badly in need of the short-cut method that can produce nanotube in batches of a kind of environmental protection at present, and realizes and azotized carbon nano prepared by this method
Pipe yield is high, function admirable.
Summary of the invention
For at present potential demand to azotized carbon nano pipe, existing prepare problem present in nanotube method, and nitridation
The blank that CNT and preparation and application thereof exist, the present invention proposes a kind of azotized carbon nano pipe, and proposes a kind of environmental protection
, can produce in batches, the simplicity of good product performance prepares method and the application thereof of this azotized carbon nano pipe.
Azotized carbon nano pipe of the present invention, it is characterised in that: the composition of described azotized carbon nano pipe is chemical structural formula C3N(4±x)The carbonitride of statement, wherein x=0～1, the pattern of described azotized carbon nano pipe is long circular tube shape, its a length of 2-5 μm,
In it, warp is 100-500nm, and its external diameter is 120-600nm, and its wall thickness is 10-100nm.Carbonitride of the present invention is received
Mitron size is unified, is evenly distributed.Described azotized carbon nano pipe productivity, up to more than 60%, has the performance of excellence.
The preparation method of azotized carbon nano pipe of the present invention, step is:
(1) preparation solution: carbamide and sodium bicarbonate are dissolved in pure water with the ratio that mol ratio is 1～100:1,
It is sufficiently stirred for and mix homogeneously, makes the colourless transparent solution that urea concentration is 1～10mol/L；
(2) freezing: the colourless transparent solution that step (1) obtains is placed in low temperature environment freezing, cryogenic temperature be-20 DEG C～
-80 DEG C, cooling time is more than 24h, makes solution entirety freezing, obtains uniform white clumpy solid；
(3) it is dried: the white clumpy solid that step (2) prepares is transferred quickly in vacuum freeze dryer, in vacuum
≤ 20Pa, lyophilization under the conditions of cryogenic temperature≤-50 DEG C, sublimation drying is more than 20h, makes white clumpy solid cold
Lyophilizing is dry to constant weight；
(4) calcining: the white clumpy solid that step (3) prepares is positioned in crucible with cover, and is placed on nitrogen atmosphere stove
In, the calcining heat of 400～700 DEG C it is warming up to the programming rate of 1～20 DEG C/min, calcination time is 1～5h, wherein nitrogen
Gas velocity is 1～10ml/min；Then lower the temperature with stove, obtain pale yellow powder sample；
(5) purify: the sample full and uniform dispersion that step (4) prepares is obtained faint yellow settled solution in pure water；
Then standing faint yellow settled solution, time of repose is more than 12h；Remove supernatant after standing, take off layer turbid solution with retaining
Molecular weight is the bag filter dialysis of 1～10kD, and dialysis time is 1～3 day, removes sodium ion and other by-product and impurity；
Sample after purifying is dried, i.e. obtains flaxen azotized carbon nano pipe.
In the preparation method of above-mentioned azotized carbon nano pipe: described carbamide is general industry carbamide, the most pure powder, more
The preferably crystalline powder of the non-deliquescence of high-purity；Described sodium bicarbonate is general industry sodium bicarbonate, the most pure powder,
The most high-purity crystallized powder；The described preferred pure water of free from admixture water or distilled water, more preferably deionized water；Described nitrogen is
Industrial nitrogen, preferably high pure nitrogen.
