CN102126709A - Preparation method of boron nitride one-dimensional nanostructure macroscopic rope - Google Patents
Preparation method of boron nitride one-dimensional nanostructure macroscopic rope Download PDFInfo
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 75
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 57
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 20
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052810 boron oxide Inorganic materials 0.000 claims abstract description 17
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012018 catalyst precursor Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000012159 carrier gas Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 7
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 5
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 5
- MTKRXXSLFWZJTB-UHFFFAOYSA-N oxo(oxoboranyl)borane Chemical compound O=BB=O MTKRXXSLFWZJTB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract 3
- 239000002071 nanotube Substances 0.000 claims description 10
- 239000000376 reactant Substances 0.000 claims description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 239000002121 nanofiber Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- 239000002243 precursor Substances 0.000 abstract description 5
- 238000001338 self-assembly Methods 0.000 abstract description 4
- 230000001737 promoting effect Effects 0.000 abstract 2
- 229910052796 boron Inorganic materials 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000000835 fiber Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention relates to the field of boron nitride one-dimensional nanostructures, in particular to a preparation method of an oriented boron nitride one-dimensional nanostructure macroscopic rope. The method comprises the following steps of: volatilizing ferrocene serving as a floating catalyst precursor in a low-temperature region, carrying the volatilized precursor into a high-temperature region by using carrier gas so as to be decomposed into a metal catalyst, and promoting the reaction of diboron dioxide steam generated by the reaction of boron power in the high-temperature region with boron oxide with a nitrogen source by taking Fe2O3, FeS and ZnS as reaction promoting agents to generate a boron nitride one-dimensional nanostructure; stabilizing air stream by using a reaction casing in a reaction furnace to make the generated boron nitride one-dimensional nanostructure form a loose macroscopic rope structure through self-assembly; and fully soaking the loose macroscopic rope structure in an ethanol solution and assembling a dense boron nitride one-dimensional nanostructure macroscopic rope by using a boron nitride oriented nanostructure under the action of the surface tension of an ethanol-atmospheric air liquid surface. By adopting the method, damage to the structure by subsequent treatment assembly, molding and the like is avoided, and the excellent intrinsic properties of the boron nitride one-dimensional nanostructure are kept.
Description
The technical field is as follows:
the invention relates to the field of boron nitride one-dimensional nanostructures, in particular to a preparation method of a macroscopic rope with a directional boron nitride nanostructure.
Background art:
the boron nitride one-dimensional nanostructure is a wide band gap semiconductor, and has excellent performance and wide application prospect. Because of the strong covalent bond combination, the carbon nano tube has the same mechanical property as the carbon nano tube, and simultaneously, because of the high chemical stability and the oxidation resistance, the carbon nano tube can be used as mechanical enhancement and the like under the harsh conditions of high temperature, oxidizing atmosphere and the like. Since the first discovery in 1995, various methods have been developed to prepare boron nitride nanostructures, such as arc method, laser sputtering method, chemical vapor deposition and solid phase reaction method. Among them, the chemical vapor deposition method is widely used because of its advantages such as low cost, good controllability and easy amplification. By using the method, the high-purity and large-scale preparation of the boron nitride nanotube is realized.
In practical application, how to realize the connection and assembly of the boron nitride one-dimensional nanostructure needs to be assembled into a macroscopic material, and the excellent performance of the nanostructure is shown after the macroscopic material is formed, which is a key point and a difficulty in the current research.
The invention content is as follows:
the invention aims to provide a preparation method of a boron nitride one-dimensional nano-structure macroscopic rope, which realizes the connection and assembly of the boron nitride one-dimensional nano-structure and shows the excellent performance of the nano-structure after a macroscopic material is formed.
The technical scheme of the invention is as follows:
a method for preparing a macroscopic rope with a boron nitride one-dimensional nano structure adopts a horizontal chemical vapor deposition tube type reaction furnace, takes ferrocene as a floating catalyst precursor, volatilizes the floating catalyst precursor in a low-temperature region and is carried by a carrier gas to a high-temperature region to be decomposed into a metal catalyst, and promotes boron powder and boron oxide (B) in the high-temperature region2O3) Diboron dioxide (B) formed by the reaction2O2) The steam reacts with the nitrogen source to generate the boron nitride one-dimensional nanostructure. Meanwhile, the reaction sleeve in the reaction furnace has the function of stabilizing the airflow, so that the generated boron nitride one-dimensional nano structure is self-assembled to form a loose macroscopic rope-shaped structure.
