CN105837252B - porous alumina ceramic and preparation method thereof - Google Patents
porous alumina ceramic and preparation method thereof Download PDFInfo
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- CN105837252B CN105837252B CN201510392366.2A CN201510392366A CN105837252B CN 105837252 B CN105837252 B CN 105837252B CN 201510392366 A CN201510392366 A CN 201510392366A CN 105837252 B CN105837252 B CN 105837252B
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Abstract
The present invention relates to a kind of porous alumina ceramics and preparation method thereof.Wherein, according to mass percentage, the raw material of the porous alumina ceramic includes following component:40%~60% aluminium oxide, 30%~50% diatomite and 6%~15% Ludox, the mass percentage of the silica in Ludox is 25%~30%.Above-mentioned porous alumina ceramic has preferable permeability and preferable intensity.
Description
Technical field
The present invention relates to ceramic material fields more particularly to a kind of porous alumina ceramic and preparation method thereof.
Background technology
Porous ceramics is a kind of novel ceramic material, with the hole being evenly distributed, with very big specific surface
Product, with unique physical surface properties, with to the selectable permeability of liquids and gases medium and energy can be absorbed
(such as sound wave) or there is damping characteristic, and its porosity is compared with high, bulk density is small;Simultaneously as ceramic material inherently has
The excellent performances such as high temperature resistant, rub resistance, corrosion-resistant, high intensity, high rigidity and high elastic modulus, this just makes porous ceramics, and this is green
Color material can be in gas or liquid filtering, purification separation, chemical industry catalytic carrier, sound absorption damping, high-quality thermal insulating material, biological plants
Enter material, the extraordinary various aspects such as materials for wall and sensor material are widely used.
And in numerous porous ceramic film materials, since porous alumina ceramic has, raw material is cheap, the strength of materials is good, system
Make that of low cost, heat-conductive characteristic is low, the good characteristics such as anti-aging, and as a kind of porous ceramics material being most widely used
Material.Porous alumina ceramic refers to being formed in inside by by material forming is with high-temperature sintering process using aluminium oxide as aggregate
A large amount of holes for communicating with each other or being closed.The preparation method of usual porous alumina ceramic has extrusion forming, particle packing to be formed
Air hole structure, gas foaming form porous structure, the foam impregnation method of forming, pore creating material method, sol-gal process and gel note
Modulus method etc..In these types of preparation method, pore creating material method because simple for process, short preparation period, aperture and controlled porosity, with
And the porous ceramics prepared has many advantages, such as good intensity and is widely adopted.
However, the porosity of the porous alumina ceramic prepared at present using pore creating material method is relatively low, generally all 50% with
Under, cause its permeability poor;Porosity is more slightly higher, may result in the strength reduction of porous alumina ceramic, directly affects
To its normal use.
Invention content
In consideration of it, a kind of preferable porous alumina ceramic of and intensity preferable it is necessary to provide permeability.
In addition, also providing a kind of preparation method of porous alumina ceramic.
A kind of porous alumina ceramic, according to mass percentage, the raw material of the porous alumina ceramic includes as follows
Component:40%~60% aluminium oxide, 30%~50% diatomite and 6%~15% Ludox, in the Ludox
The mass percentage of silica is 25%~30%.
A kind of preparation method of porous alumina ceramic, includes the following steps:
Following component is weighed according to mass percent:40%~60% aluminium oxide, 30%~50% diatomite and 6%
The mass percentage of~15% Ludox, the silica in the Ludox is 25%~30%;
The diatomite is pre-processed using hole sealing agent, wherein the hole sealing agent is paraffin or polyethylene glycol;
The pretreated diatomite, the Ludox are mixed with the aluminium oxide in water, mixed slurry is obtained;
The mixed slurry is dry and broken, obtain composite granule;
The composite granule is molded, green body is obtained;And
By the green body in 1450 DEG C~1600 DEG C heat preservation sinterings 1 hour~5 hours, porous alumina ceramic is obtained.
Carrying out pretreated step to the diatomite using the hole sealing agent in one of the embodiments, is:By institute
It states hole sealing agent to be dissolved in solvent, obtains pretreatment fluid, wherein the hole sealing agent and the diatomaceous mass ratio be 10~
25:100;The diatomite is vacuumized after vacuum degree is 5Pa~10Pa, the pretreatment fluid is added, is then passed through filter
And drying, obtain the pretreated diatomite.
The mass percentage of the hole sealing agent in the pretreatment fluid is 10%~20% in one of the embodiments,.
The solvent is kerosene, n-hexane or dimethylbenzene in one of the embodiments,.
In one of the embodiments, before carrying out pretreated step to the diatomite using the hole sealing agent,
Further include to the diatomaceous granulation step:By the diatomite ball milling ,~200 mesh sieve is then sieved with 100 mesh sieve.
In one of the embodiments, by the pretreated diatomite, the Ludox and the aluminium oxide in water
The step of mixing is:The aluminium oxide is added into water for ball milling 10 hours~30 hours, obtains alumina slurry;It then will be pretreated
The diatomite, the Ludox are mixed with the alumina slurry and ball milling.
In one of the embodiments, by the pretreated diatomite, the Ludox and the alumina slurry
Mix and the step of ball milling in, rotating speed when ball milling is 5~15 revs/min.
In one of the embodiments, by the pretreated diatomite, the Ludox and the alumina slurry
Mix and the step of ball milling in, the pretreated diatomite, the Ludox and the alumina slurry quality sum with
The mass ratio 1 of ball milling:0.5~1.
In the step of aluminium oxide is added water for ball milling in one of the embodiments, the aluminium oxide, ball milling and water
Mass ratio be 1:3~5:0.5~1.