In the preparation method of above-mentioned azotized carbon nano pipe:
Step (1) described carbamide and sodium bicarbonate mol ratio are preferably 5～50:1, more preferably 10:1；Described urea concentration
It is preferably 3～6mol/L, more preferably 4mol/L；
Step (2) described cryogenic temperature and cooling time determine according to the number of amount of solution, make solution be frozen into entirety, excellent
Electing cryogenic temperature as and be-40 DEG C～-60 DEG C, preferably cooling time is 30～50h；
Vacuum described in step (3) is the highest more is conducive to the quick of product to prepare, and described cryogenic temperature is the lowest more is conducive to producing
The efficient preparation of product, but consider from working condition and overall efficiency angle, preferred 8Pa～10Pa of vacuum, cryogenic temperature is preferred
-80 DEG C～-70 DEG C, described drying time determines according to the number of block total amount, make solid lyophilization to constant weight, preferably
48h；
Calcining heat described in step (4) is preferably 500 DEG C～600 DEG C, and more preferably 550 DEG C, temperature retention time is preferably 2～4
H, more preferably 3h, programming rate is preferably 5～15 DEG C/min, more preferably 10 DEG C/min, and nitrogen flow rate is preferably 3～7
Ml/min, more preferably 5ml/min；
Time of repose described in step (5) is preferably 20h, and the preferably molecular cut off of bag filter is 3kD, when preferably dialysing
Between be 2 days.
The present invention proposes a kind of azotized carbon nano pipe and has what eco-friendly low cost high yield high-performance can be mass
Easy method prepare this azotized carbon nano pipe, it implements to have and highlights effect as follows:
1. the raw material used by the present invention is industrial urea and industrial sodium bicarbonate, and auxiliary material is industrial nitrogen and free from admixture water,
Material source is extensive, simple and easy to get, with low cost, and nontoxic pollution-free, does not works the mischief environment and biology health, is
Environment friendly material；
Preparation method the most involved in the present invention is simple, with short production cycle, can set technique flexibly according to working condition and benefit
Parameter, is not related to any poisonous and harmful additive and by-product in process of production, is the production technology of environmental protection；
3. simple due to preparation method of the present invention, do not limit single and prepare the production scale of azotized carbon nano pipe, simultaneously productivity
It is high up to more than 60%, so the present invention may be used for high-volume pipeline system and produces azotized carbon nano pipe；
4. the azotized carbon nano pipe produced by the present invention, size can regulate within the specific limits, and size is unified, is evenly distributed,
There is the performance of excellence, sensor can be met, capacitor, thing fix, hydrogen storage, catalysis, battery electrode, the field such as photoelectricity
Or the demand of industry, there is great researching value and application prospect.
In a word, the method preparing azotized carbon nano pipe that can produce in batches of environmental protection disclosed by the invention is a kind of effective practicality
Straightforward procedure, is suitable for laboratory preparation and industrialized production, has wide development space.Prepared azotized carbon nano pipe
Can be excellent, there is huge application prospect.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) photo of the azotized carbon nano pipe prepared by embodiment 1.
Fig. 2 is transmission electron microscope (TEM) photo of the azotized carbon nano pipe prepared by embodiment 3.
Fig. 3 is technique (embodiment 4) flow chart that azotized carbon nano pipe is prepared in a typical industrialization.
Detailed description of the invention
Embodiment 1:
(1) preparation solution: carbamide and the sodium bicarbonate ratio with mol ratio as 40:1 are dissolved in 100mL deionized water,
It is sufficiently stirred for and mix homogeneously, makes the colourless transparent solution that urea concentration is 6mol/L；
It is (2) freezing: the colourless transparent solution that step (1) obtains is placed in low temperature environment freezing, and cryogenic temperature is-80 DEG C,
Cooling time is 30h, makes solution entirety freezing, obtains uniform white clumpy solid；
(3) it is dried: the white clumpy solid that step (2) prepares is transferred quickly in vacuum freeze dryer, in vacuum
≤ 20Pa, lyophilization under the conditions of cryogenic temperature-80 DEG C, sublimation drying is 48h, makes white clumpy solid lyophilization
To constant weight；
(4) calcining: the white clumpy solid that step (3) prepares is positioned in crucible with cover, and is placed on nitrogen atmosphere stove
In, the calcining heat of 500 DEG C it is warming up to the programming rate of 5 DEG C/min, calcination time is 4h, and wherein nitrogen flow rate is 7
ml/min；Then lower the temperature with stove, obtain pale yellow powder sample；
(5) purify: the sample full and uniform dispersion that step (4) prepares is obtained faint yellow settled solution in pure water；
Then faint yellow settled solution, time of repose 20h are stood；Remove supernatant after standing, take off layer turbid solution with retaining molecule
The bag filter dialysis that amount is 10kD, dialysis time is 1 day, removes sodium ion and other by-product and impurity；After purifying
Sample be dried, i.e. obtain flaxen azotized carbon nano pipe.
