CN106348736A - Method for rapidly curing ceramic slurry - Google Patents
Method for rapidly curing ceramic slurry Download PDFInfo
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- CN106348736A CN106348736A CN201610710499.4A CN201610710499A CN106348736A CN 106348736 A CN106348736 A CN 106348736A CN 201610710499 A CN201610710499 A CN 201610710499A CN 106348736 A CN106348736 A CN 106348736A
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Abstract
The invention discloses a method for rapidly curing ceramic slurry. The method comprises the following steps: firstly, mixing ceramic powder, a dispersant and water and sufficiently carrying out ball milling to prepare the ceramic slurry with a negatively-charged particle surface; then, adding iodate of high-valence metal cations and carrying out the ball milling; stirring the obtained slurry under a vacuum condition and degassing; then adding an esters pH (Potential of Hydrogen) regulator; after uniformly stirring, injecting the slurry into a pore-free mold; storing the pore-free mold at 45 DEG C to 70 DEG C for 15 minutes to 45 minutes; de-molding to obtain a ceramic wet blank; drying the ceramic wet blank to obtain a dry blank; then putting the dry blank into a sintering furnace and sintering to obtain a sintered ceramic body. According to the method provided by the invention, the common effect of decomposing the iodate through temperature control to release the high-valence metal cations and decomposing and regulating the pH value to an isoelectric point through the esters pH regulator realizes rapid curing and molding of the ceramic slurry; the method has the advantages that the method is suitable for any ceramic slurry with negative charges, is rapid in curing speed, high in slurry molding efficiency, environment-friendly, excellent in performance and simple to operate, is convenient for large-scale production and the like.
Description
Technical field
The invention belongs to inorganic non-metallic ceramics curing technical field, more particularly, to a kind of fast setting pottery
The method of porcelain slurry.
Background technology
Direct Coagulation Casting technique (direct coagulation casting, dcc) be using enzyme or from
Body catalytic reaction, make to occur inside slurry chemical reaction come to increase ionic intension in slurry or adjust slurry ph value electric to waiting
Point, to realize the solidification of ceramic size.Wherein, method, hardening time very long (1～3 day) and the ceramic wet of ionic strength are increased
Base easily cracks, thus affecting the performance of pottery；Though adjusting ph value to the good pottery of the method energy processability of isoelectric point, IP
Porcelain, but its ceramic wet blank intensity is too low, and the inconvenient demoulding and later stage are processed.
According to collochemistry principle, schulze-hardy electrostatic valence rule theory is incorporated into by the outstanding person et al. that permitted of Tsing-Hua University
Direct Coagulation Casting technique proposes a kind of new shaping method of ceramics, and that is, directly solidification is injection molded as ceramic high price counter ion
Type technique (direct coagulation casting via high valence counter ions, dcc-hvci), leads to
The controllable release crossing high price counter ion makes ceramic suspension body that in-situ solidifying to occur.The biscuit of ceramics of the method molding has intensity relatively
High (1～2mpa), the advantages of crackle is less, hardening time is shorter, but the method generally need to more than 60 DEG C water bath processing 1～3h
Just enable the solidification of ceramic size, bath temperature is too high, and water bath time is long, blank density all can be led to uneven it is difficult to
The ceramic part in molding large-scale thickness section.
Content of the invention
Disadvantages described above for prior art or Improvement requirement, the invention provides a kind of side of fast setting ceramic size
Method, it decomposes release high valent cationic by temperature control iodate increases ionic strength and esters in ceramic size
Ph regulator decomposes the collective effect close to isoelectric point, IP for the ph value making ceramic size, realizes the fast setting of ceramic size, to solve
Certainly existing pottery high price counter ion Direct Coagulation Casting method length hardening time, solidification temperature height, biscuit lack of homogeneity, one-tenth
The low problem of type efficiency.
