CN108840671A - The preparation method and product of silica heat-barrier material with Multi-scale model - Google Patents
The preparation method and product of silica heat-barrier material with Multi-scale model Download PDFInfo
- Publication number
- CN108840671A CN108840671A CN201810737891.7A CN201810737891A CN108840671A CN 108840671 A CN108840671 A CN 108840671A CN 201810737891 A CN201810737891 A CN 201810737891A CN 108840671 A CN108840671 A CN 108840671A
- Authority
- CN
- China
- Prior art keywords
- silica
- barrier material
- scale model
- preparation
- heat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- 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
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
-
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/636—Polysaccharides or derivatives thereof
- C04B35/6365—Cellulose or derivatives 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
The preparation method and product of the present invention relates to a kind of silica heat-barrier material with Multi-scale model, preparation method include：1) SiO 2 hollow microsphere and binder are dispersed in water, are made into mixed solution；2) mixed solution is placed in mold and carries out two-way frost；The bottom of the mold is silicon rubber block, and the contact surface of silicon rubber block and mixed solution is inclined-plane, and cold source is arranged in silicon rubber block lower part；3) two-way frost product is freeze-dried to remove solvent, obtains the silica with Multi-scale model/binder composite material；4) silica/binder composite material is subjected to high temperature sintering.The preparation method makes heat-barrier material form Multi-scale model, reduces its heat conduction efficiency.
Description
Technical field
The present invention relates to engineering heat-barrier material fields, and in particular to a kind of heat-insulated material of silica with Multi-scale model
The preparation method and product of material.
Background technique
Heat preserving and insulating material is a kind of energy-saving material that building energy consumption can be greatly decreased, and is to construct sustainable development society
Important means.Have benefited from the characteristic and some special structure designs, some inorganic material and organic material quilt of material itself
Heat-barrier material is made.Ideal heat-barrier material should take into account the characteristics such as heat-insulated, fire-retardant, lightweight, high-strength, environmental-friendly.With polyphenyl second
Alkene and polyurethane are the organic heat-barrier material of representative, have many advantages, such as low thermally conductive, lightweight, cheap, thus are to apply at this stage most
Extensive heat-barrier material, but its inflammable characteristic brings for its large-scale application cannot be neglected security risk.And have
The thermal insulation inorganic material of flame-retarding characteristic such as mineral wool etc., thermal insulation is poor, and is difficult to design by structure and promotes its thermal insulation.
Aerosil has the characteristics such as high-specific surface area, low-density and ultra-low thermal conductivity, is preferably to keep the temperature
Heat-barrier material.But pure silicon dioxide Mechanical Properties of Aerogels is poor, is difficult to use separately as heat-barrier material.It is industrial usual
Aerosil and other materials are used in combination, but often reduced with complex manufacturing technology, composite property, system
Make the problems such as cost height and is unable to get extensive use.
Chinese invention patent application (104609820 A of CN) discloses a kind of nanometer titanium dioxide of glass fibre orientation enhancing
Silicon heat-barrier material preparation method solidifies by using cryogenic freezing and realizes that glass fibre aligns in nano silica,
And then guarantee that the nano silica heat-barrier material of glass fibre orientation enhancing has high-intensitive and low heat conductivity characteristic.Due to
Using traditional orientation freezing method, it is only able to achieve arranging along orientation freezing direction for glass fibre, and titanium dioxide can not be made
Silicon forms lamellar orientation structure.
Chinese invention patent application (103896561 A of CN) disclose a kind of silica with regular layer structure every
Hot material preparation method, including orientation freezing step, drying steps, sintering step, orientation freezing step are by binder and two
Silicon oxide colloid mixed liquor injects in mold, makes the freezing interface of binder and silicon dioxide colloid mixed liquor from one end of mold
To the other end gradually directional solidification, the solidification products of binder Yu silicon dioxide colloid mixed liquor are obtained.Also due to using passing
The orientation freezing method of system, silica heat-barrier material can only be orientated along frost direction, and can not be perpendicular to frost side
It is orientated upwards.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of silica with Multi-scale model every
The preparation method of hot material reduces its heat conduction efficiency so that heat-barrier material forms Multi-scale model.