Wherein:
the weight ratio of the boron powder to the boron oxide is 1: 1-1: 7.
The reaction temperature in the low temperature region is 100-.
The weight ratio of the floating catalyst precursor to the sum of the reactant boron powder and boron oxide is (0.5-2) to 1.
The flow ratio of the carrier gas to the nitrogen source is 0.25-6: 1, and the gas flow of the nitrogen source is 10-200 ml/min.
B2O2Keeping the temperature of the steam and the nitrogen source at the reaction temperature for 60-180 minutes, wherein the reaction promoter is Fe2O3FeS and ZnS, Fe2O3The weight ratio of FeS to ZnS is 2: 1: 2, and the weight ratio of the reaction accelerator to the sum of the reactant boron powder and boron oxide is 0.25-0.5: 1.
The boron nitride one-dimensional nanostructure may be a boron nitride nanotube or a boron nitride nanofiber. Wherein,
under the condition that the using amount of the floating catalyst precursor is small (0.1-0.5 part by weight, not 0.5 part by weight), a boron nitride nanotube can be obtained, wherein the inner diameter of the boron nitride nanotube is 20-40 nm, and the wall thickness is 5-10 nm;
under the condition that the using amount of the floating catalyst precursor is large (0.5-1 part by weight), the boron nitride nano-fiber can be obtained, and the diameter of the boron nitride nano-fiber is about 100-200 nm.
In addition, the prepared boron nitride one-dimensional nanostructure is soaked in an ethanol solution for one hour, fully soaked and then slightly lifted by using tweezers. Due to the action of surface tension of the ethanol-atmosphere liquid surface, the loose boron nitride structure becomes compact, and the original high directional arrangement is kept, so that the compact boron nitride one-dimensional nano-structure macroscopic rope is operated and assembled through a gas-liquid interface. The length of the macroscopic rope can reach 0.5-5 cm, and the diameter of the macroscopic rope can reach 1 mu m to 1 mm.
The invention has the beneficial effects that:
1. the invention provides a self-assembly preparation method of a macroscopic rope of a boron nitride one-dimensional nano structure, namely, the macroscopic rope-shaped boron nitride structure with the length of centimeter grade is formed by self-assembly in situ in the preparation process, so that the damage to the structure caused by subsequent treatment, assembly, forming and the like is avoided, and the excellent intrinsic performance of the boron nitride one-dimensional nano structure is maintained.
2. On the basis of self-assembly synthesis, the boron nitride fiber with compact structure is prepared by gas-liquid interface assembly.
3. The invention lays a foundation for the application of the boron nitride nano structure in the structure reinforced composite material.
Description of the drawings:
FIG. 1 is a schematic structural diagram of a device for preparing a macroscopic rope with a boron nitride one-dimensional nanostructure.
In the figure, 1 a catalyst precursor is floated; 2, reacting a reactant; 3, graphite flakes; 4, a thermocouple; 5, a reaction vessel; 6, air inlet pipe; 7 exhausting pipe; 8 reaction sleeve.
FIG. 2 shows the characterization results of the macroscopic ropes of one-dimensional boron nitride nanostructures prepared in example 1. Wherein (a-b) a scanning electron micrograph; (c-d) Transmission Electron micrograph.
FIG. 3 is a scanning electron microscope photograph of the boron nitride nanostructured macroscopic lines after gas-liquid interface manipulation and assembly in example 2. Wherein, the picture (a) is a low magnification photograph; (b) the figure is a high magnification photograph.
FIG. 4 scanning electron microscope photograph of the boron nitride nanostructure in example 3. Wherein, the picture (a) is a structure of a boron nitride high-purity nanotube; (b) and (4) compacting the nanotubes.