Diatomite in the raw material of above-mentioned porous alumina ceramic is pore creating material, because diatomite is by unicellular in Haihe River
The biogenic mineral material that the remains of low water plant diatom were formed by millions of years deposition mineralizations, so by it
Unique and ordered arrangement microcellular structure can be brought to porous alumina ceramic as pore creating material so that ceramics have higher
Porosity, suitable aperture and higher percent opening;Aluminium oxide therein makes ceramics have preferable intensity;And Ludox conduct
Aluminium oxide and diatomaceous Binder Phase, by aluminium oxide and diatomaceous contact position in-situ preparation mullite phase, further
The intensity of porous alumina ceramic is improved, so that the porous oxidation obtained jointly by diatomite, aluminium oxide and Ludox
Aluminium ceramics have preferable permeability and preferable intensity.
Description of the drawings
Fig. 1 is the flow chart of the preparation method of the porous alumina ceramic of an embodiment.
Specific implementation mode
Porous alumina ceramic and preparation method thereof is made mainly in combination with drawings and the specific embodiments below further detailed
Explanation.
The porous alumina ceramic of one embodiment, according to mass percentage, the raw material of porous alumina ceramic includes
Following component:40%~60% aluminium oxide, 30%~50% diatomite and 6%~15% Ludox.
Wherein, aluminium oxide is preferably alpha-aluminium oxide.
Wherein, pore creating material of the diatomite as porous alumina ceramic.Since diatomite is by unicellular low in Haihe River
The biogenic mineral material that the remains of equal water plants diatom were formed by millions of years deposition mineralizations so that it has
Unique and ordered arrangement microcellular structure, porosity high (up to 80%~92%), aperture size are distributed wide, light weight, accumulation
Density is small, and (loose thickness is 0.3~0.5g/cm3), that large specific surface area, thermal coefficient are low, strong adsorption and activity are good etc. is excellent
Point so that diatomite can be as excellent pore-forming material.But since diatomaceous mechanical strength is poor, and aluminium oxide have compared with
Good mechanical strength can obtain the preferable porous ceramics of intensity by being jointly raw material by diatomite and aluminium oxide.
And diatomite not will produce toxic gas as pore creating material in sintering process, and it is very environmentally friendly, avoid use
The pore creating material of volatilization is not decomposed in high temperature sintering, such as sodium chloride, calcium sulfate can participate in sintering reaction, to the performance production at porcelain
Raw serious harmful effect, especially to high-purity ingredient ceramics.
Wherein, diatomaceous aperture is 40 microns~80 microns.
Wherein, the mass percentage of the silica in Ludox is 25%~30%.Ludox is that silica is micro-
Grain is in water or the dispersion liquid in solvent (such as ethyl alcohol).In a particular embodiment, the silicon in the raw material of porous alumina ceramic is molten
The mass percentage of glue is 8%~10%.
Wherein, Ludox can be the model Ludox used for refractory material of Shangyu city Yin Yu silicon Products Co., Ltd.
In the present embodiment, Ludox is made by the steps to obtain:By sodium metasilicate and water mixed diluting, through settling,
Take clear liquid, and the Na in clear liquid2O:nSiO2N be 2.2~3.7;It is 1 according to mass ratio under conditions of being stirred continuously:1
The NaHCO that mass percentage concentration is 3%~6% is added in clear liquid3Aqueous solution, be mixed until clear liquid in without SiO2, continue
Stirring 15 minutes~20 minutes filters taking precipitate, sediment is washed with water to neutrality;Then it is 1 by volume ratio:2 precipitation
Object is mixed with deionized water, obtains suspension;It is 5% in mass percentage concentration under conditions of being stirred continuously and constantly heating up
Partial suspended liquid is added in the aqueous solution of~7% NaOH, stops heating up until temperature is 85 DEG C~90 DEG C, and continue stirring
Under conditions of in 85 DEG C~90 DEG C insulation reactions 2 hours~3 hours, be subsequently added into remaining suspension, obtain mixed liquor;Then
The pH value of mixed liquor is adjusted to 8.0~9.0, continuation is stirred to react 1 hour under conditions of 85 DEG C~90 DEG C, obtains reactant;
The mass percentage that reactant is concentrated into the silica in reactant is 25%~30%, obtains Ludox.
Wherein, in by sodium metasilicate and the step of water mixed diluting, the mass ratio of sodium metasilicate and water is 1:3~1:4.
Wherein, the quality for the suspension being added in the aqueous solution for the NaOH for being 5%~7% in mass percentage concentration is suspension
The 10%~15% of the gross mass of liquid;And the mass ratio of the aqueous solution of NaOH and partial suspended liquid is 1:20.
Wherein, the Baume degrees of sodium metasilicate is 37 ° of é~50 ° B B é (under the conditions of 20 DEG C).
Wherein, the step of mass percentage that reactant is concentrated into the silica in reactant is 25%~30%
For:Reactant is concentrated using semipermeable membrane device, concentration time is 1 hour~3 hours, and the dioxy in reactant is measured after concentration
The mass percentage of SiClx is 25%~30%.
Ludox is as aluminium oxide and diatomaceous Binder Phase.Ludox can be in aluminium oxide and diatomaceous contact position
Originally it was to generate mullite phase, and aluminium oxide and diatomite are bonded together.Due to mullite (3A12O3·2SiO2) it is silicic acid
The object phase that aluminium system is uniquely stablized in high temperature and normal atmosphere pressure, and the object mutually has high refractoriness, thermal expansion and thermal conductivity
The excellent performances such as low, creep rate is low, chemical stability and thermal stability are good, toughness and intensity height so that Ludox plus
Enter the intensity for being conducive to further increase porous alumina ceramic.
Diatomite in the raw material of above-mentioned porous alumina ceramic is pore creating material, because diatomite is by unicellular in Haihe River
The biogenic mineral material that the remains of low water plant diatom were formed by millions of years deposition mineralizations, so by it
Unique and ordered arrangement microcellular structure can be brought to porous alumina ceramic as pore creating material so that ceramics have higher
Porosity, suitable aperture and higher percent opening;Aluminium oxide therein makes ceramics have preferable intensity;And Ludox conduct
Aluminium oxide and diatomaceous Binder Phase, by aluminium oxide and diatomaceous contact position in-situ preparation mullite phase, further
The intensity of porous alumina ceramic is improved, so that the porous oxidation obtained jointly by diatomite, aluminium oxide and Ludox
Aluminium ceramics have preferable permeability and preferable intensity.
