CN106187142A - A kind of preparation method of high porosity complex phase porous ceramic film material - Google Patents
A kind of preparation method of high porosity complex phase porous ceramic film material Download PDFInfo
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- 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
- C04B35/16—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 silicates other than clay
- C04B35/22—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 silicates other than clay rich in calcium oxide, e.g. wollastonite
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- 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
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
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- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
- C04B2235/321—Dolomites, i.e. mixed calcium magnesium carbonates
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- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- 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
- C04B2235/38—Non-oxide ceramic constituents or additives
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Abstract
The invention discloses the preparation method of a kind of high porosity complex phase porous ceramic film material, belong to porous ceramics preparing technical field.Wollastonite, dolomite, gangue are respectively prepared powder by the present invention, again wollastonite and dolomite are mixed, gangue soaks filtration with mixed acid after carrying out heat treatment, the filter residue and drying obtained makes dried object, again the powder that above-mentioned mixed-powder, dried object are made with carborundum, aluminium sesquioxide powder, white carbon black and starch is stirred, the mixed-powder finally prepared is loaded stainless steel mould cold moudling, prepared block pressed compact is carried out high temperature sintering, stand subsequently be cooled to room temperature high porosity complex phase porous ceramic film material.Raw material of the present invention is easy to get, and preparation technology is simple, and the porous ceramics porosity made is up to more than 85%, and even air hole distribution, is suitable for industrialized production, has broad mass market prospect.
Description
Technical field
The invention discloses the preparation method of a kind of high porosity complex phase porous ceramic film material, belong to porous ceramics and prepare skill
Art field.
Background technology
In the tide of global economic development, environment and resource are two hang-ups that the mankind run into, people to save resource,
The requirement of protection environment is more and more higher.Porous ceramics has adapted to the new material of this development of the situation demand just, and it can improve
Efficiency, the saving energy, especially play increasing effect in terms of environmental conservation.Porous ceramics is in the application of all trades and professions
Become increasingly popular to have embodied the meaning of this two broad aspect.
Porous ceramic film material is as major ingredient, through overmolding and special height with quality raw materials such as emergy, carborundum, cordierites
Temperature sintering process prepare a kind of have open pore size, a kind of porous ceramic materials of high apparent porosity, have high temperature resistant,
High pressure, antiacid, alkali and organic media corrosion, good biologically inert, controlled pore structure and high open porosity, use longevity
The advantages such as life is long, product regenerability is good, go for the secondary filter of various medium and separate, gases at high pressure aerofluxus disappears
The distribution of sound, gas and electrolyte membrane etc..
The material of porous ceramic film material is of a great variety, owing to application target is different, different to the performance requirement of material, therefore, closely
Many different technologies of preparing are gradually developed over Nian.Wherein Application comparison success, having that research is relatively more active is following several:
Add pore creating material technique: this technique, by adding pore creating material in ceramic batch, utilizes pore creating material to occupy one in base substrate
Fixed space, is then passed through sintering, and pore creating material leaves matrix and forms pore to prepare porous ceramics.
Foam dipping method: Polymeric sponge method is to use foam impregnation ceramic size, burns after drying and has
Machine foam, it is thus achieved that a kind of method of porous ceramics.
Foam process: foam process is compared with foam impregnation technique, it is easier to control the shape of goods, composition and density,
And the porous ceramics of various pore size and shape can be prepared, be particularly suitable for producing the ceramic in hole of holding one's breath.
Sol-gel technology: sol-gel process is mainly used to prepare micropore ceramics material, particularly micropore ceramics thin film.
But porous ceramics prepared by prior art generally exists that the porosity is low, even air hole distribution is poor, and make work
Skill is complicated, the problem high to ingredient requirement.
