CN1513811A - Cermic Sizing material fast and controllable solidfying colloied state shaping method and device - Google Patents
Cermic Sizing material fast and controllable solidfying colloied state shaping method and device Download PDFInfo
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Abstract
A process and apparatus for controllable fast solidification of shaped colloidal ceramics are disclosed. Said apparatus is composed of two vacuum storage tanks for different ceramic slurries, mixing system, diaphragm-type metering unit, high-pressure opposite jetting mixer, static mier, and mould. Said process includes stirring two ceramics slurries in vacuum state respectively, fostly injecting them in static mixer, high-pressure opposite jetting mixing, injecting in vacuum mould, and fast reaction and solidification. Its advantages are uniform solidifying and no internal stress.
Description
Technical field
The invention belongs to the forming process of ceramics technology, particularly under vacuum condition, utilize the different qualities rapid reaction of each ingredients suspension body and the fast controllable curing colloidal shaping method of a kind of ceramic size and the device of curing molding.
Background technology
The preparation technology of high performance ceramic material and parts is prerequisites of stupalith development and application.And moulding technology plays a part to form a connecting link in the preparation process of whole stupalith, is reliability, yield rate and the repeatable key that guarantees stupalith and parts, and is directly related with industrialization and large-scale production.Enter after the nineties, round improving the ceramic body homogeneity and solving the stupalith reliability problems, colloidal state consolidation in-situ forming technology is arisen at the historic moment and is become the focus of research, gel casting forming (Gelcasting), temperature-induced flocculation moulding (Temperature Induced Floculation), directly solidifies casting (DirectCoagulation Casting) etc. and occurs in succession.The common feature of these forming techniques is to realize making pottery the in-situ solidifying moulding of slurry body, and the ceramic body density distribution of acquisition is even, any surface finish; And the organic content that uses is lower, has avoided long-time binder removal and cracking problem.But, all be to bring out ceramic slurry curing as principal element by temperature, curing occurs in certain temperature range, and there is thermograde in suspensoid inside.When temperature reaches the solidified stagnation point, at first solidify in the inner part that can take place of suspensoid, this has just caused the problem of two aspects: slurry just may not solidify when injecting mould, or after injecting mould the long period also uncured, perhaps in mould, solidify the lasting long period.Owing to have thermograde in suspensoid inside, must cause the solidified ununiformity, thereby cause the inner internal stress that produces of base substrate, in subsequent drying and sintering process, easily form defective.
Overcome the above problems, ceramic size viscosity after injecting mould is increased sharply and almost curing simultaneously of each several part, finally become the inflexible base substrate.And key wherein just is to grasp control solidified processing parameter, and must make slurry was stable before injecting mould, had good flowability, and did not contain bubble; And after injecting mould, can solidify rapidly.The inventor proposes in patent ZL 00 1 7495.4 places ceramic size in the hopper of flow casting molding device, and will cause the solidified initiator to be sprayed on the casting belt; When slurry flows on the casting belt, solidify immediately and take place; If slurry does not contact initiator and just can not solidify.This is the blank of fast controllable curing thought.At application number is the method that a kind of on-line mixing is implemented colloidal formation that proposes in 01132070.2 the patent, be solidified ceramic size or additive separated deposit can take place after the mixing in two or more containers, inject the on-line mixing device of sealing by the pump pressurization, each raw material mixes under the effect of stirring during by mixing tank, then from spout ejection curing molding.This method has realized the controllability of solidification process, but owing to adopt the mode that stirs to mix, must cause entrained gas in the slurry, produces bubble in the slurry thereby make, and influences the quality of ceramic; In addition, this method is difficult to guarantee the solidified homogeneity; This method is longer set time simultaneously, is 10 minutes to 1 hour, and efficient is not high.
Summary of the invention
The objective of the invention is to propose under vacuum condition, to utilize the different qualities rapid reaction of each ingredients suspension body and the fast controllable curing colloidal shaping method of a kind of ceramic size and the device of curing molding.