As shown in Figure 1, the preparation method of the porous alumina ceramic of an embodiment, can be used for preparing above-mentioned porous oxidation
Aluminium ceramics, the preparation method include the following steps:
Step S110:Following component is weighed according to mass percent:40%~60% aluminium oxide, 30%~50% silicon
Diatomaceous earth and 6%~15% Ludox.
Wherein, aluminium oxide is preferably alpha-aluminium oxide.
Wherein, diatomite is as pore creating material.Ludox is as aluminium oxide and diatomaceous Binder Phase.Ludox can be in oxygen
It is to generate mullite phase, and aluminium oxide and diatomite are bonded together to change aluminium and diatomaceous contact position originally.Due to not coming
Stone (3A12O3·2SiO2) it is the object phase that alumina silicate system is uniquely stablized in high temperature and normal atmosphere pressure, and the object is mutually with resistance to
Fiery degree is high, thermally expands and the Optimalities such as thermal conductivity is low, creep rate is low, chemical stability and thermal stability are good, toughness and intensity height
Can, so that the addition of Ludox is conducive to further increase the intensity of porous alumina ceramic.
Wherein, diatomaceous aperture is 40 microns~80 microns.
Wherein, the mass percentage of the silica in Ludox is 25%~30%.Ludox can be titanium dioxide
Silicon particle is in water or the dispersion liquid in solvent (such as ethyl alcohol).In a particular embodiment, in the raw material of porous alumina ceramic
The mass percentage of Ludox is 8%~10%.
Wherein, Ludox can be the model Ludox used for refractory material of Shangyu city Yin Yu silicon Products Co., Ltd.
In the present embodiment, Ludox is made by the steps to obtain:By sodium metasilicate and water mixed diluting, through settling,
Take clear liquid, and the Na in clear liquid2O:nSiO2N be 2.2~3.7;It is 1 according to mass ratio under conditions of being stirred continuously:1
The NaHCO that mass percentage concentration is 3%~6% is added in clear liquid3Aqueous solution, be mixed until clear liquid in without SiO2, continue
Stirring 15 minutes~20 minutes filters taking precipitate, sediment is washed with water to neutrality;Then it is 1 by volume ratio:2 precipitation
Object is mixed with deionized water, obtains suspension;It is 5% in mass percentage concentration under conditions of being stirred continuously and constantly heating up
Partial suspended liquid is added in the aqueous solution of~7% NaOH, stops heating up until temperature is 85 DEG C~90 DEG C, and continue stirring
Under conditions of in 85 DEG C~90 DEG C insulation reactions 2 hours~3 hours, be subsequently added into remaining suspension, obtain mixed liquor;Then
The pH value of mixed liquor is adjusted to 8.0~9.0, continuation is stirred to react 1 hour under conditions of 85 DEG C~90 DEG C, obtains reactant;
The mass percentage that reactant is concentrated into the silica in reactant is 25%~30%, obtains Ludox.
Wherein, in by sodium metasilicate and the step of water mixed diluting, the mass ratio of sodium metasilicate and water is 1:3~1:4.
Wherein, the quality for the suspension being added in the aqueous solution for the NaOH for being 5%~7% in mass percentage concentration is suspension
The 10%~15% of the gross mass of liquid;And the mass ratio of the aqueous solution of NaOH and partial suspended liquid is 1:20.
Wherein, the Baume degrees of sodium metasilicate is 37 ° of é~50 ° B B é (under the conditions of 20 DEG C).
Wherein, the step of mass percentage that reactant is concentrated into the silica in reactant is 25%~30%
For:Reactant is concentrated using semipermeable membrane device, concentration time is 1 hour~3 hours, and the dioxy in reactant is measured after concentration
The mass percentage of SiClx is 25%~30%.
Step S120:Diatomite is pre-processed using hole sealing agent.
Wherein, hole sealing agent is paraffin or polyethylene glycol.By first being pre-processed to diatomite using hole sealing agent, to block
Diatomaceous hole, to prevent in subsequent raw material mixed process, other raw materials enter in diatomaceous hole, cause more
The problem that the porosity of hole ceramics reduces and pore communication is poor.And hole sealing agent can volatilize at high temperature, not interfere with
The porosity of porous alumina ceramic.
Further include being walked to diatomaceous granulation specifically, before carrying out pretreated step to diatomite using hole sealing agent
Suddenly:By diatomite ball milling ,~200 mesh sieve is then sieved with 100 mesh sieve.
Wherein, in step S120, carrying out pretreated step to diatomite using hole sealing agent is:Hole sealing agent is dissolved in molten
In agent, wherein hole sealing agent is 10~25 with diatomaceous mass ratio:100, obtain pretreatment fluid;Diatomite is vacuumized until
After vacuum degree is 5Pa~10Pa, pretreatment fluid is added, is then passed through filter and drying, obtains pretreated diatomite.By first right
Diatomite vacuumize process, then be added pretreatment fluid mixing so that pretreatment fluid can successfully be inhaled into it is diatomaceous
In hole.Specifically, being vacuumized to diatomite until vacuum degree is specially the step of being 5Pa~10Pa:Diatomite is positioned over
It in vacuum tank, then vacuumizes, until the vacuum degree in vacuum tank is 5Pa~10Pa.
Wherein, after being vacuumized to diatomite, be added pretreatment fluid the step of after drying steps drying temperature be 20
DEG C~40 DEG C.
Wherein, the mass percentage of the hole sealing agent in pretreatment fluid is 10%~20%.
Wherein, solvent can be that there are commonly solvents, and in the present embodiment, solvent is kerosene, n-hexane or dimethylbenzene.
Step S130:Pretreated diatomite, Ludox are mixed with aluminium oxide in water, mixed slurry is obtained.
Specifically, the step of pretreated diatomite, Ludox are mixed with aluminium oxide in water is:By aluminium oxide plus water
Ball milling 10 hours~30 hours, obtains alumina slurry;Then pretreated diatomite, Ludox are mixed with alumina slurry
And ball milling.And Ludox is mixed with alumina slurry and the time of ball milling is 5 hours~10 hours.
