WO2013105740A1 - Composite de ciment comprenant un nanotube de carbone, son procédé de préparation, et procédé de production d'une structure nanotube de carbone-ciment utilisant ledit composite de ciment - Google Patents

Composite de ciment comprenant un nanotube de carbone, son procédé de préparation, et procédé de production d'une structure nanotube de carbone-ciment utilisant ledit composite de ciment Download PDF

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Publication number
WO2013105740A1
WO2013105740A1 PCT/KR2012/010718 KR2012010718W WO2013105740A1 WO 2013105740 A1 WO2013105740 A1 WO 2013105740A1 KR 2012010718 W KR2012010718 W KR 2012010718W WO 2013105740 A1 WO2013105740 A1 WO 2013105740A1
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WIPO (PCT)
Prior art keywords
cement
carbon nanotube
composite material
cement composite
silica fume
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PCT/KR2012/010718
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English (en)
Korean (ko)
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이행기
김형기
남일우
전정희
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한국과학기술원
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Publication of WO2013105740A1 publication Critical patent/WO2013105740A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/38—Fibrous materials; Whiskers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B16/04—Macromolecular compounds
    • C04B16/06—Macromolecular compounds fibrous
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B18/04—Waste materials; Refuse
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/04—Carboxylic acids; Salts, anhydrides or esters thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
    • C04B2111/00258—Electromagnetic wave absorbing or shielding materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Definitions

