CN109081704A - A kind of preparation method of the carbon foam of bore diameter gradient variation - Google Patents

A kind of preparation method of the carbon foam of bore diameter gradient variation Download PDF

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Publication number
CN109081704A
CN109081704A CN201810937819.9A CN201810937819A CN109081704A CN 109081704 A CN109081704 A CN 109081704A CN 201810937819 A CN201810937819 A CN 201810937819A CN 109081704 A CN109081704 A CN 109081704A
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carbon foam
silicon dioxide
dioxide microsphere
mold
slurry
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汤浩
其他发明人请求不公开姓名
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Suzhou Superlong Aviation Heat Resistance Material Technology Co Ltd
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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
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/04—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by dissolving-out added substances
    • C04B38/045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by dissolving-out added substances the dissolved-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a prepreg obtained by bonding together dissolvable particles
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Abstract

The invention discloses a kind of preparation methods of the carbon foam of bore diameter gradient variation, comprising the following steps: the silicon dioxide microsphere of three kinds of diameters successively tiles three layers of varying thickness in mold, is mixed into slurry with organic additive and water after pitch is crushed；It adds slurry into mold, then dry solidification, demoulds and presoma is made, be then carbonized presoma, and silicon dioxide microsphere/carbon foam composite is made, and the carbon foam of bore diameter gradient variation is made with hydrofluoric acid clean silicon dioxide microsphere/carbon foam composite.Using one-shot forming technique, without using bonding agent, it is more excellent that carbon foam performance is made in the present invention；Compared to the uniform carbon foam in aperture, gradient carbon foam filtration resistance is lower, separative efficiency is higher, can be used as filtering material；Spacecraft inside and outside temperature difference is adapted to, can be used as the super heat proof material of aerospace flight technology；It can according to need the bore diameter gradient of the carbon foam of control.