Summary of the invention
The technical problem that present invention mainly solves: the porous ceramics prepared for prior art exists that the porosity is low, pore
Distributing homogeneity is poor, complex manufacturing technology, the problem high to ingredient requirement.A kind of high porosity complex phase porous ceramic film material is provided
Preparation method, wollastonite, dolomite, gangue are respectively prepared powder, then wollastonite and dolomite are mixed, coal by the method
Spoil carries out soaking with mixed acid after heat treatment filtering, and the filter residue and drying obtained makes dried object, then by above-mentioned mixed-powder, dry
The powder that dry thing is made with carborundum, aluminium sesquioxide powder, white carbon black and starch stirs, the mixed-powder that will finally prepare
Load stainless steel mould cold moudling, prepared block pressed compact is carried out high temperature sintering, stand subsequently and to be cooled to room temperature
High porosity complex phase porous ceramic film material.Raw material of the present invention is easy to get, and preparation technology is simple, the porous ceramics porosity made up to
More than 85%, and even air hole distribution, be suitable for industrialized production, have broad mass market prospect.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) weigh 200～300g wollastonite, add and sieve after ball mill pulverizes 30～40min, obtain 120～130 mesh wollastonite
Powder, then weigh 30～50g dolomites, sieve after ball mill pulverizing to obtain 180～200 whitish eye marble powder, by wollastonite powder and
Mixed-powder is obtained after dolomite powder mix homogeneously, standby；
(2) weighing 100～120g gangues, broken, grinding and sieving obtains 100～120 mesh gangue powder, by gangue powder
Put in Muffle furnace, be that 5 DEG C/min is warming up to 300～400 DEG C with heating rate, after heat treatment 20～25min, be cooled to room temperature
Taking out, add in mixed acid by the gangue powder after heat treatment by solid-to-liquid ratio 1:10, after soaking 1～2h, sucking filtration obtains filtering residue, will
Filtering residue is put in vacuum drying oven, is dried 6～8h at 80～90 DEG C, obtains dried object；Described mixed acid is by mass fraction 5% salt
Acid solution and mass fraction 50% sulfuric acid solution 1:1 by volume mixing；
(3) 90～120g carborundums, 50～70g aluminium sesquioxide powder, 20～30g white carbon blacks, 15～20g starch, difference are weighed
By material ball mill pulverizing, sieve to obtain 120～130 mesh powder, adds in high-speed mixer, stirs at 800～1000r/min rotating speeds
Mixing 5～10min, mixes and adds the mixed-powder and 70～80g that 200～250g steps (1) are standby in backward high-speed mixer
Above-mentioned dried object, after continuing mixing 40～50min, obtains mixed-powder；
(4) mixed-powder obtained above is loaded stainless steel mould, cold moudling under the pressure of 100～300MPa, obtain
Block pressed compact, loads block pressed compact in graphite jig, then inserts in discharge plasma sintering stove, and system vacuum is evacuated to 2～6Pa
After carry out high temperature sintering, be 8～10 DEG C with heating rate and be first warming up to 600～800 DEG C, insulation 5～10min after again with the speed that heats up
Rate 15～20 DEG C/min is warming up to 1200～1500 DEG C of heat preservation sinterings 1～2h, be cooled to after sintering room temperature high porosity
Complex phase porous ceramic film material.
The application process of the present invention is: in the tunnel that noise is bigger, appropriate adhesive is coated in the building wall in tunnel
On body, then, the porous ceramics present invention prepared cuts into sheet material of uniform size, is uniformly attached on body of wall, treats adhesive
It is dried, fixes, sound-absorbing wall can be formed.After testing, this material porosity reaches more than 85%, and pore size is 2～5 μm, and space is put down
The most a diameter of 30～50 μm, pore size is consistent, is evenly distributed, and after using the porous ceramic film material sound insulation that the present invention prepares, surveys
Sound be 30～50 decibels, after using 3～5 years, ceramic material does not deforms, fragmentation, obscission, sound-absorbing effect without
Significant change.
The invention has the beneficial effects as follows:
(1) between the porous ceramic film material hole prepared and hole, space is little, even air hole distribution, and the porosity is higher；
(2) the porous ceramic film material size prepared is unrestricted, can the most arbitrarily regulate, and the low technological process of preparation cost
Short, it is possible to achieve industrialized requirement.