Technical solution provided by the present invention is：
A kind of preparation method of the silica heat-barrier material with Multi-scale model, includes the following steps：
1) SiO 2 hollow microsphere and binder are dispersed in water, are made into mixed solution；
2) mixed solution is placed in mold and carries out two-way frost；The bottom of the mold is silicon rubber block, silicon rubber
The contact surface of blob of viscose and mixed solution is inclined-plane, and cold source is arranged in silicon rubber block lower part；
3) two-way frost product is freeze-dried the silica that obtains that there is Multi-scale model to remove solvent/
Binder composite material；
4) silica/binder composite material is subjected to high temperature sintering.
The present invention prepares silica heat-barrier material using two-way freezing method, on the basis of tradition orients freezing method,
Mold bottom introducing thermal conductivity is poor and has the silicon rubber block of certain slope.In frost, due to having acclive silicon rubber
The presence of block is grown as shown in Figure 1, ice crystal is nucleated on one-dimensional straight line along two-dimensional surface, perpendicular to frost direction
Large area orientation texture is formed on section.As shown in Fig. 2, traditional orientation freezing method random nucleation on two-dimensional surface, along
Single temperature gradient growth causes to form multiple small range orientation areas on the section perpendicular to frost direction, can not obtain
To the lamellar orientation structure of large area, its practical application is seriously limited.
In addition, starting silica selects tiny balloon, cooperate two-way freezing method, so that silica heat-barrier material has
Multi-scale model.It is multiple dimensioned to be embodied in：Heat-barrier material is a kind of porous material on a macroscopic scale；It is heat-insulated on submillimeter scale
Material has the lamellar orientation structure of large area；On micro-meter scale, the lamellar structure of each orientation is by silicon dioxide hollow
Ball stacks.The special Multi-scale model, so that the heat conduction efficiency of silica heat-barrier material further decreases, thus
Improve the heat-proof quality of material.
Preferably, the diameter of the SiO 2 hollow microsphere is 5~20 μm.When diameter is too small, microballoon easily sinks；
When diameter is excessive, microballoon easily floats.Diameter is excessive or the too small stability that all will affect mixed solution.
Preferably, the density of the SiO 2 hollow microsphere is about 1~1.5g/cm3.Further preferably 1.1g/
cm3。
Preferably, volume fraction of the SiO 2 hollow microsphere in mixed solution is 15~25%.Concentration mistake
Hour, obtained porous silica material matter is crisp, easily collapses.When concentration is excessive, one side mixed solution is easily settled, another party
Face, ice crystal can not arrange excessive microballoon when two-way frost, so that piece interlayer has more connection, to influence thermal insulation
Energy.
Preferably, the mass ratio of the SiO 2 hollow microsphere and binder is 10~15:1.Binder content mistake
When few, the silicon dioxide microsphere in mixed solution is easily settled；When binder content is excessive, mixed solution viscosity is excessive, is unfavorable for
Form large area lamella orientation texture.
Preferably, the binder is hydroxypropyl cellulose, hydroxymethyl cellulose or polyvinyl alcohol.
Preferably, the gradient on the inclined-plane is 5~20 °.When the gradient is too small, the temperature gradient in horizontal direction is too small,
The structure of lamellar orientation can not be formed；When the gradient is excessive, the temperature gradient in horizontal direction is excessive, can not also form lamellar orientation
Structure.
Preferably, the silicon rubber block is wedge structure；Further preferably right angled triangle column, inclined-plane upward with it is mixed
Close solution contact.
Preferably, the temperature of the two-way frost reaction is -100~-60 DEG C.When temperature is too low, ice-crystal growth speed
Too fast, ice crystal, which has little time to form lamellar structure just to have frozen, to be finished；When the temperature is excessively high, ice-crystal growth speed is excessively slow, mixed solution
It is easily layered, leads to that ununiform shrinkage easily occurs when follow-up sintering, influence the orientation of lamellar structure to influence heat-proof quality.
