CN100427434C - Method for preparing ceramic with pore gradient - Google Patents
Method for preparing ceramic with pore gradient Download PDFInfo
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- CN100427434C CN100427434C CNB2006100115513A CN200610011551A CN100427434C CN 100427434 C CN100427434 C CN 100427434C CN B2006100115513 A CNB2006100115513 A CN B2006100115513A CN 200610011551 A CN200610011551 A CN 200610011551A CN 100427434 C CN100427434 C CN 100427434C
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Abstract
The present invention relates to a method for preparing ceramic with pore gradient, which belongs to the manufacturing technology of a ceramic material. The method for preparing ceramic with pore gradient is characterized in that deionized water is added in ceramic powder and a dispersing agent first, a slurry is made by ball milling, at the same time, deionized water is added in solidified organic substances, and another slurry is made by ultrasonic dispersion or ball milling; the coal water slurry are mixed quickly in a vacuum static mixer, are injected designed moulds, and are solidified, formed, dried and sintered, and an excellent ceramic material with pore gradient is made. The ceramic powder in the preparation method is one of alumina powder, SiC powder and Si3N4 powder. The dispersing agent is ammonium citrate or tetramethyl ammonium hydroxide, and the solidified organic substances comprise starch, modified starch and one or more of other organic substances which have in-situ controllable solidification property. The preparation method has the advantages of easy operation and high automation, the porosity and the pore size of the prepared ceramic with pore gradient are easily controlled, and the industrial continuous production is easy to realize.
Description
Technical field
The present invention relates to a kind of preparation technology of ceramic with pore gradient, belong to technical field of ceramic material.
Background technology
Ceramic with pore gradient is meant that void content or aperture make the pottery of Gradient distribution with specimen size.The main Application Areas of ceramic with pore gradient comprises: flame-proof thermal insulation material, building thermal insulation material, engine chamber, ceramic separation film, biomaterial etc.At present, the preparation method of ceramic with pore gradient has centrifugal spraying, foam impregnation, the notes technologies such as type, electrochemical deposition moulding of congealing into.But because above-mentioned complicated process of preparation generally needs special equipment and means to realize, productive rate is lower simultaneously, is difficult to satisfy the needs of commercial scale production.
The polysaccharide that starch is made up of glucose, can separate chaining starch and two parts of starch, wherein the former has linear chain structure, the latter has a fork structure, starch granules is about all water insoluble below 50 ℃, but, when starch suspension is heated between 55～90 ℃, the Intermolecular Forces that keeps particle to combine will weaken, this moment, irreversible fast expansion took place owing to absorb water in particle, cause particle size than the initial stage bigger manyfold, particle contacts with each other, become translucent viscous liquid, this phenomenon is called " gelatinization ".The gelatinization of starch is at a certain temperature, and water molecules destroys the hydrogen bond in the starch structure, makes starch chain part unfolded result.Utilize the thickening and the cohesive action of starch pasting, make the ceramic powder particle in the slip fixing in position, can realize the dead size moulding of stupalith, prepared stupalith blank strength is generally at 2～4MPa.
Simultaneously, when starch was heated to 200～550 ℃, oxygenolysis can take place and stay onesize hole in sample in starch granules.Thereby utilize this two specific character of starch can the in-situ preparing porous ceramics.
At present, utilizing the starch formed in situ to prepare ceramic with pore gradient does not appear in the newspapers both at home and abroad.
Summary of the invention
The present invention is directed to the characteristic of ceramic with pore gradient, prepare the preparation technology of a kind of ceramic with pore gradient of proposition of the characteristics innovation of porous ceramics according to the starch in-situ solidifying.The principle that forms the void content gradient in the material is at first to introduce the Gradient distribution of starch content in base substrate, base substrate is discharged back sample void content through high-temperature starch and had the distribution same with starch content.Different types of starch has different particle diameters, utilizes different types of starch to realize in-situ solidifying in view of the above, then has the Gradient distribution of starch particle diameter in the base substrate, and high-temperature starch is discharged the back sample and then had the Gradient distribution of air vent aperture.
A kind of method for preparing ceramic with pore gradient that the present invention proposes, it is characterized in that: described method comprises following each step:
(1) at first in ceramic powder and dispersion agent, adds deionized water, utilize ball milling method to prepare slurry, in solidifying organism, add deionized water simultaneously, utilize ultra-sonic dispersion or ball milling method to prepare slurry, described two kinds of slurries place independently storage tank respectively, and valve control flow rate of slurry is set at storage tank slurry outlet place;
(2) with above-mentioned two kinds of slurries short mix in the vacuum static mixer, the degassing is simultaneously handled;
(3) in the mould that mixed slurry continuous pouring is advanced to design;
(4) in the constant temperature oven that the mould immigration that cast is finished is 55 ℃～90 ℃, be incubated 30 minutes～5 hours, die sealing during insulation;
(5) treat to place room temperature to 60 a ℃ constant temperature oven to leave standstill 12～48 hours together with mould behind the slurry curing, the demoulding afterwards places 80 ℃～110 ℃ baking ovens to continue dry 12～48 hours, and dry back blank strength is between 2～4MPa;
(6) dried base substrate is at first sloughed starch 200～550 ℃ of insulations, temperature rise rate is less than 30 ℃/h in this process, and continuation 1000～2000 ℃ of sintering in high temperature sintering furnace obtain finished product.