The fast controllable curing colloidal shaping method of described ceramic size divides following three steps:
Step 1: ceramic size branch component is stored in respectively in the different storage tanks, but prolonged preservation during each component Individual existence and not solidifying, slurry viscosity＜1Pas, slurry temperature can be controlled between 0～80 ℃, under vacuum state, stir, and slurry is in the self-circulation state, removes the bubble in the slurry and not to precipitate guaranteeing.
Step 2: during mixed slurry, need the quantity of slurry by the metering surge pump First Astronautic Research Institute for Measurement and Test, each component ceramic size injects the static mixer uniform mixing fast by high pressure 1～8Mpa correlation in 0.5～10 second short period of time, because in high pressure correlation and the static mixer is vacuum state, can not cause the generation of bubble in the slurry in the blended process.
Step 3: under the effect of pressure, inject the mould that has vacuumized from the slurry of static mixer ejection, utilize the different qualities rapid reaction and the curing molding of each component slurry, obtain ceramic.
Realize that by described three steps several approach of rapid reaction and curing molding are:
(1) ceramic size is divided into: the electronegative B component of the A component of ceramic particle positively charged and ceramic particle, with A, B two component short mix and curing molding.
(2) the A component contains and the charged identical high valence ion of this component; The B component has opposite electric charge with the A component, and it is homo-ion equally also to contain the high price identical with the B component.When A, B two component short mix,, and cause slurry fast curing-formed because the two has the interaction of opposite electric charge and high valence ion.
(3) disperse same suspensoid with the antipodal dispersion agent of character, when their short mix, because the interaction of dispersion agent increases sharply and curing molding the viscosity of suspensoid.
(4) directly solidify in the casting technology existing, biological enzyme and ceramic size are placed one, and independently batch can and ceramic size place the another one batch can, when these two batch can short mix, biological enzyme and ceramic size generation chemical reaction, slurry is fast curing-formed.
(5) in existing gel casting forming technology, catalyzer, organic monomer solution and ceramic size are placed an independently batch can; With initiator with do not contain monomeric ceramic size and place the another one batch can.When these two batch can short mix, the trigger monomer polymerization, slurry is fast curing-formed.
The antipodal dispersion agent of described character comprises citric acid ammonia and Tetramethylammonium hydroxide, citric acid ammonia and polymethyl acrylic acid ammonia and calcium chloride electrolyte and ammonium sulfate ionogen.
Described biological enzyme comprises urine enzyme, huge beans urine enzyme, urease.
Described catalyzer comprises Tetramethyl Ethylene Diamine.
Described initiator comprises ammonium persulphate, hydrogen peroxide.
Described organic monomer is acrylamide monomer and methylene-bisacrylamide.
The fast controllable curing colloidal formation of described realization ceramic size device stores the different components ceramic size respectively by two-way vacuum storing and mixing system, diaphragm type metering unit by separately is connected with high pressure correlation mixing device, again with static mixer, mould UNICOM; Comprise following each several part composition: storage tank 1, storage tank 2, internal recycle valve 3, internal recycle valve 4, outer circulation valve 5, outer circulation valve 6, mixing valve 7, mixing valve 8, static mixer 9, mould 10, vacuum valve 11, vacuum valve 12, diaphragm type metering unit 13, diaphragm type metering unit 14, support 15, agitator motor 16, agitator motor 17, high pressure correlation mixing device 18, water cleaning system 19 automatically.
The invention has the beneficial effects as follows the different qualities rapid reaction and the curing molding that under vacuum condition, utilize each ingredients suspension body, there is not thermograde in suspensoid inside, solidify evenly, the inner internal stress free of base substrate, overcome the deficiency that in subsequent drying and sintering process, easily forms defective, can obtain high-quality ceramic.The slurry curing time is short, and generally between 1～60 second, the present invention has the automatization level of height, is fit to large-scale production.
Description of drawings
Fig. 1 is the fast controllable curing colloidal formation of a ceramic size apparatus structure synoptic diagram.