Preferably, the high temperature sintering refers to 1~5 DEG C/min from room temperature to 500~700 DEG C, 500~
60~240min is kept the temperature at 700 DEG C.Sintering temperature is too low, and SiO 2 hollow microsphere surface is not melted, and sintered structure is easy
It collapses；Sintering temperature is excessively high, and SiO 2 hollow microsphere excessive surface melts, and causes volume contraction excessive, and thermal conductivity rises.
The silica with Multi-scale model that the present invention also provides a kind of to be prepared such as above-mentioned preparation method every
Hot material.Silica heat-barrier material prepared by the present invention has large area lamella orientation texture on perpendicular to frost direction,
Each layer is all stacked by SiO 2 hollow microsphere, forms unique Multi-scale model.
Compared with the existing technology, the beneficial effects of the present invention are embodied in：
(1) preparation method in the present invention can be by adjusting the conditions such as cryogenic temperature, mixed solution concentration, and preparing has
The silica heat-barrier material of different interlamellar spacings and microscopic appearance.
(2) the silica heat-barrier material being prepared in the present invention has preferable heat-proof quality, and tiny balloon makes
Heat conduction efficiency is reduced with the design with large area lamella orientation texture, to improve the heat-proof quality of material.
(3) preparation method of the invention is easy to operate, low in cost, environmental-friendly, is suitble to industry amplification application.
Detailed description of the invention
Fig. 1 is the schematic diagram that two-way freezing method forms orientation texture used in the embodiment of the present invention；
Fig. 2 is the schematic diagram that orientation freezing method traditional used in comparative example forms orientation texture；
Fig. 3 is the structural schematic diagram of two-way freezing device used in the present invention；
Fig. 4 is the SEM figure of the silica heat-barrier material with Multi-scale model prepared by embodiment 1；
Fig. 5 is the SEM figure of the silica heat-barrier material with Multi-scale model prepared by embodiment 2；
Fig. 6 is the SEM figure of the silica heat-barrier material with Multi-scale model prepared by embodiment 3；
Fig. 7 is the SEM figure of porous silica material prepared by comparative example 1；
Fig. 8 is the SEM figure of porous silica material prepared by comparative example 2.
Specific embodiment
Following embodiment further illustrates the contents of the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case where spirit of that invention and essence, to modification made by the method for the present invention, step or condition and replaces, belong to the present invention
Range.Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.
For two-way freezing device used in embodiment as shown in figure 3,1 be wherein cold ethanol, 2 be copper post, and 3 be copper sheet, 4
It is Teflon mould for silicon rubber block, 5,6 be mixed solution.
Wherein, 5 bottom of Teflon mould is silicon rubber block 4, and mixed solution 6, silicon is added in Teflon mould 5
The contact surface of rubber block 4 and mixed solution 6 is inclined-plane, and the gradient on inclined-plane is 5~20 °.Cold ethanol 1 is used as cold source, passes through copper
Column 2 and copper sheet 3 carry out heat transfer cooling.
Embodiment 1
(1) solution is prepared：6.6g SiO 2 hollow microsphere, 0.66g hydroxypropyl cellulose is taken to be scattered at room temperature
In 34mL deionized water, ball milling 12h or more makes it be uniformly dispersed, and more stable mixed solution is obtained after vacuum degassing bubble, wherein two
The content of silica tiny balloon is 15vol%.
(2) two-way frost：The mixed solution that step (1) obtains is placed in mold and carries out two-way frost, silicon rubber block
The gradient is 15 °, and cryogenic temperature is -90 DEG C.
(3) it is freeze-dried：The two-way frost product that step (2) is obtained is freeze-dried 36h or more at -60 DEG C, 10Pa
Sufficiently to remove solvent, the silica with Multi-scale model/hydroxypropyl cellulose composite material is obtained.