For achieving the above object, the present invention proposes a kind of method of fast setting ceramic size, comprises the steps:
(1) ceramic powder, dispersant and water are passed through ball milling mixing uniformly, to prepare the electronegative ceramic slurry of particle surface
Material, wherein, solid volume fraction is 50%～60%, and the quality of dispersant is the 0.5%～3.0% of ceramic powder quality；
(2) add iodate firming agent in the ceramic size obtaining in step (1), and make the concentration of iodate be
4.5g/l～8.0g/l, then ball milling 5～10min under 150～300r/min speed, above-mentioned iodate is slightly soluble at room temperature
Water, raises its dissolubility with temperature and increases, by adjusting the decomposition of temperature control iodate come the ionic strength in strengthening slurry；
(3) the ceramic size stirring degassing 10～30min under vacuum that will obtain after ball milling in step (2), then
Add esters ph regulator, and stirred using Glass rod, wherein, the volume that esters ph regulator adds is ceramic size body
Long-pending 0.5%～3.0%, the decomposition rate of above-mentioned esters ph regulator is accelerated with the rising of temperature, by adjusting temperature control
The decomposition of esters ph regulator processed is adjusting ph to isoelectric point, IP；
(4) slurry obtaining in step (3) is injected in non-porous mold, and at 45～70 DEG C water bath processing 15～
After 45min, the demoulding obtains ceramic wet blank, described ceramic wet blank is vacuum dried under the conditions of 70～80 DEG C 12～24h and obtains pottery
Dry body；
(5) the ceramic dry body obtaining in step (4) is placed in sintering furnace, with 3 DEG C per minute～10 DEG C of heating rate
It is warming up to 1250 DEG C～2200 DEG C, after insulation 2～4h, obtain ceramic sintered bodies.
As it is further preferred that ceramic powder in described step (1) be preferably silicon dioxide, aluminium oxide, stannum oxide,
One or more of silicon nitride, boron nitride, titanium nitride, carborundum, boron carbide and titanium carbide.
As it is further preferred that the dispersant in described step (1) is preferably ammonium citrate, ammonium polyacrylate, tetramethyl
One or more of base ammonium hydroxide, tetraethyl ammonium hydroxide or TPAOH.
As it is further preferred that the esters ph regulator in described step (3) is preferably diacetine, triacetic acid
One or more of in glyceride, gluconic acid lactone or ethyl acetate.
As it is further preferred that ball milling speed in described step (1) is 150～300r/min, Ball-milling Time is 1～
3h.
As it is further preferred that the iodate firming agent in described step (2) is calcium iodate, Magnesium iodate., strontium iodate, iodine
One or more of sour zinc, barium iodate, nickelous iodate and iodic acid yttrium.
As it is further preferred that the Glass rod mixing time in described step (3) is 10～30s, it is slowly stirred to ester
Class ph regulator is uniformly dispersed and does not bring bubble into in slurry.
As it is further preferred that the concentration of described iodate is preferably 6.0g/l～7.5g/l, esters ph regulator adds
Plus volume be preferably ceramic size volume 1.5%～2.5%.In general, by above technology that the present invention is contemplated
Scheme compared with prior art, mainly possesses following technological merit:
1. the present invention provides a kind of temperature control sustained-release high price counter ion and the method adjusting ph fast setting ceramic size, is based on
Decomposition discharges high valent cationic and generation is sour respectively at relatively high temperatures for iodate and esters ph regulator, makes ceramic slurry
Ionic strength in material strengthens and ph value is close to isoelectric point, IP, and both collective effects realize the direct curing molding of ceramic size.
2. the solidification temperature scope of the present invention is relatively low, can achieve the solidification of slurry in 45～70 DEG C of temperature ranges；Solidification
Time is short, can achieve fast setting, substantially increase the shaping efficiency of ceramic size in 15～45min time range.
3. the present invention is suitable for any electronegative ceramic size fast setting, the pottery of plastic various complicated shapes and size
Porcelain part, forming ceramic even green body is preferable, internal stress is little, any surface finish, dimensional accuracy high.
4., compared with traditional Direct Coagulation Casting technique, hardener dose is few, and the method for the present invention for the present invention
Organic substance need not be added, it is to avoid cracking that dumping causes, the defect of deformation.
5. the ceramic dry body density that the present invention prepares be solid density 60%～63%, shrinkage factor be 2.5%～
3.5%, the density of ceramic sintered bodies is more than the 99% of solid density, shrinkage factor 18%～21%.
Brief description
Fig. 1 is the schematic diagram of temperature control sustained-release high price counter ion of the present invention and the method adjusting ph fast setting ceramic size.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with drawings and Examples, right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only in order to explain the present invention, and
It is not used in the restriction present invention.As long as additionally, involved technical characteristic in each embodiment of invention described below
The conflict of not constituting each other just can be mutually combined.