Embodiment
The present invention utilizes fast controllable curing colloidal shaping method of a kind of ceramic size of the different qualities rapid reaction of each ingredients suspension body and curing molding and device under vacuum condition.The fast controllable curing colloidal shaping method of this ceramic size divides following three steps:
Step 1: ceramic size branch component is stored in respectively in the different storage tanks, but prolonged preservation during each component Individual existence and not solidifying, slurry viscosity＜1Pas, slurry temperature can be controlled between 0～80 ℃, under vacuum state, stir, and slurry is in the self-circulation state, removes the bubble in the slurry and not to precipitate guaranteeing.
Step 2: during mixed slurry, need the quantity of slurry by the metering surge pump First Astronautic Research Institute for Measurement and Test, (under 1～8MPa) the effect each component is injected static mixer fast at pressure, (0.5～10 second) by high pressure (mix, and then by static mixer guarantee many component material uniform mixing in a short period of time by 1～8Mpa) correlation for ceramic size.Because in high pressure correlation and the static mixer is vacuum state, can not cause the generation of bubble in the slurry in the blended process.
Step 3: under the effect of pressure, inject the mould that has vacuumized from the slurry of static mixer ejection, utilize the different qualities rapid reaction and the curing molding of each component slurry, obtain ceramic.
Realize that by described three steps several approach of rapid reaction and curing molding are:
(1) ceramic size is divided into: the electronegative B component of the A component of ceramic particle positively charged and ceramic particle, with A, B two component short mix and curing molding.
(2) the A component contains and the charged identical high valence ion of this component; The B component has opposite electric charge with the A component, and it is homo-ion equally also to contain the high price identical with the B component.When A, B two component short mix,, and cause slurry fast curing-formed because the two has the interaction of opposite electric charge and high valence ion.
(3) disperse same suspensoid with the antipodal dispersion agent of character, when their short mix, because the interaction of dispersion agent increases sharply and curing molding the viscosity of suspensoid.
(4) directly solidify in the casting technology existing, biological enzyme and ceramic size are placed one, and independently batch can and ceramic size place the another one batch can, when these two batch can short mix, biological enzyme and ceramic size generation chemical reaction, slurry is fast curing-formed.
(5) in existing gel casting forming technology, catalyzer, organic monomer solution and ceramic size are placed an independently batch can; With initiator with do not contain monomeric ceramic size and place the another one batch can.When these two batch can short mix, the trigger monomer polymerization, slurry is fast curing-formed.
The antipodal dispersion agent of described character comprises citric acid ammonia and Tetramethylammonium hydroxide, citric acid ammonia and polymethyl acrylic acid ammonia, calcium chloride electrolyte and ammonium sulfate ionogen.
Described biological enzyme comprises urine enzyme, huge beans urine enzyme, urease.
Described catalyzer comprises Tetramethyl Ethylene Diamine.
Described initiator comprises ammonium persulphate, hydrogen peroxide.
Described organic monomer is acrylamide monomer and methylene-bisacrylamide.
Realize that the fast controllable curing colloidal formation of ceramic size device stores the different components ceramic size respectively by two-way vacuum storing and mixing system, the diaphragm type metering unit by separately is connected with high pressure correlation mixing device, again with static mixer, mould UNICOM; This device has the automatization level of height, and collection stirring, refrigeration, metering, froth in vacuum, batch mixing, injection, pressurize are one, and its working process is:
Storage tank 1 and storage tank 2 are stored two kinds of ceramic sizes of A, B respectively.A material and B material can not solidify when depositing separately.When equipment is in recurrent state, opens vacuum valve 11,12 and vacuumize; Opening agitator motor 16,17 stirs; A material and B material internal recycle valve 3,4 and outer circulation valve 5,6 are all opened, and this moment, two kinds of slurries were in recurrent state, did not precipitate.When equipment was in the hybrid injection state, the recycle valve 3,4,5,6 of A material and B material all cut out, and mixing valve 7,8 is opened, and two kinds of slurries are in that (static mixer 9 by being in vacuum state under 1～8MPa) the pressure mixes in a short period of time at this moment.The amount that enters the ceramic size of static mixer is controlled by diaphragm type metering unit 13,14.The ceramic size that mixes injects the mould 10 that has vacuumized under the effect of pressure.Mould 10 is the opening and closing left and right structure, adopts support 15 to support, and the folding of mould 10 and injection pressurize action provide power by a Hydraulic Station, and Hydraulic Station has safety protection function by electric time variable control.Material feeding finishes, and starts the pressurize oil cylinder to mould 10 pressurizes, and compound is fully solidified; The curing cycle of product is determined by production technique, die sinking pickup behind the curing molding, and remove mould running channel and waste material.For embodiment the present invention is further specified again below.
