CN108610086A - A kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material - Google Patents
A kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material Download PDFInfo
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Abstract
A kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material, it is related to a kind of preparation method of porous fibre matter heat-barrier material.The present invention is to solve be unable to control green density when existing freezing injection molding prepares porous material.The present invention：One, the length of chopped strand；Two, slurry is prepared；Three, it stands to be combined with Pressure water discharging and prepares the green compact of different densities；Four, the freezing and drying of slurry；Five, the heat treatment of green compact.The method being combined with pressure pipe Pressure water discharging using standing in the step three of the present invention, depth by controlling pressure pipe press-in die is to obtain the green compact of different densities by controlling the volume of green compact in mold, eventually by performance characterization, the relationship between preparation process and performance is established, realizes low to density, the small sample of thermal coefficient preparation.
Description
Technical field
The present invention relates to a kind of preparation methods of porous fibre matter heat-barrier material.
Background technology
Recently as the rapid development of aerospace and energy technology, high temperature insulating material has received widespread attention.
Porous fibre material is because of its good high-temperature stability, lower thermal conductivity, low elastic modulus and well resists the characteristics such as thermal shock resistance,
It has a good application prospect in high temperature insulating material etc..Porous fibre material be by the chopped strand that stacks at random and
Adhesives on fiber crossovers node form, and then form stable three-dimensional net structure, have high porosity, low close
Degree, the high feature of temperature tolerance promise to be the heat-barrier material used in Aeronautics and Astronautics, the energy and the fields such as civilian.
There are many preparation methods of porous fibre material.The preparation generally use vacuum filtration system of traditional fibre material
Standby, this method is efficient, economy, high porosity sample may be implemented, but since the pressure of vacuum pump is difficult to control, may lead to fibre
Frame is undesirable collapses for dimension, the uneven distribution of binder, and it is uneven finally to often result in fiber overlap joint, and then is difficult to control
The density and intensity of material.In past two ten years, freezing injection molding, which has become, a kind of new prepares porous fibre matter
The forming method of material, and quick development has been obtained, this method is conducive to keep three-dimensional scatter and has higher porosity
And intensity.Freezing injection molding mostly uses when preparing porous material slurry standing a period of time, after slurry sedimentation, draws upper layer
After extra slurry solution, by lower slurry freezing and freeze-dried rear acquisition green compact.The problem of this method, is, due to only leaning on slurry
Itself precipitation maintains the content of fiber in green body, and cannot control the uniformity of slurry sediment, therefore can not accomplish close to green compact
The control of degree, to can not achieve relatively accurately controlling to final sample density.
Invention content
The present invention is to solve the technologies that green density is unable to control when existing freezing injection molding prepares porous material to ask
Topic, and a kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material is provided.
The preparation method of the three-dimensional network shape porous fibre matter heat-barrier material of the present invention carries out according to the following steps：
One, the length of chopped strand：
Polycrystalline mullite fibre often contains certain slag ball in process of production, and the presence of slag ball is unfavorable for mullite fiber
The structure of three-dimensional net structure.The slagging-off of the present invention is carried out in two steps, the first step：Utilize the difference of slag spherical shape shape and fiber shape
Not, slag ball is the smaller graininess of diameter, and fiber is cylindric compared with big L/D ratio, in the sieve Zhong Zha clubs of certain size
Fiber will not spill slagging-off by sieve pore leaks out；Second step：Using the difference of slag ball density and fibre density, using sedimentation