  • the present invention relates to a cement composite material containing carbon nanotubes and a method for manufacturing the same, and more particularly, to a cement composite material having improved dispersion performance by improving carbon nanotube dispersion performance by physical methods using nanomaterials and The manufacturing method and the method of manufacturing a carbon nanotube-cement structure using this cement composite material.
  • Carbon nanotube (CNT) one of the advanced nanomaterials, has been steadily researched and commercialized in various fields since its discovery in 1991 based on its unique structural, chemical, mechanical and electrical properties due to its highly stable chemical bonding. .
  • CNT Carbon nanotube
  • Sonication a method of dispersing carbon nanotubes, which has been used in the related art, is a method of physically separating and dispersing entangled carbon nanotubes using a sound wave of 10-20 Hz after putting carbon nanotubes in a surfactant.
  • the present invention is to solve the conventional problems as described above, an object of the present invention is to mix the carbon nanotubes (CNT) with low dispersibility to the cement to prepare a cement composite material of the carbon nanotubes in the cement matrix
  • the present invention provides a cement composite material and a method for manufacturing the same, and a method for producing a carbon nanotube-cement structure using the cement composite material.
  • the present invention for achieving the above object, it comprises a carbon nanotube, silica fume (Silica fume), cement and a polycarboxylic acid-based admixture as a main component Cement composite material is provided.
  • the method comprises the steps of: (a) mixing the carbon nanotubes, silica fume and cement to dry beam for a set time; (b) adding a water and a polycarboxylic acid superfluiding agent to the dry non-beamed mixture to provide a method for producing a cement composite material, comprising the step of beaming for a predetermined time.
  • the step of injecting a cement composite material produced by the cement composite material manufacturing method into a mold (b) demolding after a set time to obtain a carbon nanotube-cement structure base material of a specific type; (c) providing a method for producing a carbon nanotube-cement structure, comprising curing the demolded carbon nanotube-cement structure base material in water for a set time.
  • the present invention in the conventional sonication process by simplifying the carbon nanotube dispersion process by using a physical dispersion method using nanomaterials instead of the dispersion method using a surfactant and sonication that has been widely used in the prior art It can reduce the time and cost and can also solve the physical degradation of the cement structure that can be caused by the surfactant.
  • the carbon nanotube dispersion method and the dispersibility of the carbon nanotubes in the cement matrix can be improved compared to the conventional dispersion technology, thereby increasing the usability as a construction material and improving the field applicability.
  • 1 is a flow chart illustrating a method for producing cement mortar as a cement composite material according to the present invention.
  • Figure 2 is a flow chart illustrating a method for producing a carbon nanotube-cement structure using the cement composite material of the present invention.
  • FIG. 3 is a view showing an embodiment of a test specimen used in measuring the compressive strength of the carbon nanotube-cement structure of the present invention.
  • FIG. 5 is a graph showing compressive strength according to silica fume incorporation rate of a carbon nanotube-cement structure according to the present invention.
  • FIG. 6 is a flowchart illustrating a method of manufacturing a cement paste and a carbon nanotube-cement structure using the same as a cement composite material according to another embodiment of the present invention.
  • FIG. 7 is a view schematically showing a test specimen used in an electromagnetic shielding experiment as an example of a carbon nanotube-cement structure manufactured by the manufacturing method of FIG. 6.
  • the cement composite material according to the present invention is a mixture of carbon nanotubes (CNT) and nanomaterial silica fume (Silica fume), cement, fine aggregate, polycarboxylic acid-based admixture (water) Are manufactured.
  • CNT carbon nanotubes
  • Silica fume nanomaterial silica fume
  • cement fine aggregate
  • polycarboxylic acid-based admixture water
  • Carbon nanotubes are small sized nanoparticles in the form of tubes, and are used in various fields based on their unique structural, chemical, mechanical and electrical properties due to the strong chemical bond called sp2.
  • the carbon nanotubes may be used in various kinds, but it is preferable to use multi-wall carbon nanotubes having various lengths.
  • the present invention is a silica fume having a small particle size, such as carbon nanotubes of 10 ⁇ 500 nm in carbon nanotubes having low dispersibility due to the high length-to-diameter ratio, strong hydrophobicity and van der Waals attraction as described above
  • a cement composite material capable of effectively dispersing carbon nanotubes in a cement matrix is prepared, and a carbon nanotube-cement structure is realized using the cement composite material thus prepared.
  • Silica fume incorporated in the cement composite material of the present invention is preferably 10 to 20% by weight of the cement, respectively.
  • a predetermined amount of carbon nanotubes, silica fume, cement and fine aggregates are mixed and dry-beamed for a predetermined time (for example, about 4 minutes) using a rotary stirrer (step S11).
  • the carbon nanotubes are mixed with 0.15 to 0.3 wt% based on the weight of cement mixed together.
  • silica fume may be mixed with 10-30% by weight (preferably 10-20% by weight) of the cement weight, but is not limited thereto.
  • the cement composite material of the present invention is completed by adding water and a polycarboxylic acid-based superfluiding agent to the beam and performing the beam for a predetermined time (for example, about 2 minutes). S12).
  • silica fume a nanomaterial for dispersing portland cement and carbon nanotubes
  • the chemical and physical properties of the portland cement and silica fume are shown in Table 1 below.
  • the cement composite material of the present invention made through the above process has a high dispersion performance by helping the physical dispersion of carbon nanotubes in the cement matrix by using silica fume which is a nanomaterial, thereby realizing physical performance improvement.
  • the cement composite material of the present invention can be made into a carbon nanotube-cement structure of a particular type by a mold. That is, as shown in Fig. 2, the cement composite material according to the present invention is injected into a mold having a cavity of a specific type (step S13), and demolded after a set time (for example, 24 hours) to form a carbon nano of a specific type. A tube-cement structure base material is obtained (step S14). Subsequently, in order to suppress cracking or shrinkage of the demolded carbon nanotube-cement structure base material, the carbon nanotube-cement structure base material is cured for a set time (for example, 14 to 15 days) (step S15), and the set time. After the passage, the completed carbon nanotube-cement structure is taken out (step S16).
  • a set time for example, 14 to 15 days