(4) high temperature sintering：The resulting composite material of step (3) is subjected to high temperature sintering, sintering procedure be with 3 DEG C/min from
Room temperature keeps the temperature 180min at 600 DEG C, is naturally cooling to room temperature to 600 DEG C.
(5) morphology characterization：The resulting silica heat-barrier material of step (4) carries out SEM characterization, and the face of characterization is titanium dioxide
Silicon heat-barrier material is perpendicular to the section for freezing direction, as shown in figure 4, silica heat-barrier material has on perpendicular to frost direction
There is large area lamella orientation texture, the lamella of orientation is stacked by SiO 2 hollow microsphere.
(6) material is tested, density 0.42g/cm3, thermal conductivity 42.0mW/mK, compressive strength is
1.5Mpa。
Embodiment 2
(1) solution is prepared：8.8g SiO 2 hollow microsphere, 0.88g hydroxypropyl cellulose is taken to be scattered at room temperature
In 32mL deionized water, ball milling 12h or more makes it be uniformly dispersed, and more stable mixed solution is obtained after vacuum degassing bubble, wherein two
The content of silica tiny balloon is 20vol%.
(2) two-way frost：The mixed solution that step (1) obtains is placed in mold and carries out two-way frost, silicon rubber block
The gradient is 15 °, and cryogenic temperature is -90 DEG C.
(3) it is freeze-dried：The two-way frost product that step (2) is obtained is freeze-dried 36h or more at -60 DEG C, 10Pa
Sufficiently to remove solvent, the silica with Multi-scale model/hydroxypropyl cellulose composite material is obtained.
(4) high temperature sintering：The resulting composite material of step (3) is subjected to high temperature sintering, sintering procedure be with 3 DEG C/min from
Room temperature keeps the temperature 180min at 600 DEG C, is naturally cooling to room temperature to 600 DEG C.
(5) morphology characterization：The resulting silica heat-barrier material of step (4) carries out SEM characterization, and the face of characterization is titanium dioxide
Silicon heat-barrier material is perpendicular to the section for freezing direction, as shown in figure 5, silica heat-barrier material has on perpendicular to frost direction
There is large area lamella orientation texture, the lamella of orientation is stacked by SiO 2 hollow microsphere.
(6) material is tested, density 0.52g/cm3, thermal conductivity 84.3mW/mK, compressive strength is
2.89Mpa。
Embodiment 3
(1) solution is prepared：11.0g SiO 2 hollow microsphere, 1.10g hydroxypropyl cellulose is taken to be scattered at room temperature
In 30mL deionized water, ball milling 12h or more makes it be uniformly dispersed, and more stable mixed solution is obtained after vacuum degassing bubble, wherein two
The content of silica tiny balloon is 25vol%.
(2) two-way frost：The mixed solution that step (1) obtains is placed in mold and carries out two-way frost, silicon rubber block
The gradient is 15 °, and cryogenic temperature is -90 DEG C.
(3) it is freeze-dried：The two-way frost product that step (2) is obtained is freeze-dried 36h or more at -60 DEG C, 10Pa
Sufficiently to remove solvent, the silica with Multi-scale model/hydroxypropyl cellulose composite material is obtained.
(4) high temperature sintering：The resulting composite material of step (3) is subjected to high temperature sintering, sintering procedure be with 3 DEG C/min from
Room temperature keeps the temperature 180min at 600 DEG C, is naturally cooling to room temperature to 600 DEG C.
(5) morphology characterization：The resulting silica heat-barrier material of step (4) carries out SEM characterization, and the face of characterization is titanium dioxide
Silicon heat-barrier material is perpendicular to the section for freezing direction, as shown in fig. 6, silica heat-barrier material has on perpendicular to frost direction
There is large area lamella orientation texture, the lamella of orientation is stacked by SiO 2 hollow microsphere.