Method removes the gred, due to big, the detaching soon than fiber sedimentation in water of the density ratio fiber of slag ball；
Dispersibility directly depends on the length of chopped strand to polycrystalline mullite fibre chopped strand in a dispersion medium, reason
Length by upper fiber is shorter, and fiber is less susceptible to mutually tangle into fibrous nodules in a dispersion medium, the slurry of preparation it is uniform
Property is also better, but fibre length is too short, fiber mutually overlap in a dispersion medium less than, do not constitute three-dimensional net structure, and
Form close-packed structure so that density of material is excessive, heat-proof quality can be caused to decline；Therefore it is necessary to select the short of appropriate length
Cut fiber；
1., first with scissors or fiber shearing machine polycrystalline mullite fibre is cut short as chopped strand, cross 40 mesh sieve, repeatedly
It is screened to until being sifted out there is no slag ball；The length of the chopped strand be 0.5mm~3mm, a diameter of 3 μm~10 μm；
2., the fiber of excessively complete sieve by step 1. be put into soy bean milk making machine, add water to carry out the 10min~15min that is chopped, soy bean milk making machine
Rotating speed be 10000r/min~11000r/min；The fiber of the excessively complete sieve of the step 1. and the mass ratio of water are 1:(100
~150)；
3., be chopped after, by step 2. in entire mixture in soy bean milk making machine pour into a container, stand 20s~
Then the fiber on upper layer is poured out and is retained by 60s, the slag ball of bottom removes；
4., repeat the operation four times~five times of step 3. and remove scaling-off ball, removed water, obtained with the fiber on filtered through gauze upper layer
Fiber to after being chopped；
Two, slurry is prepared：
Fiber 4. step 1 is chopped after is all distributed in deionized water, and dispersant and bonding agent is then added, stirs
30min~40min is mixed, slurry is obtained；The quality of the step 1 1. fiber of excessively complete sieve is the quality of deionized water in step 2
3%~5%；The quality of dispersant described in step 2 is 0.2%~0.4% of the quality of deionized water in step 2；Step
The quality of bonding agent described in rapid two is 5%~10% of the quality of deionized water in step 2；
Three, it stands to be combined with Pressure water discharging and prepares the green compact of different densities：Slurry is poured into mold, 10min is stood
One end of pressure pipe and side wall are wrapped up gauze, pressure pipe are enclosed in one end press-in die of gauze, in slurry by~20min
Water is poured out by pressure pipe inner inclination, and pressurize 30s~60s obtains green compact；The mold is open at one end, and one end is closed
Pipe；The pressure pipe is the pipe of open at both ends；
Four, the freezing and drying of slurry：Mold is put into refrigerator, under conditions of temperature is subzero 15~subzero 25 DEG C
It is refrigerated to slurry to freeze completely, then mold is put into freeze drier, be with vacuum degree at subzero 40 DEG C~subzero 60 DEG C
48h~100h, demoulding are freeze-dried under conditions of 80Pa~200Pa；
Five, the heat treatment of green compact：Green compact after step 4 is demoulded are put into Muffle furnace, in air atmosphere by room temperature with
The heating rate of 5 DEG C/min is warming up to 1200 DEG C~1250 DEG C, and 3h is kept the temperature at 1200 DEG C~1250 DEG C, and then furnace cooling obtains
To three-dimensional network shape porous fibre matter heat-barrier material.
Using the method being combined with pressure pipe Pressure water discharging is stood in the step three of the present invention, mould is pressed by controlling pressure pipe
The depth of tool is to control the volume of green compact in mold and then obtain the green compact of different densities, eventually by performance characterization, establishes system
Relationship between standby process and performance, realizes low to density, the small sample of thermal coefficient preparation.
Present invention process process is simple, inexpensively prepares low-density (0.056g/cm3~0.102g/cm3), low-heat leads
The porous fibre matter heat-barrier material of rate 0.032W/ (mK)~0.040W/ (mK), 96% or more high porosity.
The present invention drain and freezes the method that is combined of injection molding by pressurizeing, and manufactures the three of a kind of low-density and lower thermal conductivity
Network-like porous fibre matter heat-barrier material is tieed up, in the process, binder shifts fiber surface onto by ice crystal, and fibre is bonded in after sintering
Lap-joint is tieed up, the stabilization three-dimensional net structure being made of fiber is formed.