By transmission electron microscope (TEM) result of the azotized carbon nano pipe prepared by embodiment 1 as shown in Figure 1.
Embodiment 2:
(1) preparation solution: carbamide and the sodium bicarbonate ratio with mol ratio as 5:1 are dissolved in 50mL deionized water,
It is sufficiently stirred for and mix homogeneously, makes the colourless transparent solution that urea concentration is 3mol/L；
It is (2) freezing: the colourless transparent solution that step (1) obtains is placed in low temperature environment freezing, and cryogenic temperature is-80 DEG C,
Cooling time is 30h, makes solution entirety freezing, obtains uniform white clumpy solid；
(3) it is dried: the white clumpy solid that step (2) prepares is transferred quickly in vacuum freeze dryer, in vacuum
≤ 20Pa, lyophilization under the conditions of cryogenic temperature-70 DEG C, sublimation drying is 48h, makes white clumpy solid lyophilization
To constant weight；
(4) calcining: the white clumpy solid that step (3) prepares is positioned in crucible with cover, and is placed on nitrogen atmosphere stove
In, the calcining heat of 600 DEG C it is warming up to the programming rate of 15 DEG C/min, calcination time is 2h, and wherein nitrogen flow rate is 7
ml/min；Then lower the temperature with stove, obtain pale yellow powder sample；
(5) purify: the sample full and uniform dispersion that step (4) prepares is obtained faint yellow settled solution in pure water；
Then faint yellow settled solution, time of repose 24h are stood；Remove supernatant after standing, take off layer turbid solution with retaining molecule
The bag filter dialysis that amount is 1kD, dialysis time is 3 days, removes sodium ion and other by-product and impurity；After purifying
Sample is dried, and i.e. obtains flaxen azotized carbon nano pipe.
Embodiment 3:
(1) preparation solution: carbamide and the sodium bicarbonate ratio with mol ratio as 10:1 are dissolved in 100mL deionized water,
It is sufficiently stirred for and mix homogeneously, makes the colourless transparent solution that urea concentration is 4mol/L；
It is (2) freezing: the colourless transparent solution that step (1) obtains is placed in low temperature environment freezing, and cryogenic temperature is-80 DEG C,
Cooling time is 24h, makes solution entirety freezing, obtains uniform white clumpy solid；
(3) it is dried: being transferred quickly in vacuum freeze dryer by the white clumpy solid that step (2) prepares, vacuum sets
For 8Pa, lyophilization under the conditions of cryogenic temperature-80 DEG C, sublimation drying is 48h, makes white clumpy solid freezing do
Dry to constant weight；
(4) calcining: the white clumpy solid that step (3) prepares is positioned in crucible with cover, and is placed on nitrogen atmosphere stove
In, the calcining heat of 550 DEG C it is warming up to the programming rate of 10 DEG C/min, calcination time is 3h, and wherein nitrogen flow rate is 7
ml/min；Then lower the temperature with stove, obtain pale yellow powder sample；
(5) purify: the sample full and uniform dispersion that step (4) prepares is obtained faint yellow settled solution in pure water；
Then faint yellow settled solution, time of repose 12h are stood；Remove supernatant after standing, take off layer turbid solution with retaining molecule
The bag filter dialysis that amount is 3kD, dialysis time is 2 days, removes sodium ion and other by-product and impurity；After purifying
Sample is dried, and i.e. obtains flaxen azotized carbon nano pipe.
By transmission electron microscope (TEM) result of the azotized carbon nano pipe prepared by embodiment 3 as shown in Figure 2.
Embodiment 4:
A kind of embodiment being more beneficial for industrialization production azotized carbon nano pipe:
(1) preparation solution: carbamide and the sodium bicarbonate ratio with mol ratio as 10:1 are dissolved in 1 ton of pure water, fill
Divide stirring mix homogeneously, make the colourless transparent solution that urea concentration is 4mol/L；
(2) freezing: the colourless transparent solution that step (1) obtains is placed in low temperature environment freezing.