In above-mentioned preparation method, the described ceramic powder of step 1 is aluminum oxide powder, SiC powder or Si
3N
4Any in the powder.
In above-mentioned preparation method, the described dispersion agent of step 1 is ammonium citrate, Tetramethylammonium hydroxide or Sudan Gum-arabic.
In above-mentioned preparation method, the described curing organism of step 1 is that starch, treated starch and other have any or several in the organism of the controllable cured character of original position.
In above-mentioned preparation method, described curing organism is yam starch, W-Gum or wheat starch.
In above-mentioned preparation method, described ceramic powder of step 1 and deionized water volume ratio are 40: 10～60; Dispersion agent and solid phase proportion are 0.1～5: 100; Solidifying organism and deionized water volume ratio is 40: 10～60.
Because the present invention according to the design requirements of material, controls the flow velocity of two kinds of slurries, can prepare the pottery with void content gradient in good time; Utilize different sorts starch particle diameter difference, control the kind of starch size in good time, can prepare and have the air vent aperture graded ceramics.Slurry injects designed mould through short mix in the vacuum static mixer, afterwards mould is placed 55～90 ℃ constant temperature oven curing molding, base substrate after the demoulding has starch content Gradient distribution or starch particle diameter Gradient distribution, base substrate removes and sintering through super-dry, starch, and the ceramic with pore gradient material property that makes is good.Utilize that this prepared ceramic with pore gradient is easy to operate, level of automation is high, realize the industrialization continuous production easily; Simultaneously, this technology has reliably, health, economy, Environmental compatibility are good, to characteristics such as human body toxicological harmlesss; Utilizing this technology prepared ceramic with pore gradient void content and pore opening to control easily in addition, is a kind of preparation method who has much prospect therefore.
Description of drawings
Fig. 1 is the preparation principle synoptic diagram of void content Gradient distribution sample of the present invention.
Fig. 2 is the preparation principle synoptic diagram of air vent aperture Gradient distribution sample of the present invention.
Fig. 3 is a process flow diagram of the present invention.1-ceramic size storage tank, 2-starch size storage tank, 3-vacuum static mixer, 4-mould.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
The present invention controls the kind of slurry take-off rate or control starch size according to the material design requirements in good time.The flow velocity of control slurry may be controlled to each position contents of starch of base substrate behind the type, promptly control the void content Gradient distribution of final sample, dissimilar starch are of different sizes distribution, thereby the kind of starch promptly can be controlled aperture Gradient distribution in the final sample in the control slurry; In this technology, can time segment control the kind of various slurry take-off rate starch sizes, prepare discrete ceramic with pore gradient and the uniform porous ceramics of pore through the vacuum short mix.
Evidence: can accomplish the end in view
Embodiment 1:
Utilize the 196g aluminum oxide powder, add the 60ml deionized water, the 0.2g ammonium citrate is as dispersion agent, and ball milling mixing 24h prepares the slurry of good fluidity; Utilize the 60g yam starch, add the 60ml deionized water, be prepared into the slurry of good fluidity through ultra-sonic dispersion; Two kinds of slurries place two storage tanks respectively, control the flow velocity of two kinds of slurries in good time, slurry is through short mix in the vacuum static mixer, injecting diameter is the glass mold of 50mm, die sealing was placed 55 ℃ of constant temperature ovens 30 minutes, place the demoulding after the room temperature 48 hours together with die sealing behind the slurry curing, the demoulding was placed in 80 ℃ of baking ovens dry 48 hours, obtained starch content and carried out the transition to 40% base substrate from 10%; Remove starch through 200～550 ℃ of insulations, two hours sintering of insulation can prepare the sample of void content from 12% continuous transition to 45% in 1450 ℃ of air atmospheres.
Embodiment 2:
Utilize the 120gSiC powder, add 25ml deionized water and 2g Tetramethylammonium hydroxide and do dispersion agent, ball milling mixing 48h prepares the slurry of good fluidity; Utilize the 90g W-Gum, add the 40ml deionized water, be prepared into the slurry of good fluidity through ultra-sonic dispersion, two kinds of slurries place two storage tanks respectively, control the flow velocity of two kinds of slurries in good time, slurry is through short mix in the vacuum static mixer, injection is of a size of the punching block of 30mm * 20mm * 10mm, die sealing was placed 75 ℃ of constant temperature ovens two hours, place the demoulding afterwards in dry 24 hours of 40 ℃ of constant temperature ovens together with die sealing behind the slurry curing, the demoulding was placed in 100 ℃ of baking ovens dry 24 hours, can prepare starch content and carry out the transition to 30% base substrate from 5%; Remove starch through 200～550 ℃ of insulations, two hours sintering of insulation can prepare the sample of void content from 8% continuous transition to 40% in 1850 ℃ of vacuum atmospheres.