Description of the drawings
The heat-insulated material of three-dimensional network shape porous fibre matter of the sample preparation of green compact number a in the step of Fig. 1 is experiment one three
The SEM of material schemes；
The heat-insulated material of three-dimensional network shape porous fibre matter of the sample preparation of green compact number b in the step of Fig. 2 is experiment one three
The SEM of material schemes；
The heat-insulated material of three-dimensional network shape porous fibre matter of the sample preparation of green compact number c in the step of Fig. 3 is experiment one three
The SEM of material schemes；
The heat-insulated material of three-dimensional network shape porous fibre matter of the sample preparation of green compact number d in the step of Fig. 4 is experiment one three
The SEM of material schemes；
The heat-insulated material of three-dimensional network shape porous fibre matter of the sample preparation of green compact number a in the step of Fig. 5 is experiment one three
The SEM of material schemes；
The heat-insulated material of three-dimensional network shape porous fibre matter of the preparation of the green compact of different densities in the step of Fig. 6 is experiment one three
The thermal conductivity figure of material；
The heat-insulated material of three-dimensional network shape porous fibre matter of the preparation of the green compact of different densities in the step of Fig. 7 is experiment one three
The porosity figure of material.
Specific implementation mode
Specific implementation mode one：Present embodiment is a kind of preparation side of three-dimensional network shape porous fibre matter heat-barrier material
Method specifically carries out according to the following steps：
One, the length of chopped strand：
1., first with scissors or fiber shearing machine polycrystalline mullite fibre is cut short as chopped strand, cross 40 mesh sieve, repeatedly
It is screened to until being sifted out there is no slag ball；The length of the chopped strand be 0.5mm~3mm, a diameter of 3 μm~10 μm；
2., the fiber of excessively complete sieve by step 1. be put into soy bean milk making machine, add water to carry out the 10min~15min that is chopped, soy bean milk making machine
Rotating speed be 10000r/min~11000r/min；The fiber of the excessively complete sieve of the step 1. and the mass ratio of water are 1:(100
~150)；
3., be chopped after, by step 2. in entire mixture in soy bean milk making machine pour into a container, stand 20s~
Then the fiber on upper layer is poured out and is retained by 60s, the slag ball of bottom removes；
4., repeat the operation four times~five times of step 3. and remove scaling-off ball, removed water, obtained with the fiber on filtered through gauze upper layer
Fiber to after being chopped；
Two, slurry is prepared：
Fiber 4. step 1 is chopped after is all distributed in deionized water, and dispersant and bonding agent is then added, stirs
30min~40min is mixed, slurry is obtained；The quality of the step 1 1. fiber of excessively complete sieve is the quality of deionized water in step 2
3%~5%；The quality of dispersant described in step 2 is 0.20%~0.40% of the quality of deionized water in step 2；
The quality of bonding agent described in step 2 is 5%~10% of the quality of deionized water in step 2；
Three, it stands to be combined with Pressure water discharging and prepares the green compact of different densities：Slurry is poured into mold, 10min is stood
One end of pressure pipe and side wall are wrapped up gauze, pressure pipe are enclosed in one end press-in die of gauze, in slurry by~20min
Water is poured out by pressure pipe inner inclination, and pressurize 30s~60s obtains green compact；The mold is open at one end, and one end is closed
Pipe；The pressure pipe is the pipe of open at both ends；
Four, the freezing and drying of slurry：Mold is put into refrigerator, under conditions of temperature is subzero 15~subzero 25 DEG C
It is refrigerated to slurry to freeze completely, then mold is put into freeze drier, be with vacuum degree at subzero 40 DEG C~subzero 60 DEG C
48h~100h, demoulding are freeze-dried under conditions of 80Pa~200Pa；
Five, the heat treatment of green compact：Green compact after step 4 is demoulded are put into Muffle furnace, in air atmosphere by room temperature with
The heating rate of 5 DEG C/min is warming up to 1200 DEG C~1250 DEG C, and 3h is kept the temperature at 1200 DEG C~1250 DEG C, and then furnace cooling obtains
To three-dimensional network shape porous fibre matter heat-barrier material.
Specific implementation mode two：The present embodiment is different from the first embodiment in that：Dispersion described in step 2
Agent is neopelex.Other are same as the specific embodiment one.