More specifically, in the step of aluminium oxide is added water for ball milling, the mass ratio of aluminium oxide, ball milling and water is 1:3~
5:0.5~1.
Wherein, pretreated diatomite, Ludox are mixed with alumina slurry and the step of ball milling in, when ball milling
Rotating speed is 5 revs/min~15 revs/min.And pretreated diatomite, Ludox mixed with alumina slurry and ball milling
In step, the quality sum of pretreated diatomite, Ludox and alumina slurry is 1 with the mass ratio of ball milling:0.5~1.
By low speed ball milling mixing, and the purpose for controlling the material ball ratio be in order to during mitigating ball milling mixing as possible ball milling to locating in advance
Reason diatomaceous destruction, caused by pretreated diatomaceous granularity become smaller.
Step S140:Mixed slurry is dry and broken, obtain composite granule.
Further include the steps that mixed slurry is filtered by vacuum specifically, before the step for drying mixed slurry.
The step can remove extra moisture, avoid mixed slurry viscosity too small and be layered during drying.
Wherein, in step S140, temperature when mixed slurry is dried is 40 DEG C~50 DEG C.
Step S150:Composite granule is molded, green body is obtained.
Wherein, further include the steps that being sieved to composite granule before being molded composite granule.Specifically, will answer
It closes powder and crosses 60 mesh sieve~100 mesh sieve.
Wherein, the forming method of composite granule can be dry-pressing formed, isostatic pressing or injection molding.
Step S160:Green body is sintered 1 hour~5 hours in 1450 DEG C~1600 DEG C, obtains porous alumina ceramic.
Wherein, further include the steps that green body is sloughed into organic matter and water before the step of by blank sintering.Wherein, will
Green body sloughs the step of organic matter and water and is:Green body is warming up to 300 DEG C with 1 DEG C/minute~2 DEG C/minute of speed, and it is small to keep the temperature 2
When~4 hours, 650 DEG C then are warming up to 2 DEG C/minute~4 DEG C/minute of speed, keeps the temperature 2 hours~4 hours, moisture is completed and has
The removing of machine object.
Specifically, step S160 is carried out in air calcination stove.
Above-mentioned preparation method is simple, by before mixing diatomite with aluminium oxide, Ludox, first using hole sealing agent pair
Diatomite is pre-processed, to block diatomaceous hole, to avoid in the raw materials mixed process such as diatomite and aluminium oxide,
Its raw material penetrates into diatomaceous hole, and cause ceramics porosity reduce the problem of;And because diatomite is by Haihe River
Unicellular low water plant diatom the biogenic mineral material that is formed by millions of years deposition mineralizations of remains,
So unique and ordered arrangement microcellular structure can be brought to porous alumina ceramic as pore creating material so that ceramics tool
There are higher porosity, suitable aperture and higher percent opening;Aluminium oxide therein makes ceramics have preferable intensity;And silicon
Colloidal sol is as aluminium oxide and diatomaceous Binder Phase, by aluminium oxide and diatomaceous contact position in-situ preparation mullite
Phase further improves the intensity of porous alumina ceramic, so that obtained jointly by diatomite, aluminium oxide and Ludox
Porous alumina ceramic has preferable permeability and preferable intensity.
It is specific embodiment part below:
Embodiment 1
The preparation process of the porous alumina ceramic of the present embodiment is as follows:
(1) it is the sodium metasilicate of 37 ° of B é (under the conditions of 20 DEG C) to take Baume degrees, is 1 according to the mass ratio of sodium metasilicate and water:4,
Sodium metasilicate and water mixed diluting are taken into clear liquid, wherein the Na in clear liquid through natural subsidence to clarifying2O:nSiO2In n be
2.2;It is 1 according to mass ratio under conditions of being stirred continuously:1 is added the NaHCO that mass percentage concentration is 3% in clear liquid3's
Aqueous solution is mixed until without SiO in clear liquid2, continue stirring 15 minutes, filter taking precipitate, sediment is washed with water extremely
Then neutrality is 1 according to the volume ratio of sediment and deionized water:2, sediment and deionized water are mixed, hanged
Supernatant liquid;The aqueous solution for the NaOH that mass percentage concentration is 5% is added in reaction kettle, wherein the aqueous solution and clear liquid of NaOH
Mass ratio be 1:20, under conditions of being stirred continuously and constantly heating up, partial suspended liquid is added, until temperature is 85 DEG C of stoppings
Heating, and continue to be subsequently added into remaining suspension in 85 DEG C of insulation reactions 2 hours under stirring conditions, obtain mixed liquor,
Then the pH value of mixed liquor is adjusted to 8.0, and continuation is stirred to react 1 hour under conditions of 85 DEG C, obtains reactant;By reactant
The mass percentage that the silica in reactant is concentrated into semipermeable membrane device is 25%, obtains Ludox.Wherein, exist
The quality for the suspension being added in the aqueous solution of NaOH is the 10% of the gross mass of suspension.
(2) following component is weighed according to mass percentage:40% aluminium oxide, 50% diatomite and 10% silicon it is molten
Glue, wherein diatomaceous aperture is 80 microns.
(3) paraffin is dissolved in kerosene, obtains the pretreatment fluid that the mass percentage of paraffin is 20%, wherein stone
Wax is 15 with diatomaceous mass ratio:100.
(4) by diatomite in ball mill ball milling, then sieve with 100 mesh sieve, the diatomite after sieving be then put into vacuum
In container, vacuumize until vacuum tank in vacuum degree reach 5Pa, pretreatment fluid is poured into, at this point, pretreatment fluid enters silicon
In the hole of diatomaceous earth, then filter, it is dry in baking oven 20 DEG C, obtain pretreated diatomite.
(5) it is 1 according to the mass ratio of aluminium oxide, ball milling and water:5:0.5, aluminium oxide plus water for ball milling are mixed 10 hours,
Obtain alumina slurry;Pretreated diatomite, Ludox and alumina slurry are put into togerther in ball grinder, in 5 revs/min
Rotating speed under conditions of ball milling mixing, obtain mixed slurry;And the quality of pretreated diatomite, Ludox and alumina slurry
The sum of mass ratio 1 with ball milling:0.5.