The present invention provide a kind of fast setting ceramic size method, specially a kind of temperature control sustained-release high price counter ion and
The method adjusting ph fast setting ceramic size, on the one hand, it passes through the decomposition of temperature control iodate and discharges high-valency metal sun
Ion, to increase the ionic strength in ceramic size, shown in its chemical formula such as equation (1), rises high-temperature taking calcium iodate as a example,
The release of promotion calcium ion:
On the other hand, the ph value making ceramic size is decomposed close to isoelectric point, IP by temperature control esters ph regulator, with two
As a example acetin, shown in its chemical formula such as equation (2), rise high-temperature, promote the decomposition of diacetine, be conducive to
The generation of acetic acid, adjusts ph to isoelectric point, IP:
In sum, the present invention is under conditions of heating, by increasing ionic strength and to adjust ph common to isoelectric point, IP
Effect, realizes the fast setting of ceramic size, and the method that the present invention adopts has that hardening time is short, solidification temperature is relatively low, biscuit
The advantages of uniformity is preferable, simple to operate, shaping efficiency is high.
The invention mainly includes steps:
(1) by ceramic powder, dispersant and water mix homogeneously, ball milling mixing uniformly, prepares the electronegative pottery of particle surface
Porcelain slurry, wherein ceramic powder volume fraction are 50%～60%, the quality of dispersant be ceramic powder quality 0.5%～
3.0%.When the volume fraction of above-mentioned ceramic powder selects 50%～60%, both can guarantee that the high solid loading of ceramic size, had
Benefit the compactness improving molding biscuit, prevent the deformation in later stage process and cracking；Can guarantee that the low viscosity of ceramic size again,
It is beneficial to degasification and the molding process in ceramic size later stage.Dispersant selects 0.5%～3.0% can make the equal of ceramic particle
Even dispersion is it is ensured that the low viscosity of ceramic size requires.
Specifically, ceramic powder is preferably silicon dioxide, aluminium oxide, stannum oxide, silicon nitride, boron nitride, titanium nitride, carbonization
One of silicon, boron carbide and titanium carbide or two kinds and two or more, dispersant can be selected for ammonium citrate, ammonium polyacrylate, four
One or more of ammonium hydroxide, tetraethyl ammonium hydroxide or TPAOH.
Further, described ball milling speed is 150～300r/min, and Ball-milling Time is 1～3h, under this ball-milling technology
Preferably, slurry preparation efficiency is higher for the uniformity of the ceramic size of preparation.
(2) add firming agent in the ceramic size obtaining in step (1), above-mentioned firming agent is iodate, and iodate adds
After entering ceramic size, the concentration making iodate is 4.5g/l～8.0g/l, and preferred concentration is 6.0g/l～7.5g/l, Ran Hou
Ball milling 5～10min under 150～300r/min speed.Above-mentioned iodate is slightly soluble in water at room temperature, raises its dissolubility with temperature
Increase (i.e. in follow-up water bath processing, with the rising of temperature, the dissolubility of iodate constantly increases), by adjusting temperature
The decomposition controlling iodate carrys out the ionic strength in strengthening slurry.
Wherein, iodate is in calcium iodate, Magnesium iodate., strontium iodate, zinc iodate, barium iodate, nickelous iodate and iodic acid yttrium
Plant or multiple.
(3) by the ceramic size stirring degassing 10～30min under vacuum obtaining in step (2), removed by stirring
Gas 10～30min both can effectively remove the bubble in ceramic size, slurry can be avoided again because standing time is longer and cause
Part settles；It is subsequently adding esters ph regulator, is stirred using Glass rod, esters regulator is chosen as diethyl acid glycerol
One or more of ester, glyceryl triacetate, gluconic acid lactone or ethyl acetate, esters ph regulator add volume be
The 0.5%～3.0% of ceramic size volume, preferred volume fraction addition is 1.5%～2.5%.Above-mentioned esters ph is adjusted
The decomposition rate of agent is accelerated with the rising of temperature (i.e. in follow-up water bath processing, with the rising of temperature, esters ph regulation
The decomposition rate of agent is constantly accelerated), adjust ph to isoelectric point, IP by adjusting the decomposition of temperature control esters ph regulator.
Wherein, the time 10～30s of Glass rod uniform stirring, be slowly stirred to esters ph regulator be uniformly dispersed and without
Enter bubble in slurry.
(4) slurry obtaining in step (3) is injected in non-porous mold, during water bath processing, iodine is controlled by temperature simultaneously
Hydrochlorate decomposes release high valent cationic and esters ph regulator decomposes regulation ph value to the collective effect of isoelectric point, IP, realizes
The curing molding of ceramic size, obtains ceramic wet blank after the demoulding, be vacuum dried 12～24h, in this work under the conditions of 70～80 DEG C
Slowly can effectively exclude the moisture in wet base under skill, it is to avoid cracking in dry run for the wet base, then obtain dry body.
Further, the temperature of described water bath processing is 45～70 DEG C, and the time is 15～45min, can be real under this technique
Effective decomposition of existing iodate, and adjust ph to isoelectric point, IP, to realize ceramic size fast setting at a lower temperature, and can
It is effectively improved the uneven phenomenon of molding biscuit composition.