Specific implementation mode three：The present embodiment is different from the first and the second embodiment in that：Described in step 2
Bonding agent is Ludox, and specific preparation method is：Ethyl orthosilicate is poured into container first, absolute ethyl alcohol is added, then
Deionized water is added and forms mixed liquor, mixed liquor is put into heat preservation 10min~30min in 40 DEG C of water-bath, it is water-soluble to instill hydrochloric acid
Liquid keeps the temperature 1h in 40 DEG C of water-bath, obtains Ludox；A concentration of 0.2mol/L of the aqueous hydrochloric acid solution；It is described just
The molar ratio of silester and deionized water is 1:4；The molar ratio of the ethyl orthosilicate and absolute ethyl alcohol is 1:(4~8)；
The molar ratio of hydrogen chloride in the ethyl orthosilicate and aqueous hydrochloric acid solution is 1:(7.5×10-4~15 × 10-4).Other with
Specific implementation mode one or two is identical.
Specific implementation mode four：Unlike one of present embodiment and specific implementation mode one to three：Institute in step 3
The gauze stated is 300 mesh.Other are identical as one of specific implementation mode one to three.
Specific implementation mode five：Unlike one of present embodiment and specific implementation mode one to four：Institute in step 3
The internal diameter for the mold stated is 30mm, volume 50mL；The internal diameter of pressure pipe described in step 3 is 22mm, outer diameter 26mm.Its
He is identical as one of specific implementation mode one to four.
The present invention is verified with following tests：
Experiment one：This experiment be a kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material, specifically press with
What lower step carried out：
One, the length of chopped strand：
1., first with scissors polycrystalline mullite fibre is cut short as chopped strand, cross 40 mesh sieve, be screened to repeatedly there is no
Until slag ball sifts out；The length of the chopped dimension be 1mm~3mm, a diameter of 3 μm~10 μm；
2., the fiber of excessively complete sieve by step 1. be put into soy bean milk making machine, add water to carry out the 10min that is chopped, the rotating speed of soy bean milk making machine
For 10000r/min；The fiber of the excessively complete sieve of the step 1. and the mass ratio of water are 1:100；
3., be chopped after, by step 2. in entire mixture in soy bean milk making machine pour into a beaker, stand 20s, then
The fiber on upper layer is poured out and retained, the slag ball of bottom removes；
4., repeat the operation four times~five times of step 3. and remove scaling-off ball, removed water, obtained with the fiber on filtered through gauze upper layer
Fiber to after being chopped；
Two, slurry is prepared：
Fiber 4. step 1 is chopped after is all distributed in deionized water, and dispersant and bonding agent is then added, stirs
30min is mixed, slurry is obtained；Step 1 1. the fiber of excessively complete sieve quality be step 2 in deionized water quality 3%；Step
The quality of dispersant described in two is 0.24% of the quality of deionized water in step 2；Bonding agent described in step 2
Quality is 5% of the quality of deionized water in step 2；
Three, it stands to be combined with Pressure water discharging and prepares the green compact of different densities：Slurry is poured into mold, 10min is stood,
Gauze is wrapped up into one end of pressure pipe and side wall, pressure pipe is enclosed in one end press-in die of gauze, the water in slurry passes through pressure
Pipe inner inclination is poured out, and pressurize 30s obtains green compact；The mold is open at one end, the closed pipe in one end；The pressure
Pipe is the pipe of open at both ends；
Four, the freezing and drying of slurry：Mold is put into refrigerator, freezes 6h under conditions of temperature is subzero 18, so
Mold is put into freeze drier afterwards, 72h is freeze-dried under conditions of subzero 60 DEG C and vacuum degree are 200Pa, demoulds；
Five, the heat treatment of green compact：Green compact after step 4 is demoulded are put into Muffle furnace, in air atmosphere by room temperature with
The heating rate of 5 DEG C/min is warming up to 1200 DEG C, and 3h is kept the temperature at 1200 DEG C, and it is porous to obtain three-dimensional network shape for then furnace cooling
Cellulosic heat-barrier material；
Dispersant described in step 2 is neopelex；
Bonding agent described in step 2 is Ludox, and specific preparation method is：Ethyl orthosilicate is poured into burning first
In cup, absolute ethyl alcohol is added, deionized water is then added and forms mixed liquor, mixed liquor is put into 40 DEG C of water-bath and is kept the temperature
10min instills aqueous hydrochloric acid solution, keeps the temperature 1h in 40 DEG C of water-bath, obtain Ludox；The aqueous hydrochloric acid solution it is a concentration of
0.2mol/L；The molar ratio of the ethyl orthosilicate and deionized water is 1:4；The ethyl orthosilicate and absolute ethyl alcohol
Molar ratio is 1:4；The molar ratio of hydrogen chloride in the ethyl orthosilicate and aqueous hydrochloric acid solution is 1:7.5×10-4；
Gauze described in step 3 is 300 mesh；
The internal diameter of mold described in step 3 is 30mm, volume 50mL；The internal diameter of pressure pipe described in step 3 is
22mm, outer diameter 26mm.