The moulding of embodiment 1 alumina-ceramic
α-Al
2O
3Be commercially available industrial raw material, the particulate diameter is that shape is comparatively even about 2 μ m.Use the salt acid for adjusting pH value in deionized water between 3.5～4, add alumina-ceramic powder 6Kg, ball milling is after 24 hours, and being mixed with viscosity is 280mPas, and volume fraction is 60% suspensoid, places the A batch can, at this moment the aluminum oxide positively charged.Use ammonium citrate as dispersion agent in deionized water, the pH value adds alumina-ceramic powder 6Kg between 5～6, behind the ball milling 24 hours, being mixed with viscosity is 200mPas, and volume fraction is 60% suspensoid, place the B batch can, this moment is because the adsorption aluminum oxide of ammonium citrate is electronegative.Slurry in two batch cans of A, B measures 50ml respectively by METERING DIAPHRAGM PUMPS, goes in the static mixing tank by 8MPa high pressure vacuum correlation, and uniform mixing in 0.5 second injects the positive electronegativity neutralization of mould rear oxidation aluminum particulate, and suspensoid is fast curing-formed.
The moulding of embodiment 2 alumina-ceramic
α-Al
2O
3Be commercially available industrial raw material, the particulate diameter is about 0.5 μ m, is shaped as sphere.In the deionized water of 1000ml, use the salt acid for adjusting pH value between 3.5～4, the calcium chloride electrolyte 5g that adds alumina-ceramic powder 6Kg and 0.4mmol/l, behind the ball milling 24 hours, being mixed with viscosity is 360mPas, volume fraction is 60% suspensoid, place the A batch can, at this moment the aluminum oxide positively charged.In the 1000ml deionized water, use the 5g ammonium citrate as dispersion agent, the pH value is between 5～6, the ammonium sulfate ionogen 5g that adds alumina-ceramic powder 6Kg and 0.4mmol/l, behind the ball milling 24 hours, being mixed with viscosity is 300mPas, volume fraction is 60% suspensoid, places the B batch can, and this moment is because the adsorption aluminum oxide of ammonium citrate is electronegative.Slurry in two batch cans of A, B measures 50ml respectively by METERING DIAPHRAGM PUMPS, mixes and static mixer uniform mixing in 0.5 second the not only positive electronegativity neutralization of alumina particle behind the injection mould, and high valence ion Ca by 5MPa high pressure vacuum correlation
2+To the rapid effect of electronegative alumina particle, SO
4 2-To the rapid effect of positively charged alumina particle, suspensoid is fast curing-formed, and curing speed is far above embodiment 1, and blank strength also is higher than embodiment 1.
The moulding of embodiment 3 silicon carbide ceramics
SiC is commercially available industrial raw material, and the particulate diameter is about 0.7 μ m.Contain the acrylamide monomer of 16wt% and the premixed liquid of methylene-bisacrylamide with the deionized water preparation.The ratio of methylene-bisacrylamide and acrylamide is 1: 12.A group powder prepares the silicon carbide ceramics concentrated suspension of 55vol% volume fraction with this premixed liquid, adds the catalyzer Tetramethyl Ethylene Diamine simultaneously, and ball milling is after 24 hours, and viscosity is less than 100mPas.The B component directly with the silicon carbide ceramics concentrated suspension of deionized water configuration 55vol% volume fraction, adds initiator ammonium persulfate or hydrogen peroxide 5g simultaneously, and ball milling is after 24 hours, and viscosity is less than 150mPas.Slurry in two batch cans of A, B measures 350ml respectively by METERING DIAPHRAGM PUMPS, mixes and static mixer uniform mixing in 1 second by the high pressure vacuum correlation, and the rapid polymerization of acrylamide behind the injection mould, suspensoid is fast curing-formed.