Detailed description of the invention
First weigh 200～300g wollastonite, add and sieve after ball mill pulverizes 30～40min, obtain 120～130 mesh
Wollastonite powder, then weigh 30～50g dolomites, sieve after ball mill pulverizing to obtain 180～200 whitish eye marble powder, by wollastonite
Mixed-powder is obtained after powder and dolomite powder mix homogeneously, standby；Weigh 100～120g gangues subsequently, broken, pulverize after
Sieve to obtain 100～120 mesh gangue powder, puts in Muffle furnace by gangue powder, is that 5 DEG C/min is warming up to heating rate
300～400 DEG C, it is cooled to room temperature after heat treatment 20～25min and takes out, by the gangue powder after heat treatment by solid-to-liquid ratio 1:10
Adding in mixed acid, after soaking 1～2h, sucking filtration obtains filtering residue, is put into by filtering residue in vacuum drying oven, is dried 6～8h at 80～90 DEG C,
Obtain dried object；Described mixed acid is to be mixed by mass fraction 5% hydrochloric acid solution and mass fraction 50% sulfuric acid solution 1:1 by volume
Close；Weigh 90～120g carborundums, 50～70g aluminium sesquioxide powder, 20～30g white carbon blacks, 15～20g starch again, respectively will
Material ball mill pulverizing, sieve to obtain 120～130 mesh powder, adds in high-speed mixer, mixed in 800～1000r/min rotating speeds stirrings
Close 5～10min, mix in backward high-speed mixer add 200～250g above-mentioned steps prepare standby mixed-powder and 70～
The above-mentioned dried object of 80g, after continuing mixing 40～50min, obtains mixed-powder；Finally mixed-powder obtained above is loaded stainless
Steel mold, cold moudling under the pressure of 100～300MPa, obtain block pressed compact, block pressed compact is loaded in graphite jig, then
Inserting in discharge plasma sintering stove, system vacuum carries out high temperature sintering after being evacuated to 2～6Pa, is 8～10 DEG C of elder generations with heating rate
It is warming up to 600～800 DEG C, after insulation 5～10min, is warming up to 1200～1500 DEG C of insulations with heating rate 15～20 DEG C/min again
Sintering 1～2h, be cooled to after sintering room temperature high porosity complex phase porous ceramic film material.
Example 1
First weigh 200g wollastonite, add and sieve after ball mill pulverizes 30min, obtain 120 mesh wollastonite powder, then weigh
30g dolomite, sieve after ball mill pulverizing to obtain 180 whitish eye marble powder, after wollastonite powder and dolomite powder mix homogeneously
Obtain mixed-powder, standby；Weighing 100g gangue subsequently, broken, grinding and sieving obtains 100 mesh gangue powder, by gangue
Powder is put in Muffle furnace, is that 5 DEG C/min is warming up to 300 DEG C with heating rate, is cooled to room temperature and takes out after heat treatment 20min,
Adding in mixed acid by the gangue powder after heat treatment by solid-to-liquid ratio 1:10, after soaking 1h, sucking filtration obtains filtering residue, is put into by filtering residue
In vacuum drying oven, at 80 DEG C of dry 6h, obtain dried object；Described mixed acid is by mass fraction 5% hydrochloric acid solution and mass fraction
50% sulfuric acid solution 1:1 by volume mixes；Weigh 90g carborundum, 50g aluminium sesquioxide powder again, 20g white carbon black, 15g starch,
Respectively by material ball mill pulverizing, sieve to obtain 120 mesh powder, adds in high-speed mixer, in the stirring mixing of 800r/min rotating speed
5min, mixes addition 200g above-mentioned steps in backward high-speed mixer and prepares standby mixed-powder and the above-mentioned dried object of 70g, continue
After continuous mixing 40min, obtain mixed-powder；Finally mixed-powder obtained above is loaded stainless steel mould, in the pressure of 100MPa
Cold moudling under power, obtains block pressed compact, is loaded in graphite jig by block pressed compact, then inserts in discharge plasma sintering stove,
System vacuum carries out high temperature sintering after being evacuated to 2Pa, is 8 DEG C with heating rate and is first warming up to 600 DEG C, again to heat up after insulation 5min
15 DEG C/min of speed is warming up to 1200 DEG C of heat preservation sintering 1h, be cooled to after sintering room temperature high porosity complex phase porous ceramics
Material.