(5) dry body obtaining in step (4) is placed in sintering furnace, is heated up with 3 DEG C per minute～10 DEG C of heating rate
To 1250 DEG C～2200 DEG C, it is incubated 2～4h, dry body can be prevented effectively under this technique in sintering process due to heating rate mistake
The deformation causing soon and cracking phenomena, then obtain ceramic sintered bodies.
It is below the specific embodiment of the present invention.
Embodiment 1:
6.5g/l calcium iodate, 2.0vol% diacetine solidification 2.0wt% Tetramethylammonium hydroxide are scattered
50vol%sio2Slurry.
By 100 grams of silicon-dioxide powderies, 2.0 grams of Tetramethylammonium hydroxide and 37.7 grams of water mixing, in the ball of 250r/min
Under mill speed, ball milling is prepared into the electronegative ceramic size of the particle surface that solid volume fraction is 50%, then after 1.5 hours
Add the calcium iodate of 0.54g, mixing and ball milling after 8 minutes under the ball milling speed of 250r/min, stirring degassing 15 under vacuum condition
Minute, add 1.66 milliliters of diacetines, Glass rod stir 30 seconds after injection molding, after placing 20 minutes at a temperature of 60 DEG C
The demoulding, is dried 12 hours at 80 DEG C, then is warmed up to 3 hours sintering of 1250 DEG C of insulations with the heating rate of 3 DEG C/min.Made pottery
The relative theory density of porcelain dry body is 60.0%, and shrinkage factor is 2.8%；The relative theory density obtaining ceramic post sintering part is
99.4%, shrinkage factor is 18.0%.
Embodiment 2:
7.5g/l calcium iodate, the 1.5vol% glyceryl triacetate solidification scattered 60vol%al of 0.5wt% ammonium citrate2o3
Slurry.
By 100 grams of alumina powder jointed, 0.5 gram of ammonium citrates and 16.7 grams of water mixing, under the ball milling speed of 200r/min
Ball milling is prepared into the electronegative ceramic size of the particle surface that solid volume fraction is 60% after 2 hours.It is subsequently adding 0.6g's
Calcium iodate, mixing and ball milling after 10 minutes under the ball milling speed of 200r/min, stirring degassing 10 minutes under vacuum condition.Add
1.2 milliliters of glyceryl triacetate, Glass rod stir 15 seconds after injection molding.The demoulding after placing 30 minutes at a temperature of 50 DEG C, at 70 DEG C
Lower drying 24 hours, then 2 hours sintering of 1550 DEG C of insulations are warmed up to the heating rate of 5 DEG C/min.Obtain the phase of ceramic dry body
It is 61.8% to solid density, shrinkage factor is 2.5%；The relative theory density obtaining ceramic post sintering part is 99.5%, shrinkage factor
For 19.2%.
Embodiment 3:
6.0g/l nickelous iodate, the 2.5vol% ethyl acetate solidification scattered 55vol%sno of 2.5wt% ammonium polyacrylate2Slurry
Material.
By 100 grams of stannum oxide powder body, 2.5 grams of ammonium polyacrylates and 16.7 grams of water mixing, in the ball milling speed of 150r/min
Lower ball milling is prepared into the electronegative ceramic size of the particle surface that solid volume fraction is 55% after 3 hours.It is subsequently adding 0.50g
Nickelous iodate, mixing and ball milling after 10 minutes under the ball milling speed of 150r/min, stirring degassing 20 minutes under vacuum condition.Again plus
Enter 2.1 milliliters of ethyl acetate, Glass rod stir 10 seconds after injection molding.The demoulding after placing 45 minutes at a temperature of 45 DEG C, at 80 DEG C
It is dried 24 hours, then 4 hours sintering of 1500 DEG C of insulations are warmed up to the heating rate of 10 DEG C/min.Obtain the relative of ceramic dry body
Solid density is 62.3%, and shrinkage factor is 2.6%；The relative theory density obtaining ceramic post sintering part is 99.6%, and shrinkage factor is
18.7%.
Embodiment 4:
7.0g/l nickelous iodate, 2.5vol% glyceryl triacetate solidification 3.0wt% tetraethyl ammonium hydroxide are scattered
55vol%si3n4Slurry.
By 100 grams of beta-silicon nitride powders, 3.0 grams of tetraethyl ammonium hydroxides and 23.8 grams of water mixing, in the ball milling of 300r/min
Under speed, ball milling is prepared into the electronegative ceramic size of the particle surface that solid volume fraction is 55% after 1 hour.It is subsequently adding
The nickelous iodate of 0.58g, mixing and ball milling after 5 minutes under the ball milling speed of 300r/min, stirring degassing 30 minutes under vacuum condition.