Embodiment 3:
Utilize 200gSi
3N
4Powder adds 16ml deionized water and 16g Sudan Gum-arabic and does dispersion agent, and ball milling mixing 36h prepares the slurry of good fluidity; Utilize the 120g wheat starch, add the 20ml deionized water, be prepared into the slurry of good fluidity through ball milling, two kinds of slurries place two storage tanks respectively, control the flow velocity of two kinds of slurries in good time, slurry is through short mix in the vacuum static mixer, injection is of a size of the punching block of 30mm * 20mm * 10mm, die sealing was placed 90 ℃ of constant temperature ovens five hours, place the demoulding afterwards in dry 12 hours of 60 ℃ of constant temperature ovens together with die sealing behind the slurry curing, the demoulding was placed in 110 ℃ of baking ovens dry 12 hours, can prepare starch content and carry out the transition to 30% base substrate from 5%; Remove starch through 200～550 ℃ of insulations, two hours sintering of insulation can prepare the sample of void content from 8% continuous transition to 40% in 1800 ℃ of nitrogen atmospheres.
Claims (3)
1, a kind of method for preparing ceramic with pore gradient is characterized in that: described method comprises following each step:
(1) at first in ceramic powder and dispersion agent, adds deionized water, utilize ball milling method to prepare slurry, in solidifying organism, add deionized water simultaneously, utilize ultra-sonic dispersion or ball milling method to prepare slurry, described two kinds of slurries place independently storage tank respectively, valve control flow rate of slurry is set at storage tank slurry outlet place, and described ceramic powder is aluminum oxide powder, SiC powder or Si
3N
4Any in the powder; Described dispersion agent is ammonium citrate, Tetramethylammonium hydroxide or Sudan Gum-arabic; Described curing organism is that starch, treated starch and other have any or several in the organism of the controllable cured character of original position;
(2) with above-mentioned two kinds of slurries short mix in the vacuum static mixer, the degassing is simultaneously handled;
(3) in the mould that mixed slurry continuous pouring is advanced to design;
(4) in the constant temperature oven that the mould immigration that cast is finished is 55 ℃～90 ℃, be incubated 30 minutes～5 hours, die sealing during insulation;
(5) treat to place room temperature to 60 a ℃ constant temperature oven to leave standstill 12～48 hours together with mould behind the slurry curing, the demoulding afterwards places 80 ℃～110 ℃ baking ovens to continue dry 12～48 hours, and dry back blank strength is between 2～4MPa;
(6) dried base substrate is at first sloughed the curing organism 200～550 ℃ of insulations, temperature rise rate is less than 30 ℃/h in this process, and continuation 1000～2000 ℃ of sintering in high temperature sintering furnace obtain finished product.
2, according to the described preparation method of claim 1, it is characterized in that: described curing organism is yam starch, W-Gum or wheat starch.
3, according to the described preparation method of claim 1, it is characterized in that: described ceramic powder of step 1 and deionized water volume ratio are 40: 10～60; Dispersion agent and solid phase proportion are 0.1～5: 100; Solidifying organism and deionized water volume ratio is 40: 10～60.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101293784B (en) * | 2007-04-25 | 2011-09-28 | 中原工学院 | Method of preparing multi-gas hole ceramic |
| CN102060563A (en) * | 2010-11-11 | 2011-05-18 | 九江学院 | Quartz ceramic material with porous gradient structure and preparation process thereof |
| CN102320856B (en) * | 2011-08-24 | 2013-06-19 | 中国科学院上海硅酸盐研究所 | Method for preparing porous silicon-nitride ceramic material |
| CN102701778B (en) * | 2012-06-01 | 2013-10-16 | 清华大学 | Preparation method for ceramic film with hierarchical pore structure |
| CN105777082B (en) * | 2016-03-15 | 2018-11-30 | 武汉理工大学 | A kind of method that starch pregel consolidation in-situ forming prepares nano aluminium oxide ceramics |
| CN109676776B (en) * | 2019-03-01 | 2019-11-08 | 天津大学 | A kind of ceramic membrane and preparation method thereof of aperture distribution gradient |
| CN114050007A (en) * | 2021-11-25 | 2022-02-15 | 萍乡市长岭电瓷制造有限公司 | Rotary cantilever porcelain insulator and preparation method thereof |
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| CN1513811A (en) * | 2003-08-22 | 2004-07-21 | 清华大学 | Cermic Sizing material fast and controllable solidfying colloied state shaping method and device |
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