In the step of this experiment three green compact in mold are controlled by controlling 4 different depth in pressure pipe press-in die
Volume obtains 4 porous fibre matter heat-barrier materials of different densities in turn, and calculates its density, specific such as table 1：
Table 1
The heat-insulated material of three-dimensional network shape porous fibre matter of the sample preparation of green compact number a in the step of Fig. 1 is experiment one three
The SEM of material schemes, and can be clearly seen that fiber mutually overlaps and forms network-like skeleton structure, Hole is more, therefore has
Higher porosity (98.23%).
The heat-insulated material of three-dimensional network shape porous fibre matter of the sample preparation of green compact number b in the step of Fig. 2 is experiment one three
The three-dimensional network shape porous fibre matter of the sample preparation of green compact number c is heat-insulated in the step of SEM of material schemes, and Fig. 3 is experiment one three
In the step of SEM of material schemes, and Fig. 4 be experiment one three the three-dimensional network shape porous fibre matter of the sample preparation of green compact number d every
The SEM of hot material schemes, it can be seen that with being continuously increased for sample rate, is filled out by more fibers and Ludox between hole
It fills, hole tapers into, and to make the aperture of sample be gradually reduced, porosity also reduces therewith.It can be clearly from figure
To fiber lap-joint it is bonded together by the binder melted, with the increase of density, fibre three-dimensional is network-like in sample
Overlap joint skeleton structure can increase, and fiber tends to closer overlapping mode.
The heat-insulated material of three-dimensional network shape porous fibre matter of the sample preparation of green compact number a in the step of Fig. 5 is experiment one three
The SEM of material schemes, and region A is adhesive silicon sol.
The heat-insulated material of three-dimensional network shape porous fibre matter of the preparation of the green compact of different densities in the step of Fig. 6 is experiment one three
The thermal conductivity figure of material, 1 is green compact a, and 2 be green compact b, and 3 be green compact c, and 4 be green compact d, as can be seen from Figure, with the increasing of density
Add, the thermal coefficient of sample increases to 0.040W/ (mK) from 0.032W/ (mK).Its reason is analyzed, this is because density increases
Adding makes fiber overlap joint tend to compact reactor cumuliformis, and to make sample interior stomata reduce, pore size reduces so that the hole of sample
Rate reduces, and with the reduction of sample porosity, gas phase heat transfer reduces, and the thermal coefficient of sample also increases.This experiment
The small raising of middle sample thermal coefficient, it is corresponding with small reduction (98.23%~96.77%) of sample porosity.Specifically
The scale for weighing heat-proof quality is the thermal coefficient of material, and the size of thermal coefficient reflects the quality of material heat-proof quality.It should
The low thermal coefficient of sample shows that it is a kind of preferable heat-barrier material.
The heat-insulated material of three-dimensional network shape porous fibre matter of the preparation of the green compact of different densities in the step of Fig. 7 is experiment one three
The porosity figure of material, 1 is green compact a, and 2 be green compact b, and 3 be green compact c, and 4 be green compact d, it can be seen from the figure that porous fibre material
The porosity change rule of material is more apparent, and with the increase of density, porosity is gradually reduced.This is because as sample is close
The increase of degree, gradually overlap joint is close between fiber, and the microstructure of sample is gradually densified, and causes porosity that reduction trend is presented.
From the point of view of porosity, the porosity of sample illustrates that this experiment is based on freezing injection molding all 96% or more, close by controlling sample
Degree in a certain range, can prepare the higher porous fibre material of porosity.