For improving refrigerating effect, save cooling time, 1 ton of homogeneous solution can be dispensed in some bottles of same containers；Have large-scale
Sample can be placed in-80 DEG C of environment freezing standing 30h together during container；Only during small containers, can successively sample be turned
Move on to freezing standing 30h in-80 DEG C of environment, make every bottle of solution IQF become an entirety, obtain uniform white chunks solid
Body；
(3) it is dried: the white clumpy solid that step (2) prepares is transferred quickly in vacuum freeze dryer, in vacuum
For 20Pa, lyophilization under the conditions of cryogenic temperature-50 DEG C, sublimation drying is 48-60h, makes white clumpy solid freezing
It is dried to constant weight；
(4) calcining: the white clumpy solid that step (3) prepares is positioned in crucible with cover, and is placed on nitrogen atmosphere stove
In, the calcining heat of 550 DEG C it is warming up to the programming rate of 10 DEG C/min, calcination time is 3h, and wherein nitrogen flow rate is 7
ml/min；Then lower the temperature with stove, obtain pale yellow powder sample；
(5) purify: the sample full and uniform dispersion that step (4) prepares is obtained faint yellow settled solution in deionized water；
Then faint yellow settled solution, time of repose 20h are stood；Remove supernatant after standing, take off layer turbid solution with retaining molecule
The bag filter dialysis that amount is 3kD, dialysis time is 3 days, removes sodium ion and other by-product and impurity；After purifying
Sample is dried, and i.e. obtains flaxen azotized carbon nano pipe.
The flow chart of above-mentioned whole preparation process is as shown in Figure 3.
JEM 2100 type transmission electron microscope is produced to the nitrogen prepared by embodiment 1 and embodiment 3 with JEOL company of Japan
Carbon nano tube is observed.Nanotube length prepared by embodiment 1 (see Fig. 1) is about 1.5 μm, and interior warp is about 150nm,
External diameter is about 200nm；Nanotube prepared by embodiment 3 (see Fig. 2), length is about 1 μm, and interior warp is about 200nm,
External diameter is about 220nm.Thus result understands, and can be realized nitridation by the ratio of carbamide and sodium bicarbonate in regulation raw material
The regulation and control of carbon nanotube sizes.
Claims (7)
1. an azotized carbon nano pipe, it is characterised in that: the composition of described azotized carbon nano pipe is chemical structural formula C3N(4 ± x)The carbonitride of statement, wherein x=0～1, the pattern of described azotized carbon nano pipe is long circular tube shape, its a length of 2-5 μm, and in it, warp is 100-500nm, and its external diameter is 120-600nm, and its wall thickness is 10-100nm.
2. the preparation method of the azotized carbon nano pipe described in claim 1, step is:
(1) preparation solution: carbamide and sodium bicarbonate are dissolved in pure water with the ratio that mol ratio is 1～100:1, is sufficiently stirred for and mix homogeneously, makes the colourless transparent solution that urea concentration is 1～10mol/L；
(2) freezing: the colourless transparent solution that step (1) obtains is placed in low temperature environment freezing, and cryogenic temperature is-20 DEG C～-80 DEG C, and cooling time is more than 24h, make solution entirety freezing, obtain uniform white clumpy solid；
(3) it is dried: the white clumpy solid that step (2) prepares is transferred quickly in vacuum freeze dryer, at vacuum≤20Pa, lyophilization under the conditions of cryogenic temperature≤-50 DEG C, sublimation drying is more than 20h, makes white clumpy solid lyophilization to constant weight；
(4) calcining: the white clumpy solid that step (3) prepares is positioned in crucible with cover, and be placed in nitrogen atmosphere stove, the calcining heat of 400～700 DEG C it is warming up to the programming rate of 1～20 DEG C/min, calcination time is 1～5h, and wherein nitrogen flow rate is 1～10ml/min；Then lower the temperature with stove, obtain pale yellow powder sample；
(5) purify: the sample full and uniform dispersion that step (4) prepares is obtained faint yellow settled solution in pure water；Then standing faint yellow settled solution, time of repose is more than 12h；Removing supernatant after standing, take off the bag filter dialysis that layer turbid solution molecular cut off is 1～10kD, dialysis time is 1～3 day, removes sodium ion and other by-product and impurity；Sample after purifying is dried, i.e. obtains flaxen azotized carbon nano pipe.