Description

A kind of preparation method of the carbon foam of bore diameter gradient variation
Technical field
The present invention relates to a kind of preparation methods of carbon foam, more particularly, to a kind of system of the carbon foam of bore diameter gradient variation Preparation Method belongs to carbon material field.
Background technique
Functionally gradient material (FGM) is met under extreme environment constantly repeatedly just to adapt to new material in the needs of high-tech sector A kind of advanced composite material (ACM) for often working and developing.Its Nomenclature Composition and Structure of Complexes through-thickness changes in gradient, therefore the property of material Can also it change in gradient.Due to its mechanical strength with higher, heat shock resistance, the excellent performance such as high temperature resistant, once proposition It just causes the great attention of countries in the world researcher and expands research to it.It is usually viscous for the foamed material of low-density The method connect prepares the gradient foam with laminated construction.But bonding agent is used, bonding interface will lead to fine and close The presence of adhesive layer, foam gradient-structure can be destroyed.It, also can thin-walled knot to foam when applying pressure during the bonding process Structure is destroyed, to influence foamy body.
Carbon foam is that a kind of steeped by hole has tridimensional network with what hole steep that wall interconnected formed, spongy in class Novel carbonaceous material, have low-density, high porosity, biggish specific surface area, good absorption property, lower thermal expansion The features such as coefficient and low thermal conductivity coefficient, it can be used as heat-barrier material, high-quality sandwich material, ability storage electrode, energy absorbing material, Catalyst carrier and deodorization eliminating smell agent etc., in chemical industry, the fields such as aerospace and electronics are widely used in value.
Application No. is the patents of CN 201710671166.X to provide a kind of preparation of vitreous silica gradient pore foamed ceramics Method, it is characterised in that: the preparation method includes the following steps: (1) by fused quartz powder, water, water-soluble resin, dispersing agent Stirring 2-4 hours, obtains vitreous silica slurry；(2) by the impregnating slurry of step (1) on polyurethane sponge, roller is squeezed out more Remaining slurry material, obtains biscuit, and dry biscuit is obtained after being placed in oven and dried；(3) by fused quartz ceramic powder, water, dispersing agent and Foam stabilizer ball milling obtains slurry for 3-6 hours, and foaming agent is added, and stirring foaming obtains foamed slurry；(4) by the foam of step (3) Slurry is coated in the drying biscuit of step (2) preparation, be then placed in baking oven it is dry after be warming up to 1100-1250 DEG C and be sintered To gradient pore vitreous silica foamed ceramics；The vitreous silica gradient pore foamed ceramics of invention preparation realizes aperture grade to micro- Meter level change of gradient has higher fine, the stronger adsorbing contaminant ability of filtering compared with conventional foam ceramic filter.
Application No. is the patents of CN 200710173126.9 to provide a kind of high-strength coal tar asphalt carbon foam material Coal tar asphalt is prepared mesophase pitch by pyrolysis, is added in toluene solution and extracts after crushing by preparation method, dry, Add autoclave, vacuumize and be warming up to asphalt softening point or more and be filled with inert gas, in 350-500 DEG C of temperature and 6-80kg/cm2Pressure under kept for 120-240 minutes, release stress, be cooled to room temperature, obtain asphalt foam material, by pitch Carbon foam is made under 1300-1600 DEG C of nitrogen protection in carbon foam, and carbon foam compressive strength is greater than 20MPa.
Application No. is the patents of CN 200910093957.4 to provide the carbon foam heat insulating material of addition hollow ceramic ball Preparation method: surfactant, foaming agent and hollow ceramic microspheres are added sequentially in phenolic resin by composition of raw materials, use machine The mode that tool stirring and supersonic oscillations combine carries out mixture evenly dispersed；It is added into the mixture after being uniformly dispersed Curing agent is poured into mold after stirring and foams and solidify, obtains phenol formaldehyde foam；After phenol formaldehyde foam decladding processing, it is put into In vacuum carburization furnace, 800 DEG C are heated to the rate of average 0.5 DEG C/min under vacuum conditions, obtains the heat-insulated material of carbon foam Material.The high temperature insulating material has light weight, and intensity is high, and thermal conductivity is low, and thermal expansion coefficient is low, and at low cost and designability etc. is excellent Point
Its preparation process and performance have very big difference, gradient carbon foam compared with the gradient carbon foam carbon foam uniform with aperture It is the carbon material for doing regular diminution or increase with thickness in the aperture of carbon foam, this is a kind of novel carbon foam.For Many particular applications are a kind of carbon materials it is intended that obtaining.Gradient carbon foam is more applied compared with general carbon foam Prospect, filtration resistance is lower, separative efficiency is higher, can be used as high efficiency filter material, is furthermore alternatively arranged as understanding aviation boat of determining Thermally protective materials, barrier material and anti-thermal shock structural material in its field.
Summary of the invention
The purpose of the present invention overcomes the shortcomings of the prior art, and provides a kind of preparation of the carbon foam of bore diameter gradient variation Method includes the steps that following sequence:
(1) successively tile three layers of silicon dioxide microsphere in mold；Lower thickness is 10-30mm, and silicon dioxide microsphere diameter is 200-250 μm, intima-media thickness 20-50mm, silicon dioxide microsphere diameter is 200-150 μm, upper thickness 10-30mm, two Silica diameter is 100-150 μm；
(2) high softening-point asphalt is crushed, be ground to 15 μm hereinafter, then with the organic additive of 1-3wt%, 25- The water of 35wt% mixes, and forms uniformity slurry, and organic additive is binder, thickener and suspending agent；
(3) slurry in step (2) is added in mold along mold wall, slurry liquid level is higher than top layer's silica 1 0- 20mm；
(4) mold in step (3) is put into and is dried to obtain presoma in baking oven, presoma is demoulded and is taken out；
(5) presoma after the drying in step (4) is put into pyrolysis oven, is passed through the argon gas of flowing, with 1-5 DEG C/min heating To 400-500 DEG C, room temperature is cooled to the furnace after keeping the temperature 1-3h；Then pass to 0.5-1m3The air of/h, with 0.2-0.8 DEG C/min It cools to room temperature after being warming up to 300-400 DEG C with the furnace, then to be passed through the argon gas of flowing, 800- is warming up to 10-20 DEG C/min 1200 DEG C, room temperature is cooled to the furnace after keeping the temperature 1h；Silicon dioxide microsphere/carbon foam composite is made；
(6) it by silicon dioxide microsphere/carbon foam composite made from step (5), is cleaned with hydrogen fluoride, aperture ladder is made Spend the carbon foam of variation.
The beneficial technical effect of the present invention lies in:
(1) it is more excellent to be made without using bonding agent using one-shot forming technique for carbon foam performance；(2) uniform compared to aperture Carbon foam, gradient carbon foam filtration resistance is lower, separative efficiency is higher, can be used as filtering material；(3) it adapts to inside and outside spacecraft Temperature gradient is poor, can be used as the super heat proof material of aerospace flight technology；(4) it can according to need the bore diameter gradient of the carbon foam of control.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention Rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalences of the invention It is as defined in the appended claims that the modification of form falls within the application.
Embodiment 1
(1) successively tile three layers of silicon dioxide microsphere in mold；Lower thickness is 22mm, and silicon dioxide microsphere diameter is 220 μ M, intima-media thickness 40mm, silicon dioxide microsphere diameter are 160 μm, upper thickness 25mm, and silica diameter is 120 μm；
(2) high softening-point asphalt is crushed, is ground to 15 μm hereinafter, the then water with the organic additive of 3wt%, 25wt% Mixing, forms uniformity slurry, and organic additive is binder, thickener and suspending agent；
(3) slurry in step (2) is added in mold along mold wall, slurry liquid level is higher than top layer's silica 1 8mm；
(4) mold in step (3) is put into and is dried to obtain presoma in baking oven, presoma is demoulded and is taken out；
(5) presoma after the drying in step (4) is put into pyrolysis oven, is passed through the argon gas of flowing, be warming up to 2 DEG C/min 400 DEG C, room temperature is cooled to the furnace after keeping the temperature 2h；Then pass to 0.5m3The air of/h, after being warming up to 350 DEG C with 0.6 DEG C/min with Furnace is cooled to room temperature, and then to be passed through the argon gas of flowing, is warming up to 850 DEG C with 15 DEG C/min, is cooled to room with the furnace after keeping the temperature 1h Temperature；Silicon dioxide microsphere/carbon foam composite is made；
(6) it by silicon dioxide microsphere/carbon foam composite made from step (5), is cleaned with hydrogen fluoride, aperture ladder is made Spend the carbon foam of variation.
Carbon foam density obtained is 6.347.68 kg/m3, with a thickness of 79.3mm, carbon foam top aperture is small, bottom hole Diameter is big, and aperture has change of gradient from top to bottom inside carbon foam, can be used as gradient filtration material, reduces filtration resistance, energy Filtering accuracy and filter efficiency are enough improved, and is prolonged the service life.
Embodiment 2
(1) successively tile three layers of silicon dioxide microsphere in mold；Lower thickness is 25mm, and silicon dioxide microsphere diameter is 250 μ M, intima-media thickness 28mm, silicon dioxide microsphere diameter are 170 μm, upper thickness 20mm, and silica diameter is 130 μm；
(2) high softening-point asphalt is crushed, be ground to 15 μm hereinafter, then with the organic additive of 2.5wt%, 35wt% Water mixing, forms uniformity slurry, and organic additive is binder, thickener and suspending agent；
(3) slurry in step (2) is added in mold along mold wall, slurry liquid level is higher than top layer's silica 20mm；
(4) mold in step (3) is put into and is dried to obtain presoma in baking oven, presoma is demoulded and is taken out；
(5) presoma after the drying in step (4) is put into pyrolysis oven, is passed through the argon gas of flowing, be warming up to 4 DEG C/min 400-500 DEG C, room temperature is cooled to the furnace after keeping the temperature 2h；Then pass to 0.5m3The air of/h is warming up to 380 DEG C with 0.8 DEG C/min After cool to room temperature with the furnace, then to be passed through the argon gas of flowing, be warming up to 900 DEG C with 17 DEG C/min, keep the temperature furnace cooling after 1h To room temperature；Silicon dioxide microsphere/carbon foam composite is made；
(6) it by silicon dioxide microsphere/carbon foam composite made from step (5), is cleaned with hydrogen fluoride, aperture ladder is made Spend the carbon foam of variation.
Carbon foam top obtained aperture is small, and lower part aperture is big, and density is 7.68 kg/m3, with a thickness of the thermally conductive system of 66.7mm Number is that 0.568 W/ (m K) can be used as lightweight aerospace heat-barrier material.
It above are only two specific embodiments of the invention, but the design concept of the present invention is not limited to this, all utilizations This design makes a non-material change to the present invention, and should belong to the behavior for invading the scope of protection of the invention.But it is all not It is detached from the content of technical solution of the present invention, it is to the above embodiments any type of simple according to the technical essence of the invention Modification, equivalent variations and remodeling, still fall within the protection scope of technical solution of the present invention.