(6) material is tested, density 0.61g/cm3, thermal conductivity 133.0mW/mK, compressive strength is
5.77Mpa。
Comparative example 1
(1) solution is prepared：6.6g SiO 2 hollow microsphere, 0.66g hydroxypropyl cellulose is taken to be scattered at room temperature
In 34mL deionized water, ball milling 12h or more makes it be uniformly dispersed, and more stable mixed solution is obtained after vacuum degassing bubble, wherein two
The content of silica tiny balloon is 15vol%.
(2) tradition orientation frost：The mixed solution that step (1) obtains is placed in the not mold of silicon rubber block and is determined
To frost, the gradient for being equivalent to silicon rubber block is 0 °, and cryogenic temperature is -90 DEG C.
(3) it is freeze-dried：The frost product that step (2) is obtained is freeze-dried 36h or more at -60 DEG C, 10Pa to fill
Divide removal solvent, obtains silica/hydroxypropyl cellulose composite material.
(4) high temperature sintering：The resulting composite material of step (3) is subjected to high temperature sintering, sintering procedure be with 3 DEG C/min from
Room temperature keeps the temperature 180min at 600 DEG C, is naturally cooling to room temperature to 600 DEG C.
(5) morphology characterization：The resulting porous silica material of step (4) carries out SEM characterization, and the face of characterization is titanium dioxide
Silicon porous material is perpendicular to the section for freezing direction, as shown in fig. 7, illustrating be prepared using traditional orientation freezing method two
Silica porous material does not have lamellar orientation structure on perpendicular to frost direction.
(6) material is tested, density 0.46g/cm3, thermal conductivity 87.2mW/mK, compressive strength is
0.97Mpa.By, it is found that under equal densities, designing large area lamellar orientation knot with the thermal conductivity data comparison in embodiment 1
Structure is conducive to improve the heat-proof quality of porous silica material.
Comparative example 2
(1) solution is prepared：Taking 13.2g silica solid microsphere, (diameter is close with tiny balloon, density 2.2g/cm3)、
1.32g hydroxypropyl cellulose is scattered at room temperature in 34mL deionized water, and ball milling 12h or more makes it be uniformly dispersed, and vacuum is removed
More stable mixed solution is obtained after bubble, wherein the content of silica solid microsphere is 15vol%.
(2) tradition orientation frost：The mixed solution that step (1) obtains is placed in the not mold of silicon rubber block and is determined
To frost, the gradient for being equivalent to silicon rubber block is 0 °, and cryogenic temperature is -90 DEG C.
(3) it is freeze-dried：The frost product that step (2) is obtained is freeze-dried 36h or more at -60 DEG C, 10Pa to fill
Divide removal solvent, obtains silica/hydroxypropyl cellulose composite material.
(4) high temperature sintering：The resulting composite material of step (3) is subjected to high temperature sintering, sintering procedure be with 3 DEG C/min from
Room temperature keeps the temperature 120min at 1200 DEG C, is naturally cooling to room temperature to 1200 DEG C.
(5) morphology characterization：The resulting porous silica material of step (4) carries out SEM characterization, and the face of characterization is titanium dioxide
Silicon heat-barrier material is perpendicular to the section for freezing direction, as shown in figure 8, illustrating be prepared using traditional orientation freezing method two
Silica porous material does not have lamellar orientation structure on perpendicular to frost direction.
(6) material is tested, density 0.45g/cm3, thermal conductivity 105.6mW/mK, compressive strength is
1.34Mpa.By comparing with the thermal conductivity data in comparative example 1 it is found that under equal densities, be conducive to mention using tiny balloon
The heat-proof quality of high silicon dioxide porous material.
Claims (9)
1. a kind of preparation method of the silica heat-barrier material with Multi-scale model, which is characterized in that include the following steps：
1) SiO 2 hollow microsphere and binder are dispersed in water, are made into mixed solution；
2) mixed solution is placed in mold and carries out two-way frost；The bottom of the mold is silicon rubber block, silicon rubber block
Contact surface with mixed solution is inclined-plane, and cold source is arranged in silicon rubber block lower part；
3) two-way frost product is freeze-dried to remove solvent, obtains the silica/bonding with Multi-scale model
Agent composite material；
4) silica/binder composite material is subjected to high temperature sintering.