The moulding of embodiment 4 zirconia ceramicss
ZrO
2Be the chemical coprecipitation preparation, the particulate diameter is about 70nm.The A component adds the citric acid ammonia dispersion agent of volume fraction 0.5% in ionized water, add Zirconium powder 6Kg then, and ball milling is after 24 hours, and configuration volume fraction 48%, viscosity are less than the zirconia ceramics concentrated suspension of 200mPas.The B component also adds the polymethyl acrylic acid ammonia dispersion agent of volume fraction 0.5% at deionized water, add Zirconium powder 6Kg then, and ball milling is after 24 hours, and configuration volume fraction 40%, viscosity are less than the zirconia ceramics concentrated suspension of 200mPas.Slurry in two batch cans of A, B measures 50ml respectively by METERING DIAPHRAGM PUMPS, mix and static mixer uniform mixing in 1 second by 1MPa high pressure vacuum correlation, inject behind the mould because the interaction of dispersant A 15 and ZA280, thereby cause suspensoid fast curing-formed.
The moulding of embodiment 5 alumina-ceramic
α-Al
2O
3Be commercially available industrial raw material, the particulate diameter is about 0.5 μ m, is shaped as sphere.Use the salt acid for adjusting pH value in the deionized water of 1000ml between 3.5～4, add alumina-ceramic powder 6Kg and 100g urease, ball milling is after 24 hours, being mixed with viscosity is 160mPa.s, volume fraction is 60% suspensoid, places the A batch can, and the temperature of slurry is 30 ℃.Use the salt acid for adjusting pH value in the deionized water of 1000ml between 3.5～4, add the huge beans urine of alumina-ceramic powder 6Kg and 5g enzyme (300unit/g), ball milling is after 24 hours, being mixed with viscosity is 160mPas, volume fraction is 60% suspensoid, places the B batch can, and the temperature of slurry is 30 ℃.Slurry in two batch cans of A, B measures 50ml respectively by METERING DIAPHRAGM PUMPS, mix and static mixer uniform mixing in 0.5 second by 3MPa high pressure vacuum correlation, inject behind the mould because the temperature of slurry is 30 ℃, huge beans urine enzyme and urease rapid reaction, the pH value is adjusted to the iso-electric point of aluminum oxide, and suspensoid is fast curing-formed.
Claims (7)
1. fast controllable curing colloidal shaping method of ceramic size, it is characterized in that: the fast controllable curing colloidal shaping method of described ceramic size divides following three steps:
Step 1: ceramic size branch component is stored in respectively in the different storage tanks, but prolonged preservation during each component Individual existence and not solidifying, slurry viscosity＜1Pas, slurry temperature can be controlled between 0～80 ℃, under vacuum state, stir, and slurry is in the self-circulation state, removes the bubble in the slurry and not to precipitate guaranteeing;
Step 2: during mixed slurry, need the quantity of slurry by the metering surge pump First Astronautic Research Institute for Measurement and Test, (under 1～8MPa) the effect each component is injected static mixer fast at pressure, ceramic size (0.5～10 second) in a short period of time passes through high pressure (1～8Mpa) correlation mixing, and then guarantee many components material uniform mixing by static mixer, because in high pressure correlation and the static mixer is vacuum state, can not cause the generation of bubble in the slurry in the blended process;
Step 3: under the effect of pressure, inject the mould that has vacuumized from the slurry of static mixer ejection, utilize the different qualities rapid reaction and the curing molding of each component slurry, obtain ceramic; Realize that by described three steps several approach of rapid reaction and curing molding are:
(1) ceramic size is divided into: the electronegative B component of the A component of ceramic particle positively charged and ceramic particle, with A, B two component short mix and curing molding;
(2) the A component contains and the charged identical high valence ion of this component; The B component has opposite electric charge with the A component, and it is homo-ion equally also to contain the high price identical with the B component; When A, B two component short mix,, and cause slurry fast curing-formed because the two has the interaction of opposite electric charge and high valence ion;
(3) disperse same suspensoid with the antipodal dispersion agent of character, when their short mix, because the interaction of dispersion agent increases sharply and curing molding the viscosity of suspensoid;
(4) directly solidify in the casting technology existing, biological enzyme and ceramic size are placed one, and independently batch can and ceramic size place the another one batch can; When these two batch can short mix, biological enzyme and ceramic size generation chemical reaction, slurry is fast curing-formed;
(5) in existing gel casting forming technology, catalyzer, organic monomer solution and ceramic size are placed an independently batch can; With initiator with do not contain single body ceramic size and place the another one batch can, when these two batch can short mix, the trigger monomer polymerization, slurry is fast curing-formed.