(6) mixed slurry is filtered by vacuum, then by filter residue in drying box 40 DEG C of dryings 10 hours, then through broken
It is broken and sieve with 100 mesh sieve, obtain composite granule.
(7) composite granule is dry-pressing formed, obtain green body.
(8) green body is put into debinding furnace, first 300 DEG C is warming up to 1 DEG C/minute of speed, and keep the temperature 2 hours, then with 2
DEG C/minute speed be warming up to 650 DEG C, keep the temperature 2 hours, complete the removing of moisture and organic matter.Then green body air is put into burn
It is sintered 2 hours in 1500 DEG C in freezing of a furnace, obtains porous alumina ceramic.It can be repaiied porous alumina ceramic as needed at this time
It is whole.
Using GB/T 1966-1996, GB/T 1967-1996 standard laws to the gas of the porous alumina ceramic of the present embodiment
Porosity, average pore size and percent opening are measured, and using the porous oxidation of GB/T 4740-1999 standard test the present embodiment
The compression strength of aluminium ceramics.The porosity, average pore size, percent opening and the compression strength of the porous alumina ceramic of the present embodiment are shown in
Table 1.
Embodiment 2
The preparation process of the porous alumina ceramic of the present embodiment is as follows:
(1) it is the sodium metasilicate of 40 ° of B é (under the conditions of 20 DEG C) to take Baume degrees, is 1 according to the mass ratio of sodium metasilicate and water:3,
Sodium metasilicate and water mixed diluting are taken into clear liquid, wherein the Na in clear liquid through natural subsidence to clarifying2O:nSiO2In n be 3;
It is 1 according to mass ratio under conditions of being stirred continuously:1 is added the NaHCO that mass percentage concentration is 5% in clear liquid3It is water-soluble
Liquid is mixed until without SiO in clear liquid2, continue stirring 20 minutes, filter taking precipitate, sediment is washed with water to neutrality,
Then it is 1 according to the volume ratio of sediment and deionized water:2, sediment and deionized water are mixed, suspension is obtained;
The aqueous solution for the NaOH that mass percentage concentration is 5% is added in reaction kettle, wherein the aqueous solution of NaOH and the quality of clear liquid
Than being 1:20, under conditions of being stirred continuously and constantly heating up, partial suspended liquid is added, stops heating up until temperature is 90 DEG C,
And continue to be subsequently added into remaining suspension in 90 DEG C of insulation reactions 2 hours under stirring conditions, obtain mixed liquor, then
The pH value of mixed liquor is adjusted to 8.5, continuation is stirred to react 1 hour under conditions of 90 DEG C, obtains reactant;By reactant with partly
The mass percentage that permeable membrane device is concentrated into the silica in reactant is 28%, obtains Ludox.Wherein, NaOH's
The quality for the suspension being added in aqueous solution is the 15% of the gross mass of suspension.
(2) following component is weighed according to mass percentage:50% aluminium oxide, 42% diatomite and 8% silicon it is molten
Glue, wherein diatomaceous aperture is 50 microns.
(3) paraffin is dissolved in dimethylbenzene, obtains the pretreatment fluid that the mass percentage of paraffin is 15%, wherein
Paraffin is 10 with diatomaceous mass ratio:100.
(4) by diatomite in ball mill ball milling, then cross 150 mesh sieve, the diatomite after sieving is then put into vacuum
In container, vacuumize until container in vacuum degree reach 7Pa, pour into pretreatment fluid, so that pretreatment fluid is entered diatomaceous
In hole, then filter, it is dry in baking oven 25 DEG C, obtain pretreated diatomite.
(5) it is 1 according to the mass ratio of aluminium oxide, ball milling and water:3:0.6, aluminium oxide plus water for ball milling are mixed 15 hours,
Obtain alumina slurry;Pretreated diatomite, Ludox and alumina slurry are put into togerther in ball grinder, in 15 revs/min
Ball milling mixing under conditions of the rotating speed of clock, obtains mixed slurry;And the matter of pretreated diatomite, Ludox and alumina slurry
Mass ratio 1 of the sum of the amount with ball milling:0.6.
(6) mixed slurry is filtered by vacuum, then by filter residue in drying box 41 DEG C of dryings 12 hours, then through broken
The broken and sieve of 60 mesh excessively, obtains composite granule.
(7) by composite granule isostatic pressing, green body is obtained.
(8) green body is put into debinding furnace, first 300 DEG C is warming up to 2 DEG C/minute of speed, and keep the temperature 4 hours, then with 4
DEG C/minute speed be warming up to 650 DEG C, keep the temperature 4 hours, complete the removing of moisture and organic matter.Then green body air is put into burn
It is sintered 2.5 hours in 1520 DEG C in freezing of a furnace, obtains porous alumina ceramic.It porous alumina ceramic can carry out as needed at this time
Finishing.
It to the porosity of the porous alumina ceramic of the present embodiment, average pore size and is opened using 1 identical method of embodiment
Porosity is measured, and use 1 identical method of embodiment measures the compression strength of the porous alumina ceramic of the present embodiment.This
The porosity, average pore size, percent opening and the compression strength of the porous alumina ceramic of embodiment are shown in Table 1.