2. the preparation method of the silica heat-barrier material according to claim 1 with Multi-scale model, feature exist
In the diameter of the SiO 2 hollow microsphere is 5~20 μm.
3. the preparation method of the silica heat-barrier material according to claim 1 with Multi-scale model, feature exist
In volume fraction of the SiO 2 hollow microsphere in mixed solution is 15~25%.
4. the preparation method of the silica heat-barrier material according to claim 1 with Multi-scale model, feature exist
In the mass ratio of the SiO 2 hollow microsphere and binder is 10~15:1.
5. the preparation method of the silica heat-barrier material according to claim 1 with Multi-scale model, feature exist
In the binder is hydroxypropyl cellulose, hydroxymethyl cellulose or polyvinyl alcohol.
6. the preparation method of the silica heat-barrier material according to claim 1 with Multi-scale model, feature exist
In the gradient on the inclined-plane is 5~20 °.
7. the preparation method of the silica heat-barrier material according to claim 1 with Multi-scale model, feature exist
In the temperature of the two-way frost is -100~-60 DEG C.
8. the preparation method of the silica heat-barrier material according to claim 1 with Multi-scale model, feature exist
In, the high temperature sintering refers to 1~5 DEG C/min from room temperature to 500~700 DEG C, at 500~700 DEG C keep the temperature 60~
240min。
9. a kind of silica with Multi-scale model that the preparation method as described in claim 1~8 is any is prepared
Heat-barrier material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810737891.7A CN108840671A (en) | 2018-07-06 | 2018-07-06 | The preparation method and product of silica heat-barrier material with Multi-scale model |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810737891.7A CN108840671A (en) | 2018-07-06 | 2018-07-06 | The preparation method and product of silica heat-barrier material with Multi-scale model |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108840671A true CN108840671A (en) | 2018-11-20 |
Family
ID=64201363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810737891.7A Pending CN108840671A (en) | 2018-07-06 | 2018-07-06 | The preparation method and product of silica heat-barrier material with Multi-scale model |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108840671A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111234502A (en) * | 2020-03-31 | 2020-06-05 | 南京理工大学 | Efficient and uniform heat conduction polymer-based heat conduction material and preparation method thereof |
| CN113956063A (en) * | 2021-10-26 | 2022-01-21 | 浙江大学 | Preparation method of porous material with long-range oriented structure or complex structure |
| WO2022204866A1 (en) * | 2021-03-29 | 2022-10-06 | 中国科学院深圳先进技术研究院 | Aerogel with double-orientation network, preparation method therefor and use thereof |
| CN115572407A (en) * | 2022-09-09 | 2023-01-06 | 天津科技大学 | Aramid nanofiber-based composite aerogel and preparation method and application thereof |
| CN117185793A (en) * | 2023-11-08 | 2023-12-08 | 天津南极星隔热材料有限公司 | Preparation method of mullite nanofiber-based porous ceramic with pine-like structure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896561A (en) * | 2014-03-06 | 2014-07-02 | 大连理工大学 | Preparation method of silicon dioxide thermal insulation material with regular layered structure |
| CN105692598A (en) * | 2016-01-22 | 2016-06-22 | 浙江大学 | Preparation method of lamellar porous graphene oxide and product of preparation method |
-
2018
- 2018-07-06 CN CN201810737891.7A patent/CN108840671A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896561A (en) * | 2014-03-06 | 2014-07-02 | 大连理工大学 | Preparation method of silicon dioxide thermal insulation material with regular layered structure |
| CN105692598A (en) * | 2016-01-22 | 2016-06-22 | 浙江大学 | Preparation method of lamellar porous graphene oxide and product of preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 梁基照: "《高分子复合材料传热学导论》", 31 March 2013, 华南理工大学出版社 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111234502A (en) * | 2020-03-31 | 2020-06-05 | 南京理工大学 | Efficient and uniform heat conduction polymer-based heat conduction material and preparation method thereof |