The specific implementation mode is as follows:
as shown in fig. 1, the device for preparing the boron nitride one-dimensional nanostructure macroscopic rope of the present invention employs a horizontal chemical vapor deposition tube type reaction furnace, and has the following specific structure:
the reaction vessel 5 of the device is of a tubular structure, the inner diameter of the reaction vessel is 40-60 mm, an electric heating part is arranged on the outer side of the reaction vessel 5, a reaction sleeve 8 is arranged in the reaction vessel 5, the reaction sleeve 8 is a corundum tube with the inner diameter of 30-40mm, the two ends of the reaction vessel 5 are respectively connected with an air inlet pipe 6 and an air outlet pipe 7, the air inlet pipe 6 extends into the reaction sleeve 8, a thermocouple 4 extends into the inner cavity of the reaction vessel 5, and temperature measurement and temperature control are achieved through the thermocouple and a computer program. The interior of a reaction sleeve 8 in a reaction container 5 is divided into a high-temperature area and a low-temperature area, the high-temperature area is positioned in the middle of the reaction container 5, the low-temperature area is positioned at one end part of the reaction container 5, a reactant 2 and a reaction promoter are placed on a graphite sheet 3 in the high-temperature area in the reaction sleeve 8, a floating catalyst precursor 1 is placed in the low-temperature area in the reaction sleeve 8, and a carrier gas (Ar) and a nitrogen source gas (NH) are introduced through an air inlet pipe 6 after the temperature is raised3)。
The invention adopts a floating catalyst chemical vapor deposition method, takes ferrocene as a floating catalyst precursor, the floating catalyst precursor is sublimated and volatilized in a low-temperature region and is carried by carrier gas to a high-temperature region to be decomposed into nano metal (Fe) particles, and the nano metal (Fe) particles are taken as a catalyst for the growth of a Boron Nitride (BN) nano structure to promote boron powder and boron oxide to react to generate B2O2The steam reacts with ammonia gas to generate the boron nitride one-dimensional nanostructure. Meanwhile, the airflow is controlled by a reaction sleeve in the reaction furnace, the boron nitride one-dimensional nano structures are directionally arranged under the action of the airflow, the generated boron nitride one-dimensional nano structures are self-assembled to form a macroscopic rope-shaped structure, the macroscopic rope-shaped structure is controlled and assembled into a compact structure through a gas-liquid interface, and a sample is collected at the tail part of the reaction sleeve after the reaction is finished.
Example 1
The precursor of the floating catalyst is 0.8g of ferrocene, the weight ratio of the usage amount of the precursor to the total weight of reactants (boron powder and boron oxide) is 0.5: 1, the evaporation temperature is 150 ℃, the flow rate of ammonia gas is 50 ml/min, the flow rate of argon gas is 300 ml/min, the weight ratio of the boron powder to the boron oxide is 1: 7, and Fe is adopted as a reaction promoter2O3FeS and ZnS, Fe2O3Weight ratio of FeS to ZnSThe weight ratio of the reaction accelerator to the sum of the reactant boron powder and the boron oxide is 2: 1: 2, the reaction temperature is 1350 ℃, the heating rate is 30 ℃/min, and the reaction time is 2 hours. The boron nitride nanofibers (single fibers) with the diameter of about 200 nanometers and the length of 100-200 micrometers are obtained, the reaction sleeve in the reaction furnace plays a role in stabilizing air flow, the generated boron nitride nanofibers are self-assembled to form a loose macroscopic rope-shaped structure, and the characterization result is shown in figure 2. From the scanning electron microscope photograph, the boron nitride nano-structure is directionally arranged, but is loose, and has a plurality of holes and branches. From the high resolution image, it is clear that (0002) is aligned perpendicular to the axial direction with a purity of about 95 wt%.
Example 2
The boron nitride oriented structure prepared in example 1 was immersed in an ethanol solution for 1 hour, sufficiently soaked, and then gently lifted with tweezers. Due to the surface tension, the loose boron nitride structure becomes dense while maintaining its original highly directional arrangement. The diameter of the boron nitride dense-micron fiber macroscopic rope can be controlled to be between 1 mu m and 1mm, and the length of the boron nitride dense-micron fiber macroscopic rope is controlled to be between 0.5cm and 5cm according to the quantity of the boron nitride nanostructures used.