Embodiment 3
The preparation process of the porous alumina ceramic of the present embodiment is as follows:
(1) it is the sodium metasilicate of 50 ° of B é (under the conditions of 20 DEG C) to take Baume degrees, is 1 according to the mass ratio of sodium metasilicate and water:3,
Sodium metasilicate and water mixed diluting are taken into clear liquid, wherein the Na in clear liquid through natural subsidence to clarifying2O:nSiO2In n be
3.7;It is 1 according to mass ratio under conditions of being stirred continuously:1 is added the NaHCO that mass percentage concentration is 6% in clear liquid3's
Aqueous solution is mixed until without SiO in clear liquid2, continue stirring 15 minutes, filter taking precipitate, sediment is washed with water extremely
Then neutrality is 1 according to the volume ratio of sediment and deionized water:2, sediment and deionized water are mixed, hanged
Supernatant liquid;The aqueous solution for the NaOH that mass percentage concentration is 7% is added in reaction kettle, wherein the aqueous solution and clear liquid of NaOH
Mass ratio be 1:20, under conditions of being stirred continuously and constantly heating up, partial suspended liquid is added, until temperature is 90 DEG C of stoppings
Heating, and continue to be subsequently added into remaining suspension in 90 DEG C of insulation reactions 3 hours under stirring conditions, obtain mixed liquor,
Then the pH value of mixed liquor is adjusted to 9.0, and continuation is stirred to react 1 hour under conditions of 90 DEG C, obtains reactant;By reactant
The mass percentage that the silica in reactant is concentrated into semipermeable membrane device is 30%, obtains Ludox.Wherein, exist
The quality for the suspension being added in the aqueous solution of NaOH is the 10% of the gross mass of suspension.
(2) following component is weighed according to mass percentage:60% aluminium oxide, 30% diatomite and 10% silicon it is molten
Glue, wherein diatomaceous aperture is 40 microns.
(3) polyethylene glycol is dissolved in n-hexane, obtains the pretreatment that the mass percentage of polyethylene glycol is 20%
Liquid, wherein polyethylene glycol is 25 with diatomaceous mass ratio:100.
(4) by diatomite in ball mill ball milling, then cross 200 mesh sieve, the diatomite after sieving is then put into vacuum
In container, vacuumize until container in vacuum degree reach 10Pa, pour into pretreatment fluid, so that pretreatment fluid is entered diatomaceous
In hole, then filter, it is dry at 40 DEG C, obtain pretreated diatomite.
(5) it is 1 according to the mass ratio of aluminium oxide, ball milling and water:5:1, aluminium oxide plus water for ball milling are mixed 22 hours, obtained
To alumina slurry;Pretreated diatomite, Ludox and alumina slurry are put into togerther in ball grinder, in 9 revs/min
Ball milling mixing under conditions of rotating speed, obtains mixed slurry;And the quality of pretreated diatomite, Ludox and alumina slurry it
With the mass ratio 1 with ball milling:1.
(6) mixed slurry is filtered by vacuum, then by filter residue in drying box 50 DEG C of dryings 13 hours, then through broken
It is broken and sieve with 100 mesh sieve, obtain composite granule.
(7) by composite granule injection molding, green body is obtained.
(8) green body is put into debinding furnace, first 300 DEG C is warming up to 2 DEG C/minute of speed, and keep the temperature 3 hours, then with 4
DEG C/minute speed be warming up to 650 DEG C, keep the temperature 3 hours, complete to be put into air calcination stove after the removing of moisture and organic matter in
1600 DEG C are sintered 5 hours, obtain porous alumina ceramic.It can be modified porous alumina ceramic as needed at this time.
It to the porosity of the porous alumina ceramic of the present embodiment, average pore size and is opened using 1 identical method of embodiment
Porosity is measured, and use 1 identical method of embodiment measures the compression strength of the porous alumina ceramic of the present embodiment.This
The porosity, average pore size, percent opening and the compression strength of the porous alumina ceramic of embodiment are shown in Table 1.
Comparative example 1
The preparation process of the porous alumina ceramic of comparative example 1 is as follows:
(1) following component is weighed according to mass percentage:40% aluminium oxide and 60% graphite, wherein graphite
Grain size is 80 microns.
(2) aluminium oxide and graphite and water are added in ball grinder, the ball milling mixing 10 under conditions of 10 revs/min of rotating speed
Hour, obtain mixed slurry;And the mass ratio of the quality sum of aluminium oxide and graphite, ball milling and water is 1:2:0.5.
(5) to 80 DEG C of dryings in mixed slurry drying box 20 hours, then through broken and sieve with 100 mesh sieve, composite powder is obtained
Body.
(6) composite granule is dry-pressing formed, obtain green body.
(7) green body is put into debinding furnace, first 300 DEG C is warming up to 1 DEG C/minute of speed, and keep the temperature 2 hours, then with 2
DEG C/minute speed be warming up to 650 DEG C, keep the temperature 2 hours, complete the removing of moisture and organic matter.Then green body air is put into burn
In 1500 DEG C of heat preservation sinterings 2 hours in freezing of a furnace, porous alumina ceramic is obtained.At this time can as needed porous alumina ceramic into
Row finishing.
Using 1 identical method of embodiment to the porosity of the porous alumina ceramic of comparative example 1, average pore size and trepanning
Rate is measured, and the compression strength of the porous alumina ceramic using 1 identical method of embodiment measurement comparative example 1, wherein
The porosity, average pore size, percent opening and the compression strength of the porous alumina ceramic of comparative example 1 are shown in Table 1.
Comparative example 2
The preparation process of the porous alumina ceramic of comparative example 2 is as follows:
(1) following component is weighed according to mass percentage:50% aluminium oxide and 50% graphite, wherein graphite
Grain size is 50 microns.
(2) aluminium oxide and graphite and water are added in ball grinder, the ball milling mixing 12 under conditions of 8 revs/min of rotating speed
Hour, obtain mixed slurry;And the mass ratio of the quality sum of aluminium oxide and graphite, ball milling and water is 1:2:0.6.
(5) to 85 DEG C of dryings in mixed slurry drying box 24 hours, then through broken and cross 150 mesh sieve, composite powder is obtained
Body.
(6) by composite granule isostatic pressing, green body is obtained.
(7) green body is put into debinding furnace, first 300 DEG C is warming up to 2 DEG C/minute of speed, and keep the temperature 4 hours, then with 4
DEG C/minute speed be warming up to 650 DEG C, keep the temperature 4 hours, complete the removing of moisture and organic matter.Then green body is removed into organic matter
After moisture, it is put into air calcination stove in 1520 DEG C of heat preservation sinterings 2.5 hours, obtains porous alumina ceramic.It at this time can root
It is modified according to porous alumina ceramic is needed.