Claims (1)

1. a kind of preparation method of the carbon foam of bore diameter gradient variation, includes the steps that following sequence:
(1) successively tile three layers of silicon dioxide microsphere in mold；Lower thickness is 10-30mm, and silicon dioxide microsphere diameter is 200-250 μm, intima-media thickness 20-50mm, silicon dioxide microsphere diameter is 200-150 μm, upper thickness 10-30mm, two Silica diameter is 100-150 μm；
(2) high softening-point asphalt is crushed, be ground to 15 μm hereinafter, then with the organic additive of 1-3wt%, 25- The water of 35wt% mixes, and forms uniformity slurry, and organic additive is binder, thickener and suspending agent；
(3) slurry in step (2) is added in mold along mold wall, slurry liquid level is higher than top layer's silica 1 0- 20mm；
(4) mold in step (3) is put into and is dried to obtain presoma in baking oven, presoma is demoulded and is taken out；
(5) presoma after the drying in step (4) is put into pyrolysis oven, is passed through the argon gas of flowing, with 1-5 DEG C/min heating To 400-500 DEG C, room temperature is cooled to the furnace after keeping the temperature 1-3h；Then pass to 0.5-1m3The air of/h, with 0.2-0.8 DEG C/min It cools to room temperature after being warming up to 300-400 DEG C with the furnace, then to be passed through the argon gas of flowing, 800- is warming up to 10-20 DEG C/min 1200 DEG C, room temperature is cooled to the furnace after keeping the temperature 1h；Silicon dioxide microsphere/carbon foam composite is made；
(6) it by silicon dioxide microsphere/carbon foam composite made from step (5), is cleaned with hydrogen fluoride, aperture ladder is made Spend the carbon foam of variation.
CN201810937819.9A 2018-08-17 2018-08-17 A kind of preparation method of the carbon foam of bore diameter gradient variation Pending CN109081704A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113264771A (en) * 2021-06-17 2021-08-17 兰州理工大学 Method for rapidly preparing high-strength carbon foam

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CN1544321A (en) * 2003-11-25 2004-11-10 复旦大学 Preparation method of carbon material with highly ordered nanometer hole of graphite hole wall structure
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CN105531241A (en) * 2013-09-20 2016-04-27 赫罗伊斯石英玻璃股份有限两合公司 Method for producing a porous carbon product

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Application publication date: 20181225