2. according to the fast controllable curing colloidal shaping method of the described ceramic size of claim 1, it is characterized in that: the antipodal dispersion agent of described character comprises citric acid ammonia and Tetramethylammonium hydroxide, citric acid ammonia and polymethyl acrylic acid ammonia.
3. according to the fast controllable curing colloidal shaping method of the described ceramic size of claim 1, it is characterized in that: described biological enzyme comprises urine enzyme, huge beans urine enzyme, urease.
4. according to the fast controllable curing colloidal shaping method of the described ceramic size of claim 1, it is characterized in that: described catalyzer comprises Tetramethyl Ethylene Diamine.
5. according to the fast controllable curing colloidal shaping method of the described ceramic size of claim 1, it is characterized in that: described initiator comprises ammonium persulphate, hydrogen peroxide.
6. according to the fast controllable curing colloidal shaping method of the described ceramic size of claim 1, it is characterized in that: described organic monomer is acrylamide monomer and methylene-bisacrylamide.
7. realize the fast controllable curing colloidal formation of ceramic size device for one kind, it is characterized in that: the fast controllable curing colloidal formation of described realization ceramic size device stores the different components ceramic size respectively by two-way vacuum storing and mixing system, diaphragm type metering unit by separately is connected with high pressure correlation mixing device, again with static mixer, mould UNICOM; Comprise following each several part composition: storage tank (1), storage tank (2), internal recycle valve (3), internal recycle valve (4), outer circulation valve (5), outer circulation valve (6), mixing valve (7), mixing valve (8), static mixer (9), mould (10), vacuum valve (11), vacuum valve (12), diaphragm type metering unit (13), diaphragm type metering unit (14), support (15), agitator motor (16), agitator motor (17), high pressure correlation mixing device (18), water cleaning system (19) automatically.
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| CN100427434C (en) * | 2006-03-24 | 2008-10-22 | 清华大学 | Method for preparing ceramic with pore gradient |
| CN100371064C (en) * | 2006-03-31 | 2008-02-27 | 清华大学 | System for preparing gel bead |
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| CN102672875B (en) * | 2012-01-11 | 2015-06-24 | 河南科技大学 | Multifunctional reacting, injecting and moulding equipment |
| CN103862593A (en) * | 2014-03-26 | 2014-06-18 | 杨恩霖 | Epoxy resin encapsulation machine set for unblocked encapsulation and encapsulation method |
| CN104402456B (en) * | 2014-10-31 | 2017-04-19 | 中航复合材料有限责任公司 | Self-foaming injection-molding gel-forming porous ceramic preparation method |
| CN104402456A (en) * | 2014-10-31 | 2015-03-11 | 中航复合材料有限责任公司 | Self-foaming injection-molding gel-forming porous ceramic preparation method |
| CN105128128A (en) * | 2015-09-16 | 2015-12-09 | 华中科技大学 | Mold-free material forming method and device |
| CN105753479A (en) * | 2016-03-09 | 2016-07-13 | 苏州莱特复合材料有限公司 | Method for preparing zirconium boride/silicon carbide ceramic material |
| CN108191430A (en) * | 2018-01-18 | 2018-06-22 | 昆明理工大学 | A kind of equipment for producing lanthanum calcium manganese oxygen powder in batches |
| CN108191430B (en) * | 2018-01-18 | 2020-11-17 | 昆明理工大学 | Equipment for producing lanthanum calcium manganese oxygen powder in batches |
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