Using 1 identical method of embodiment to the porosity of the porous alumina ceramic of comparative example 2, average pore size and trepanning
Rate is measured, and the compression strength of the porous alumina ceramic using 1 identical method of embodiment measurement comparative example 2,
In, the porosity, average pore size, percent opening and the compression strength of the porous alumina ceramic of comparative example 2 are shown in Table 1.
Comparative example 3
The preparation process of the porous alumina ceramic of comparative example 3 is as follows:
(1) following component is weighed according to mass percentage:60% aluminium oxide and 40% graphite, wherein graphite
Grain size is 40 microns.
(2) aluminium oxide and graphite and water are added in ball grinder, ball milling mixing 8 is small under conditions of 9 revs/min of rotating speed
When, obtain mixed slurry;And the mass ratio of the quality sum of aluminium oxide and graphite, ball milling and water is 1:1:0.5.
(5) to 50 DEG C of dryings in mixed slurry drying box 13 hours, then through broken and sieve with 100 mesh sieve, composite powder is obtained
Body.
(6) composite granule is injection moulded, obtains green body.
(7) green body is put into debinding furnace, first 300 DEG C is warming up to 2 DEG C/minute of speed, and keep the temperature 3 hours, then with 4
DEG C/minute speed be warming up to 650 DEG C, keep the temperature 3 hours, complete that green body is put into air calcination stove after the removing of moisture and organic matter
In in 1600 DEG C of heat preservation sinterings 5 hours, obtain porous alumina ceramic.It can be repaiied porous alumina ceramic as needed at this time
It is whole.
Using 1 identical method of embodiment to the porosity of the porous alumina ceramic of comparative example 3, average pore size and trepanning
Rate is measured, and the compression strength of the porous alumina ceramic using 1 identical method of embodiment measurement comparative example 3, wherein
The porosity, average pore size, percent opening and the compression strength of the porous alumina ceramic of comparative example 3 are shown in Table 1.
Comparative example 4
The preparation process of the porous alumina ceramic of comparative example 4 is as follows:
(1) following component is weighed according to mass percentage:40% aluminium oxide and 60% diatomite, wherein diatom
The aperture of soil is 80 microns.
(2) by diatomite in ball mill ball milling, then sieve with 100 mesh sieve.
(3) it is 1 according to the mass ratio of aluminium oxide, ball milling and water:5:0.5, aluminium oxide plus water for ball milling are mixed 10 hours,
Obtain alumina slurry;Diatomite and alumina slurry are put into togerther in ball grinder, under conditions of 5 revs/min of rotating speed
Ball milling mixing obtains mixed slurry;And the mass ratio 1 of the quality sum of diatomite and alumina slurry and ball milling:0.5.
(4) mixed slurry is filtered by vacuum, then by filter residue in drying box 40 DEG C of dryings 10 hours, then through broken
It is broken and sieve with 100 mesh sieve, obtain composite granule.
(5) composite granule is dry-pressing formed, obtain green body.
(6) green body is put into debinding furnace, first 300 DEG C is warming up to 2 DEG C/minute of speed, and keep the temperature 3 hours, then with 4
DEG C/minute speed be warming up to 650 DEG C, keep the temperature 3 hours, complete that green body is put into air calcination stove after the removing of moisture and organic matter
In in 1500 DEG C be sintered 2 hours, obtain porous alumina ceramic.It can be modified porous alumina ceramic as needed at this time.
Using 1 identical method of embodiment to the porosity of the porous alumina ceramic of comparative example 4, average pore size and trepanning
Rate is measured, and the compression strength of the porous alumina ceramic using 1 identical method of embodiment measurement comparative example 4.Comparison
The porosity, average pore size, percent opening and the compression strength of the porous alumina ceramic of example 4 are shown in Table 1.
Comparative example 5
The preparation process of the porous alumina ceramic of comparative example 5 is as follows:
(1) it is the sodium metasilicate of 37 ° of B é (under the conditions of 20 DEG C) to take Baume degrees, is 1 according to the mass ratio of sodium metasilicate and water:4,
Sodium metasilicate and water mixed diluting are taken into clear liquid, wherein the Na in clear liquid through natural subsidence to clarifying2O:nSiO2In n be
2.2;It is 1 according to mass ratio under conditions of being stirred continuously:1 is added the NaHCO that mass percentage concentration is 3% in clear liquid3's
Aqueous solution is mixed until without SiO in clear liquid2, continue stirring 15 minutes, filter taking precipitate, sediment is washed with water extremely
Then neutrality is 1 according to the volume ratio of sediment and deionized water:2, sediment and deionized water are mixed, hanged
Supernatant liquid;The aqueous solution for the NaOH that mass percentage concentration is 5% is added in reaction kettle, wherein the aqueous solution and clear liquid of NaOH
Mass ratio be 1:20, under conditions of being stirred continuously and constantly heating up, partial suspended liquid is added, until temperature is 85 DEG C of stoppings
Heating, and continue to be subsequently added into remaining suspension in 85 DEG C of insulation reactions 2 hours under stirring conditions, obtain mixed liquor,
Then the pH value of mixed liquor is adjusted to 8.0, and continuation is stirred to react 1 hour under conditions of 85 DEG C, obtains reactant;By reactant
The mass percentage that the silica in reactant is concentrated into semipermeable membrane device is 25%, obtains Ludox.Wherein, exist
The quality for the suspension being added in the aqueous solution of NaOH is the 10% of the gross mass of suspension.
(2) following component is weighed according to mass percentage:40% aluminium oxide, 50% diatomite and 10% silicon it is molten
Glue, wherein diatomaceous aperture is 80 microns.
(3) by diatomite in ball mill ball milling, then sieve with 100 mesh sieve.
(4) it is 1 according to the mass ratio of aluminium oxide, ball milling and water:5:0.5, aluminium oxide plus water for ball milling are mixed 10 hours,
Obtain alumina slurry;Diatomite, Ludox and alumina slurry are put into togerther in ball grinder, in 5 revs/min of rotating speeds
Under the conditions of ball milling mixing, obtain mixed slurry;And the matter of the quality sum of diatomite, Ludox and alumina slurry and ball milling
Measure ratio 1:0.5.