Claims (5)
1. a kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material, it is characterised in that three-dimensional network shape porous fibre
The preparation method of matter heat-barrier material carries out according to the following steps：
One, the length of chopped strand：
1., first with scissors or fiber shearing machine polycrystalline mullite fibre is cut short as chopped strand, cross 40 mesh sieve, be sieved repeatedly
Until being sifted out there is no slag ball；The length of the chopped strand be 0.5mm~3mm, a diameter of 3 μm~10 μm；
2., the fiber of excessively complete sieve by step 1. be put into soy bean milk making machine, add water to carry out the 10min~15min that is chopped, soy bean milk making machine turns
Speed is 10000r/min~11000r/min；The fiber of the excessively complete sieve of the step 1. and the mass ratio of water are 1:(100~
150)；
3., be chopped after, by step 2. in entire mixture in soy bean milk making machine pour into a container, stand 20s~60s, so
The fiber on upper layer is poured out and retained afterwards, the slag ball of bottom removes；
4., repeat the operation four times~five times of step 3. and remove scaling-off ball, removed water, obtained short with the fiber on filtered through gauze upper layer
Fiber after cutting；
Two, slurry is prepared：
Fiber 4. step 1 is chopped after is all distributed in deionized water, and dispersant and bonding agent, stirring is then added
30min~40min obtains slurry；Step 1 1. the fiber of excessively complete sieve quality be step 2 in deionized water quality 3%
~5%；The quality of dispersant described in step 2 is 0.20%~0.40% of the quality of deionized water in step 2；Step
The quality of bonding agent described in two is 5%~10% of the quality of deionized water in step 2；
Three, it stands to be combined with Pressure water discharging and prepares the green compact of different densities：Slurry is poured into mold, standing 10min~
One end of pressure pipe and side wall are wrapped up gauze, pressure pipe are enclosed in one end press-in die of gauze, the water in slurry by 20min
It is poured out by pressure pipe inner inclination, pressurize 30s~60s obtains green compact；The mold is open at one end, the closed circle in one end
Pipe；The pressure pipe is the pipe of open at both ends；
Four, the freezing and drying of slurry：Mold is put into refrigerator, is freezed under conditions of temperature is subzero 15~subzero 25 DEG C
Freeze to slurry, mold be put into freeze drier completely then, subzero 40 DEG C~subzero 60 DEG C and vacuum degree be 80Pa
48h~100h, demoulding are freeze-dried under conditions of~200Pa；
Five, the heat treatment of green compact：Green compact after step 4 is demoulded are put into Muffle furnace, in air atmosphere by room temperature with 5 DEG C/
The heating rate of min is warming up to 1200 DEG C~1250 DEG C, and 3h is kept the temperature at 1200 DEG C~1250 DEG C, and then furnace cooling obtains three
Tie up network-like porous fibre matter heat-barrier material.
2. a kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material according to claim 1, feature exist
Dispersant described in step 2 is neopelex.
3. a kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material according to claim 1, feature exist
Bonding agent described in step 2 is Ludox, and specific preparation method is：Ethyl orthosilicate is poured into container first, is added
Enter absolute ethyl alcohol, then be added deionized water formed mixed liquor, by mixed liquor be put into 40 DEG C of water-bath keep the temperature 10min~
30min instills aqueous hydrochloric acid solution, keeps the temperature 1h in 40 DEG C of water-bath, obtain Ludox；The aqueous hydrochloric acid solution it is a concentration of
0.2mol/L；The molar ratio of the ethyl orthosilicate and deionized water is 1:4；The ethyl orthosilicate and absolute ethyl alcohol
Molar ratio is 1:(4~8)；The molar ratio of hydrogen chloride in the ethyl orthosilicate and aqueous hydrochloric acid solution is 1:(7.5×10-4
~15 × 10-4)。
4. a kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material according to claim 1, feature exist
Gauze described in step 3 is the gauze of 300 mesh.
5. a kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material according to claim 1, feature exist
The internal diameter of mold described in step 3 is 30mm, volume 50mL；The internal diameter of pressure pipe described in step 3 is 22mm, outside
Diameter is 26mm.
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