As shown in fig. 3, it can be seen from the scanning electron microscope photograph that the diameter of the boron nitride dense-micron fiber macroscopic rope of the present embodiment is about 250 μm, and the macroscopic rope is dense and substantially without bifurcation, while maintaining the original directional arrangement.
Example 3
The precursor of the floating catalyst is 0.3g of ferrocene, the weight ratio of the usage amount of the precursor to the total weight of reactants (boron powder and boron oxide) is 1: 1, the evaporation temperature is 200 ℃, the ammonia flow is 100 ml/min, the argon flow is 100 ml/min, the weight ratio of the boron powder to the boron oxide is 1: 1, and Fe is adopted as a reaction promoter2O3FeS and ZnS, Fe2O3FeS and ZnS in a weight ratio of 2: 1: 2, the weight ratio of the reaction promoter to the sum of the reactant boron powder and the boron oxide is 0.5: 1, the reaction temperature is 1500 ℃, and the temperature rise rate is high20 ℃/min and the reaction time is 3 hours. Obtaining boron nitride nanotubes (single nanotubes) with the inner diameter of 20-40 nm, the wall thickness of 5-10 nm and the length of 50-80 microns, and performing the function of stabilizing air flow through a reaction sleeve in the reaction furnace, so that the generated boron nitride one-dimensional nanostructures are self-assembled to form a loose macroscopic rope-shaped structure, and the characterization result is shown in figure 4. From the scanning electron microscope photograph, the boron nitride nano-structure is directionally arranged, but is loose, and has a plurality of holes and branches. From the high resolution image, it is clear that (0002) is aligned perpendicular to the axial direction with a purity of about 95 wt%.
The prepared boron nitride nanotube is soaked in ethanol solution for 1 hour, fully soaked and then slightly lifted by tweezers. The diameter of the formed boron nitride dense macroscopic rope is between 1 μm and 1mm, and the length is between 0.5cm and 5 cm.
As shown in fig. 4, it can be seen from the scanning electron micrograph that the boron nitride high purity nanotube structure (a) of this example is converted into a dense macroscopic rope (b) having a diameter of about 25 μm by the gas-liquid interface operation.
Claims (10)
1. A method for preparing a boron nitride one-dimensional nanostructure macroscopic rope is characterized by comprising the following steps: the method adopts a horizontal chemical vapor deposition tube type reaction furnace, a reaction sleeve in the reaction furnace is divided into a high-temperature area and a low-temperature area, a floating catalyst precursor is placed in the low-temperature area, and boron powder and boron oxide are placed in the high-temperature area; ferrocene is used as a floating catalyst precursor, the floating catalyst precursor is volatilized in a low-temperature region and carried to a high-temperature region by carrier gas to be decomposed into a metal catalyst, and diboron dioxide steam generated by the reaction of boron powder and boron oxide in the high-temperature region is promoted to react with a nitrogen source to generate a boron nitride one-dimensional nanostructure; meanwhile, the reaction sleeve in the reaction furnace has the function of stabilizing the airflow, so that the generated boron nitride one-dimensional nano structure is self-assembled to form a loose macroscopic rope-shaped structure.
2. The method for preparing the boron nitride one-dimensional nanostructure macroscopic rope according to claim 1, characterized in that: the weight ratio of the boron powder to the boron oxide is 1: 1-1: 7.
3. The method for preparing the boron nitride one-dimensional nanostructure macroscopic rope according to claim 1, characterized in that: the reaction temperature in the low temperature region is 100-.
4. The method for preparing the boron nitride one-dimensional nanostructure macroscopic rope according to claim 1, characterized in that: the weight ratio of the floating catalyst precursor to the sum of the reactant boron powder and boron oxide is (0.5-2) to 1.
5. The method for preparing the boron nitride one-dimensional nanostructure macroscopic rope according to claim 1, characterized in that: the flow ratio of the carrier gas to the nitrogen source is 0.25-6: 1, and the gas flow of the nitrogen source is 10-200 ml/min.