(5) mixed slurry is filtered by vacuum, then by filter residue in drying box 40 DEG C of dryings 10 hours, then through broken
It is broken and sieve with 100 mesh sieve, obtain composite granule.
(6) composite granule is dry-pressing formed, obtain green body.
(7) green body is put into debinding furnace, first 300 DEG C is warming up to 1 DEG C/minute of speed, and keep the temperature 2 hours, then with 2
DEG C/minute speed be warming up to 650 DEG C, keep the temperature 2 hours, complete the removing of moisture and organic matter.Then green body air is put into burn
It is sintered 2 hours in 1500 DEG C in freezing of a furnace, obtains porous alumina ceramic.It can be repaiied porous alumina ceramic as needed at this time
It is whole.
Using 1 identical method of embodiment to the porosity of the porous alumina ceramic of comparative example 5, average pore size and trepanning
Rate is measured, and the compression strength of the porous alumina ceramic using 1 identical method of embodiment measurement comparative example 5, wherein
The porosity, average pore size, percent opening and the compression strength of the porous alumina ceramic of comparative example 5 are shown in Table 1.
Table 1 is in order that the porosity of the porous alumina ceramic of Examples 1 to 3 and comparative example 1~5, average pore size, trepanning
Rate and compression strength.
Table 1
From table 1 it follows that the porosity of the porous alumina ceramic of Examples 1 to 3, average pore size, percent opening are equal
Comparative example 1~3 than the almost graphite pore former of equal proportion is added is high, i.e. the porous alumina ceramic tool of Examples 1 to 3
There is better permeability;And the compression strength of the porous alumina ceramic of Examples 1 to 3 is it is also apparent that than using graphite as pore creating material
Comparative example 1~3 to get well, therefore, the porous alumina ceramic of Examples 1 to 3 has higher porosity and preferable intensity.
Meanwhile the porous alumina ceramic of comparative example 4 is compared with the porous alumina ceramic of embodiment 1, due to being not used
Binder Phase when Ludox is as sintering, therefore, compression strength is decreased obviously, and its porosity and aperture and 1 phase of embodiment
Almost.Therefore Binder Phase of the Ludox as sintering when is used, the mechanical property of porous alumina ceramic can be effectively improved.
For the porous alumina ceramic of comparative example 5 compared with the porous alumina ceramic of embodiment 1, raw material forms complete phase
Together, but due to hole sealing agent not being used to carry out sealing of hole operation to diatomite, cause in mixing, Ludox and alumina slurry enter
In diatomaceous hole, porosity and the aperture of porous alumina ceramic are greatly reduced.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (7)
1. a kind of preparation method of porous alumina ceramic, which is characterized in that include the following steps:
Following component is weighed according to mass percent:40%~60% aluminium oxide, 30%~50% diatomite and 6%~
The mass percentage of 15% Ludox, the silica in the Ludox is 25%~30%;
The diatomite is pre-processed using hole sealing agent, wherein the hole sealing agent is paraffin or polyethylene glycol;
The pretreated diatomite, the Ludox are mixed with the aluminium oxide in water, mixed slurry is obtained;
The mixed slurry is dry and broken, obtain composite granule;
The composite granule is molded, green body is obtained;And
By the green body in 1450 DEG C~1600 DEG C heat preservation sinterings 1 hour~5 hours, porous alumina ceramic is obtained;
Carrying out pretreated step to the diatomite using the hole sealing agent is:The hole sealing agent is dissolved in solvent, is obtained
To pretreatment fluid, wherein the hole sealing agent is 10~25 with the diatomaceous mass ratio:100;The diatomite is vacuumized
Until after vacuum degree is 5Pa~10Pa, the pretreatment fluid is added, is then passed through filter and drying, obtains the pretreated silicon
Diatomaceous earth;
The mass percentage of hole sealing agent in the pretreatment fluid is 10%~20%;The solvent be kerosene, n-hexane or
Dimethylbenzene.
2. the preparation method of porous alumina ceramic according to claim 1, which is characterized in that using the hole sealing agent
Further include to the diatomaceous granulation step before carrying out pretreated step to the diatomite:By the diatom soil ball
Mill then sieves with 100 mesh sieve~200 mesh sieve.
3. the preparation method of porous alumina ceramic according to claim 1, which is characterized in that by the pretreated silicon
The step of diatomaceous earth, the Ludox are mixed with the aluminium oxide in water be:The aluminium oxide is added into water for ball milling 10 hours~30
Hour, obtain alumina slurry;Then the pretreated diatomite, the Ludox are mixed simultaneously with the alumina slurry
Ball milling.
4. the preparation method of porous alumina ceramic according to claim 3, which is characterized in that will be pretreated described
Diatomite, the Ludox mixed with the alumina slurry and the step of ball milling in, rotating speed when ball milling is 5~15 revs/min
Clock.
5. the preparation method of porous alumina ceramic according to claim 3, which is characterized in that will be pretreated described
Diatomite, the Ludox were mixed with the alumina slurry in the step of simultaneously ball milling, the pretreated diatomite, the silicon
The mass ratio 1 of colloidal sol and the quality sum and ball milling of the alumina slurry:0.5~1.
6. the preparation method of porous alumina ceramic according to claim 3, which is characterized in that add by the aluminium oxide
In the step of water for ball milling, the mass ratio of the aluminium oxide, ball milling and water is 1:3~5:0.5~1.
7. the porous alumina ceramic that the preparation method of any one of claim 1~6 porous alumina ceramic is prepared.
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CN106966654A (en) * | 2017-03-31 | 2017-07-21 | 杨杰 | The method that a kind of utilization aluminosilicate industrial residue and boehmite prepare sponge urban construction water-permeable brick |
CN106866168B (en) * | 2017-04-07 | 2020-05-26 | 西安明科微电子材料有限公司 | Preparation method of α -phase microporous alumina ceramic |
CN110256103A (en) * | 2019-07-18 | 2019-09-20 | 覃向阳 | One method of porous alumina ceramics base phase becomes heat-insulation composite material |
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