This example operation is easy, during use, in the tunnel that noise is bigger, appropriate adhesive is coated in the building in tunnel
On body of wall, then, the porous ceramics present invention prepared cuts into sheet material of uniform size, is uniformly attached on body of wall, treats gluing
Agent is dried, fixes, and can form sound-absorbing wall.After testing, this material porosity reaches 86%, and pore size is 2 μm, and space is the most straight
Footpath is 30 μm, and pore size is consistent, is evenly distributed, after using the porous ceramic film material sound insulation that the present invention prepares, and the sound recorded
Be 30 decibels, after using 3 years, ceramic material does not deforms, fragmentation, obscission, sound-absorbing effect is without significant change.
Example 2
First weigh 250g wollastonite, add and sieve after ball mill pulverizes 35min, obtain 125 mesh wollastonite powder, then weigh
40g dolomite, sieve after ball mill pulverizing to obtain 190 whitish eye marble powder, after wollastonite powder and dolomite powder mix homogeneously
Obtain mixed-powder, standby；Weighing 110g gangue subsequently, broken, grinding and sieving obtains 110 mesh gangue powder, by gangue
Powder is put in Muffle furnace, is that 5 DEG C/min is warming up to 350 DEG C with heating rate, is cooled to room temperature and takes out after heat treatment 23min,
Adding in mixed acid by the gangue powder after heat treatment by solid-to-liquid ratio 1:10, after soaking 1.5h, sucking filtration obtains filtering residue, is put by filtering residue
Enter in vacuum drying oven, at 85 DEG C of dry 7h, obtain dried object；Described mixed acid is to be divided by mass fraction 5% hydrochloric acid solution and quality
Several 50% sulfuric acid solution 1:1 by volume mix；Weighing 105g carborundum, 60g aluminium sesquioxide powder, 25g white carbon black again, 18g forms sediment
Powder, respectively by material ball mill pulverizing, sieve to obtain 125 mesh powder, add in high-speed mixer, in the stirring mixing of 900r/min rotating speed
8min, mixes addition 225g above-mentioned steps in backward high-speed mixer and prepares standby mixed-powder and the above-mentioned dried object of 75g, continue
After continuous mixing 45min, obtain mixed-powder；Finally mixed-powder obtained above is loaded stainless steel mould, in the pressure of 200MPa
Cold moudling under power, obtains block pressed compact, is loaded in graphite jig by block pressed compact, then inserts in discharge plasma sintering stove,
System vacuum carries out high temperature sintering after being evacuated to 4Pa, is 9 DEG C with heating rate and is first warming up to 700 DEG C, again to heat up after insulation 8min
18 DEG C/min of speed is warming up to 1350 DEG C of heat preservation sintering 1.5h, be cooled to after sintering room temperature high porosity complex phase porous pottery
Ceramic material.
This example operation is easy, during use, in the tunnel that noise is bigger, appropriate adhesive is coated in the building in tunnel
On body of wall, then, the porous ceramics present invention prepared cuts into sheet material of uniform size, is uniformly attached on body of wall, treats gluing
Agent is dried, fixes, and can form sound-absorbing wall.After testing, this material porosity reaches 87%, and pore size is 3.5 μm, and space is average
A diameter of 40 μm, pore size is consistent, is evenly distributed, after using the porous ceramic film material sound insulation that the present invention prepares, the sound recorded
Sound is 40 decibels, after using 4 years, ceramic material does not deforms, fragmentation, obscission, sound-absorbing effect is without significant change.