  • FIG. 3 is a test specimen used for compressive strength experiments for measuring physical performance improvement according to the improvement of carbon nanotube dispersion of cement composites according to the present invention. Cylindrical carbon nanoparticles manufactured using the cement composite material according to the present invention.
  • the tube-cement structure 1 is shown. This carbon nanotube-cement structure 1 is a cylindrical specimen of 100 mm (diameter) x 200 ⁇ 5 mm (height).
  • FIG. 4 is an SEM observation photograph of the carbon nanotube-cement structure (1), in which a cross section of a cured specimen was observed for 24 hours, and it was confirmed that silica fume particles were uniformly dispersed between individual carbon nanotubes. . This confirms that silica fume helps the dispersion of carbon nanotubes. That is, the cement composite material according to the present invention was confirmed that the carbon nanotubes are dispersed by silica fume as a nano material.
  • silica fume content is set to 0 wt%, 10 wt%, 20 wt%, and 30 wt%, respectively.
  • the cement composite material was prepared according to the above-described cement composite material manufacturing method of the present invention on the basis of 12 different formulations by varying the tube mixing rate of 0.0 wt%, 0.15 wt%, and 0.3 wt%, respectively, as shown in FIG. 2.
  • the carbon nanotube / cement structure 1 was produced in the same manner as described above, and the compressive strength of the carbon nanotube-cement structure 1 was measured. The following measurement results were obtained.
  • FIG. 5 is a graph showing the compressive strength of the 14-day cement composite material showing the change in the compressive strength according to the silica fume mixing rate of the carbon nanotube mixing rate of the different specimens.
  • the relative compressive strength in the graph shows the ratio of each specimen to the compressive strength of cement composite material without carbon nanotubes.
  • the relative compressive strength of the comparative group increased significantly from 10% by weight of silica fume, and then decreased from 20% by weight, and slightly improved by 30% by weight. Showed.
  • the compressive strength was continuously increased for the comparative group until the silica fume was 20 wt%, and the compressive strength was decreased at the silica fume incorporation rate of 30 wt%.
  • Such a result can be predicted because silica fume itself performs a pozzolanic reaction, thereby making a tighter structure than a test sample in which silica fume is not incorporated, thereby improving compressive strength.
  • the carbon nanotubes When the carbon nanotubes are mixed, it can be expected that the agglomeration of the carbon nanotubes generating the voids is effectively dispersed by silica fume, thereby reducing the voids in the structure, thereby making the chamber more compact, and improving the compressive strength.
  • Figure 6 shows another embodiment of a method for producing a cement paste as a cement composite material according to the present invention
  • the cement composite material of this second embodiment is different from the cement composite material of the above-described embodiment without mixing the fine aggregate
  • the cement composite material according to this second embodiment is prepared by mixing carbon nanotubes (CNT: Carbon Nanotube) and nanomaterial silica fume, cement, polycarboxylic acid-based superfluidizer, nylon fibers with water.
  • CNT Carbon Nanotube
  • nanomaterial silica fume cement, polycarboxylic acid-based superfluidizer, nylon fibers with water.
  • a predetermined amount of carbon nanotubes, silica fume, and cement are mixed and dried for a predetermined time (for example, about 3 minutes) (step S21).
  • the carbon nanotubes are preferably mixed with 0.3 to 1.0% by weight based on the weight of the cement mixed together.
  • Silica fume may be mixed with 10-30% (preferably 10-20%) by weight of cement, but is not limited thereto.
  • step S22 After the completion of the dry beam, after the addition of water and polycarboxylic acid-based superfluidizing agent to the dry beam, and performing the beam for a set time (for example, about 3 minutes), and finally after the addition of nylon fiber set time ( For example, about 3 minutes) to perform the beam beam to complete the paste-like cement composite material according to the present invention (step S22).
  • a set time for example, about 3 minutes
  • nylon fiber set time For example, about 3 minutes
  • the cement paste of the present invention may be made into a specific type of carbon nanotube-cement structure by a plastic mold. That is, the cement paste according to the present invention is injected into a plastic mold having a specific type of cavity (step S23), and demolded after a set time (for example, 24-48 hours) to obtain a carbon nanotube-cement structure of a specific type. . Subsequently, in order to suppress cracking or shrinkage of the demolded carbon nanotube-cement structure, the carbon nanotube-cement structure is cured in water for a set time (for example, 28 days) (step S24).
  • a set time for example, 28 days
  • FIG. 7 shows an example of a carbon nanotube-cement structure 2 fabricated using the above cement paste composite material.
  • the present invention comprises a donut shape having an inner diameter of 3 mm, an outer diameter of 7 mm, and a thickness of 4.5 mm. It was used as an experiment for measuring physical performance improvement according to the improvement of carbon nanotube dispersibility of cement composite material according to the second embodiment of.
  • the silica fume incorporation rate of the test body of the carbon nanotube-cement structure (2) was set to 0 wt%, 10 wt%, 20 wt%, and 30 wt%, respectively, and the carbon nanotube incorporation rates were 0.0 wt%, 0.3 wt%, and 0.6 wt%, respectively.
  • the cement composite material was prepared according to the method of manufacturing the cement composite material of the second embodiment based on the 16 kinds in different amounts by weight and 1.0 weight%, and then carbon nanotubes in the form as shown in FIG. 8-
  • the cement structure 2 was fabricated, and the electromagnetic shielding performance of the carbon nanotube-cement structure 2 was measured. As a result, measurement results as shown in FIG. 8 were obtained.
  • Figure 8 shows the electromagnetic shielding performance according to the silica fume mixing rate in the 2.46 GHz frequency range, the overall silica shielding performance was increased up to the silica fume mixing rate up to 20% by weight as the silica fume mixing rate is increased, the silica fume mixing rate 30 weight Above%, the electromagnetic shielding performance was reduced overall. This phenomenon was remarkable in the cement paste containing 0.6 wt% of carbon nanotubes. Through this, it was confirmed that the carbon nanotubes having conductivity at the silica fume mixing rate of 10 to 20% by weight were most effectively dispersed by silica fume and exhibit the highest electric wave shielding performance.
  • the cement composite material of the present invention and the carbon nanotube-cement structure using the same have improved dispersibility of carbon nanotubes by silica fume and thus have excellent compressive strength and electromagnetic shielding performance.
  • the present invention can be applied to cement composites such as cement paste and concrete mortars, cement structures, concrete structures and methods for producing them.