The preparation method of azotized carbon nano pipe described in 2 the most as requested, it is characterised in that: step (1) described carbamide is high-purity carbamide, or for general industry carbamide；Described sodium bicarbonate is high-purity sodium bicarbonate, or for general industry sodium bicarbonate；Described free from admixture water is pure water or distilled water；Described carbamide is 5～50:1 with the mol ratio of sodium bicarbonate；Described urea concentration is 3～6mol/L.
The preparation method of azotized carbon nano pipe described in 2 the most as requested, it is characterised in that: step (2) described cryogenic temperature is-40 DEG C～-60 DEG C；Described cooling time is 30～50h.
The preparation method of azotized carbon nano pipe described in 2 the most as requested, it is characterised in that: step (3) described vacuum is 8～10Pa；Described cryogenic temperature is-80 DEG C～-70 DEG C；Described sublimation drying is 48h.
The preparation method of azotized carbon nano pipe described in 2 the most as requested, it is characterised in that: step (4) described nitrogen is high pure nitrogen, or for general industry nitrogen；Described programming rate is 5～15 DEG C/min；Described calcining heat is 500 DEG C～600 DEG C；Described temperature retention time is 2～4h；Described nitrogen flow rate is 3～7ml/min.
The preparation method of azotized carbon nano pipe described in 2 the most as requested, it is characterised in that: step (5) described free from admixture water is pure water or distilled water；Described time of repose is 20h, and the molecular cut off of described bag filter is 3kD, and described dialysis time is 2 days.
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| CN108383091A (en) * | 2017-12-28 | 2018-08-10 | 济南大学 | A kind of g-C3N4 tube-in-tubes and preparation method thereof of S, P doping |
| CN108772092A (en) * | 2018-06-06 | 2018-11-09 | 合肥学院 | A kind of Ag3PO4/g-C3N4 composite tubes nano-powder and preparation method thereof |
| WO2022109960A1 (en) * | 2020-11-26 | 2022-06-02 | 苏州大学 | Three-dimensional carbon nanotube cluster and method for preparation thereof and application thereof |
| CN115246633A (en) * | 2021-12-10 | 2022-10-28 | 浙江师范大学 | Hollow structure g-C 3 N 4 Material, preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107022809A (en) * | 2017-03-28 | 2017-08-08 | 哈尔滨工程大学 | A kind of preparation method of pervasive overlength lithium fluoride fiber |
| CN107022809B (en) * | 2017-03-28 | 2019-07-16 | 哈尔滨工程大学 | A kind of preparation method of pervasive overlength lithium fluoride fiber |
| CN108383091A (en) * | 2017-12-28 | 2018-08-10 | 济南大学 | A kind of g-C3N4 tube-in-tubes and preparation method thereof of S, P doping |
| CN108772092A (en) * | 2018-06-06 | 2018-11-09 | 合肥学院 | A kind of Ag3PO4/g-C3N4 composite tubes nano-powder and preparation method thereof |
| CN108772092B (en) * | 2018-06-06 | 2020-08-25 | 合肥学院 | Ag3PO4/g-C3N4 composite tubular nano powder and preparation method thereof |
| WO2022109960A1 (en) * | 2020-11-26 | 2022-06-02 | 苏州大学 | Three-dimensional carbon nanotube cluster and method for preparation thereof and application thereof |
| CN115246633A (en) * | 2021-12-10 | 2022-10-28 | 浙江师范大学 | Hollow structure g-C 3 N 4 Material, preparation method and application thereof |
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