Example 3
First weigh 300g wollastonite, add and sieve after ball mill pulverizes 40min, obtain 130 mesh wollastonite powder, then weigh
50g dolomite, sieve after ball mill pulverizing to obtain 200 whitish eye marble powder, after wollastonite powder and dolomite powder mix homogeneously
Obtain mixed-powder, standby；Weighing 120g gangue subsequently, broken, grinding and sieving obtains 120 mesh gangue powder, by gangue
Powder is put in Muffle furnace, is that 5 DEG C/min is warming up to 400 DEG C with heating rate, is cooled to room temperature and takes out after heat treatment 25min,
Adding in mixed acid by the gangue powder after heat treatment by solid-to-liquid ratio 1:10, after soaking 2h, sucking filtration obtains filtering residue, is put into by filtering residue
In vacuum drying oven, at 90 DEG C of dry 8h, obtain dried object；Described mixed acid is by mass fraction 5% hydrochloric acid solution and mass fraction
50% sulfuric acid solution 1:1 by volume mixes；Weighing 120g carborundum, 70g aluminium sesquioxide powder, 30g white carbon black again, 20g forms sediment
Powder, respectively by material ball mill pulverizing, sieve to obtain 130 mesh powder, adds in high-speed mixer, mixed in the stirring of 1000r/min rotating speed
Close 10min, mix in backward high-speed mixer add 250g above-mentioned steps prepare standby mixed-powder and 80g above-mentioned be dried
Thing, after continuing mixing 50min, obtains mixed-powder；Finally mixed-powder obtained above is loaded stainless steel mould, at 300MPa
Pressure under cold moudling, obtain block pressed compact, block pressed compact loaded in graphite jig, then inserts discharge plasma sintering stove
In, system vacuum carries out high temperature sintering after being evacuated to 6Pa, is 10 DEG C with heating rate and is first warming up to 800 DEG C, after insulation 10min again
Be warming up to 1500 DEG C of heat preservation sintering 2h with 20 DEG C/min of heating rate, be cooled to after sintering room temperature high porosity complex phase is many
Hole ceramic material.
This example operation is easy, during use, in the tunnel that noise is bigger, appropriate adhesive is coated in the building in tunnel
On body of wall, then, the porous ceramics present invention prepared cuts into sheet material of uniform size, is uniformly attached on body of wall, treats gluing
Agent is dried, fixes, and can form sound-absorbing wall.After testing, this material porosity reaches 88%, and pore size is 5 μm, and space is the most straight
Footpath is 50 μm, and pore size is consistent, is evenly distributed, after using the porous ceramic film material sound insulation that the present invention prepares, and the sound recorded
Be 50 decibels, after using 5 years, ceramic material does not deforms, fragmentation, obscission, sound-absorbing effect is without significant change.
Claims (1)
1. the preparation method of a high porosity complex phase porous ceramic film material, it is characterised in that concrete preparation process is:
(1) weigh 200～300g wollastonite, add and sieve after ball mill pulverizes 30～40min, obtain 120～130 mesh wollastonite
Powder, then weigh 30～50g dolomites, sieve after ball mill pulverizing to obtain 180～200 whitish eye marble powder, by wollastonite powder and
Mixed-powder is obtained after dolomite powder mix homogeneously, standby；
(2) weighing 100～120g gangues, broken, grinding and sieving obtains 100～120 mesh gangue powder, by gangue powder
Put in Muffle furnace, be that 5 DEG C/min is warming up to 300～400 DEG C with heating rate, after heat treatment 20～25min, be cooled to room temperature
Taking out, add in mixed acid by the gangue powder after heat treatment by solid-to-liquid ratio 1:10, after soaking 1～2h, sucking filtration obtains filtering residue, will
Filtering residue is put in vacuum drying oven, is dried 6～8h at 80～90 DEG C, obtains dried object；Described mixed acid is by mass fraction 5% salt
Acid solution and mass fraction 50% sulfuric acid solution 1:1 by volume mixing；
(3) 90～120g carborundums, 50～70g aluminium sesquioxide powder, 20～30g white carbon blacks, 15～20g starch, difference are weighed
By material ball mill pulverizing, sieve to obtain 120～130 mesh powder, adds in high-speed mixer, stirs at 800～1000r/min rotating speeds
Mixing 5～10min, mixes and adds the mixed-powder and 70～80g that 200～250g steps (1) are standby in backward high-speed mixer
Above-mentioned dried object, after continuing mixing 40～50min, obtains mixed-powder；
(4) mixed-powder obtained above is loaded stainless steel mould, cold moudling under the pressure of 100～300MPa, obtain
Block pressed compact, loads block pressed compact in graphite jig, then inserts in discharge plasma sintering stove, and system vacuum is evacuated to 2～6Pa
After carry out high temperature sintering, be 8～10 DEG C with heating rate and be first warming up to 600～800 DEG C, insulation 5～10min after again with the speed that heats up
Rate 15～20 DEG C/min is warming up to 1200～1500 DEG C of heat preservation sinterings 1～2h, be cooled to after sintering room temperature high porosity
Complex phase porous ceramic film material.
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Application publication date: 20161207 |