| WO2022204866A1 (en) * | 2021-03-29 | 2022-10-06 | 中国科学院深圳先进技术研究院 | Aerogel with double-orientation network, preparation method therefor and use thereof |
| CN113956063A (en) * | 2021-10-26 | 2022-01-21 | 浙江大学 | Preparation method of porous material with long-range oriented structure or complex structure |
| CN115572407A (en) * | 2022-09-09 | 2023-01-06 | 天津科技大学 | Aramid nanofiber-based composite aerogel and preparation method and application thereof |
| CN115572407B (en) * | 2022-09-09 | 2023-08-08 | 天津科技大学 | Aramid nanofiber-based composite aerogel and preparation method and application thereof |
| CN117185793A (en) * | 2023-11-08 | 2023-12-08 | 天津南极星隔热材料有限公司 | Preparation method of mullite nanofiber-based porous ceramic with pine-like structure |
| CN117185793B (en) * | 2023-11-08 | 2024-01-02 | 天津南极星隔热材料有限公司 | Preparation method of mullite nanofiber-based porous ceramic with pine-like structure |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108840671A (en) | The preparation method and product of silica heat-barrier material with Multi-scale model | |
| CN103319678B (en) | Solar water heater water tank polyurethane hard foam lagging material | |
| CN114524638B (en) | Ultralow-thermal-conductivity nanofiber aerogel composite material and preparation method thereof | |
| CN103304252B (en) | Preparation method of SiO2 aerogel/porous Si3N4 composite material | |
| CN105198375A (en) | Thermal insulation silicon dioxide aerogel/hydroxylation glass fiber felt composite and preparation method thereof | |
| CN105692598B (en) | A kind of preparation method of lamella porous oxidation graphene and products thereof | |
| CN101955350A (en) | Modified aluminum oxide aerogel composite material and preparation method thereof | |
| Ye et al. | Microstructure characterization and thermal performance of reticulated SiC skeleton reinforced silica aerogel composites | |
| CN102992333B (en) | Low-cost method for preparing aerosil | |
| CN104086150A (en) | Heat-insulated aerogel material for building and preparation method of heat-insulated aerogel material | |
| CN106892674A (en) | A kind of method for preparing gradient orienting stephanoporate cement based on two-phase pore creating material system freezing molding techniques | |
| CN104478475B (en) | A kind of high temperature resistance and high strength SiC carbon coated foam composite heat-insulated material and its preparation method | |
| CN113046030A (en) | Preparation method of delignified balsawood/phase-change composite material | |
| CN102964055B (en) | Ultra-fast preparation method for highly transparent aerogel glass | |
| CN103302861B (en) | Preparation method of polymethyl methacrylate based cell gradient material | |
| CN106084274B (en) | A kind of preparation method of light high-strength heat preservation foamed composite | |
| CN105110779B (en) | It is a kind of to weld the method that whisker prepares mullite porous ceramic | |
| CN109482882A (en) | Foam metal and preparation method thereof with microcosmic orientation pore structure | |
| CN110437469B (en) | High polymer material with micro-bending layered structure and preparation method and application thereof | |
| CN103738970B (en) | High transmittance nano-porous aerogel material and preparation method thereof | |
| CN113929488A (en) | Lithium ceramic tritium propagation agent with curved pore path structure and preparation method thereof | |
| CN109650843B (en) | Is made of amorphous SiO2Flexible silicon dioxide aerogel constructed by microtubes and preparation method thereof | |
| CN102531663B (en) | Porous silica ceramic with double layers of pores and preparation method thereof | |
| CN106587646B (en) | Preparation method of nanoporous glass and nanoporous glass | |
| CN114163681A (en) | Preparation method of silicon carbide reinforced chitosan foam thermal insulation material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181120 |
|
| RJ01 | Rejection of invention patent application after publication |