6. The method for preparing the boron nitride one-dimensional nanostructure macroscopic rope according to claim 1, characterized in that: keeping the temperature of the diboron dioxide steam and the nitrogen source constant at the reaction temperature for 60-180 minutes.
7. The method for preparing the boron nitride one-dimensional nanostructure macroscopic rope according to claim 1, characterized in that: a reaction promoter is arranged in the high-temperature zone, and the reaction promoter adopts Fe2O3FeS and ZnS, Fe2O3FeS and ZnS in a weight ratio of 2: 1: 2, and the reaction accelerator in a weight ratio with the sum of the reactant boron powder and boron oxide in an amount of (0.25 to E%0.5)∶1。
8. The method for preparing the boron nitride one-dimensional nanostructure macroscopic rope according to claim 1, characterized in that: the boron nitride one-dimensional nano structure is a boron nitride nano tube or a boron nitride nano fiber.
9. The method for preparing the boron nitride one-dimensional nanostructure macroscopic rope according to claim 1, characterized in that: soaking the loose boron nitride one-dimensional nano-structure macroscopic rope in an ethanol solution for one hour, fully soaking, and assembling the boron nitride directional nano-structure into a compact boron nitride one-dimensional nano-structure macroscopic rope under the action of surface tension of an ethanol-atmosphere liquid surface.
10. The method for preparing the boron nitride one-dimensional nanostructure macroscopic rope according to claim 1, characterized in that: the diameter of the compact boron nitride one-dimensional nanostructure macroscopic rope is controlled to be between 1 mu m and 1mm, and the length of the compact boron nitride one-dimensional nanostructure macroscopic rope is controlled to be between 0.5cm and 5 cm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104528671A (en) * | 2015-01-20 | 2015-04-22 | 河北工业大学 | Preparation method of porous boron nitride nanofibers |
| CN104743530A (en) * | 2015-03-31 | 2015-07-01 | 盐城工学院 | Method for preparing boron nitride nano-fibres by virtue of arc discharge |
| WO2017155468A1 (en) * | 2016-03-09 | 2017-09-14 | Nanyang Technological University | Chemical vapor deposition process to build 3d foam-like structures |
| CN108584891A (en) * | 2018-07-20 | 2018-09-28 | 芜湖清柏白露智能信息科技有限公司 | A kind of preparation method of boron nitride nanometer band |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1281481C (en) * | 2004-07-08 | 2006-10-25 | 北京理工大学 | Process for preparing boron nitride nano tube |
| CN100526217C (en) * | 2006-04-29 | 2009-08-12 | 中国科学院金属研究所 | Preparation method of quasi one-dimensional boron nitride nanostructure |
| CN101513995B (en) * | 2009-04-01 | 2010-12-29 | 武汉工程大学 | Method for preparing boron nitride nano-tube |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104528671A (en) * | 2015-01-20 | 2015-04-22 | 河北工业大学 | Preparation method of porous boron nitride nanofibers |
| CN104743530A (en) * | 2015-03-31 | 2015-07-01 | 盐城工学院 | Method for preparing boron nitride nano-fibres by virtue of arc discharge |
| WO2017155468A1 (en) * | 2016-03-09 | 2017-09-14 | Nanyang Technological University | Chemical vapor deposition process to build 3d foam-like structures |
| CN108699684A (en) * | 2016-03-09 | 2018-10-23 | 南洋理工大学 | Chemical vapour deposition technique builds three-dimensional foam shape structure |
| CN108699684B (en) * | 2016-03-09 | 2021-08-24 | 南洋理工大学 | Chemical vapor deposition process for building three-dimensional foam-like structures |
| US11104989B2 (en) | 2016-03-09 | 2021-08-31 | Nanyang Technological University | Chemical vapor deposition process to build 3D foam-like structures |
| CN108584891A (en) * | 2018-07-20 | 2018-09-28 | 芜湖清柏白露智能信息科技有限公司 | A kind of preparation method of boron nitride nanometer band |
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