Abstract

Cette invention concerne : un composite de ciment comprenant un nanotube de carbone (CNT) pour mettre en œuvre la dispersion élevée d'un nanotube de carbone dans une matrice de ciment lors de la préparation d'un composite de ciment par mélange d'un nanotube de carbone à basse dispersion dans le ciment ; un procédé pour le préparer ; et un procédé de production d'une structure nanotube de carbone-ciment utilisant ledit composite de ciment. Selon la présente invention, le procédé de préparation du composite de ciment comprend : (a) une étape de mélange d'un nanotube de carbone, de fumée de silice, de ciment, et d'un agrégat fin et d'homogénéisation à sec pendant un laps de temps défini ; et (b) une étape d'ajout d'eau et d'un superplastifiant à base d'acide polycarboxylique au mélange homogénéisé à sec et de mélange pendant un laps de temps défini.
PCT/KR2012/010718 2012-01-13 2012-12-10 Composite de ciment comprenant un nanotube de carbone, son procédé de préparation, et procédé de production d'une structure nanotube de carbone-ciment utilisant ledit composite de ciment WO2013105740A1 (fr)

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KR20120004384A KR101339904B1 (ko) 2012-01-13 2012-01-13 탄소나노튜브를 함유한 시멘트 복합재료의 제조방법과 이 시멘트 복합재료를 이용한 탄소나노튜브-시멘트 구조체의 제조방법
KR10-2012-0004384 2012-01-13

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CN111807772A (zh) * 2020-07-14 2020-10-23 李焕醒 一种具有电磁波吸收功能的浮石混凝土及其制备方法
CN111807772B (zh) * 2020-07-14 2021-12-07 乐清市凡山电器有限公司 一种具有电磁波吸收功能的浮石混凝土及其制备方法
CN114956771A (zh) * 2022-04-29 2022-08-30 山西中矿威特矿山技术开发有限公司 一种无机复合型矿用注浆加固材料
CN114956771B (zh) * 2022-04-29 2023-05-23 山西中矿威特矿山技术开发有限公司 一种无机复合型矿用注浆加固材料

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