Add 2.1 milliliters of glyceryl triacetate, Glass rod stir 15 seconds after injection molding.The demoulding after placing 35 minutes at a temperature of 70 DEG C,
It is dried 12 hours at 80 DEG C, then 3 hours sintering of 1800 DEG C of insulations are warmed up to the heating rate of 5 DEG C/min.Obtain pottery dry
The relative theory density of base is 63.0%, and shrinkage factor is 3.5%；The relative theory density obtaining ceramic post sintering part is 99.7%,
Shrinkage factor is 20.2%.
Embodiment 5:
7.0g/l calcium iodate, 2.0vol% diacetine solidification 2.0wt% Tetramethylammonium hydroxide are scattered
50vol%sic slurry.
By 100 grams of silicon carbide powders, 2.0 grams of Tetramethylammonium hydroxide and 31.3 grams of water mixing, in the ball milling of 250r/min
Under speed, ball milling is prepared into the electronegative ceramic size of the particle surface that solid volume fraction is 50% after 1 hour.It is subsequently adding
The calcium iodate of 0.58g, mixing and ball milling after 15 minutes under the ball milling speed of 250r/min, 25 points of stirring degassing under vacuum condition
Clock.Add 1.66 milliliters of diacetines, Glass rod stir 15 seconds after injection molding.De- after placing 15 minutes at a temperature of 70 DEG C
Mould, is dried 24 hours at 80 DEG C, then is warmed up to 2 hours sintering of 2200 DEG C of insulations with the heating rate of 5 DEG C/min.Obtain pottery
The relative theory density of dry body is 61.8%, and shrinkage factor is 2.9%；The relative theory density obtaining ceramic post sintering part is
99.7%, shrinkage factor is 21.0%.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not in order to
Limit the present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., all should comprise
Within protection scope of the present invention.
Claims (8)
1. a kind of method of fast setting ceramic size is it is characterised in that comprise the steps:
(1) ceramic powder, dispersant and water are passed through ball milling mixing uniformly, to prepare the electronegative ceramic size of particle surface,
Wherein, ceramic powder volume fraction is 50%～60%, and the quality of dispersant is the 0.5%～3.0% of ceramic powder quality；
(2) in the ceramic size obtaining in step (1) add iodate firming agent, and make iodate concentration be 4.5g/l～
8.0g/l, then ball milling 5～10min under 150～300r/min speed, above-mentioned iodate is slightly soluble in water at room temperature, with temperature
Degree raises its dissolubility and increases；
(3) the ceramic size stirring degassing 10～30min under vacuum that will obtain after ball milling in step (2), is subsequently adding
Esters ph regulator, and stirred using Glass rod, wherein, the volume that esters ph regulator adds is ceramic size volume
0.5%～3.0%, its decomposition rate is accelerated with the rising of temperature；
(4) slurry obtaining in step (3) is injected in non-porous mold, and after water bath processing 15～45min at 45～70 DEG C
The demoulding obtains ceramic wet blank, described ceramic wet blank is vacuum dried under the conditions of 70～80 DEG C 12～24h and obtains ceramic dry body；
(5) the ceramic dry body obtaining in step (4) is placed in sintering furnace, is heated up with 3 DEG C per minute～10 DEG C of heating rate
To 1250 DEG C～2200 DEG C, after insulation 2～4h, obtain ceramic sintered bodies.
2. the method for fast setting ceramic size according to claim 1 is it is characterised in that pottery in described step (1)
Porcelain powder body is preferably silicon dioxide, aluminium oxide, stannum oxide, silicon nitride, boron nitride, titanium nitride, carborundum, boron carbide and titanium carbide
One or more of.
3. the method for fast setting ceramic size according to claim 1 and 2 is it is characterised in that in described step (1)
Dispersant is preferably ammonium citrate, ammonium polyacrylate, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide and TPAOH
One or more of.
4. the method for fast setting ceramic size according to claim 3 is it is characterised in that ester in described step (3)
Class ph regulator is preferably one of diacetine, glyceryl triacetate, gluconic acid lactone and ethyl acetate or many
Kind.
5. the method for fast setting ceramic size according to claim 4 is it is characterised in that ball in described step (1)
Mill speed is 150～300r/min, and Ball-milling Time is 1～3h.
6. the method for fast setting ceramic size according to claim 5 is it is characterised in that iodine in described step (2)
Hydrochlorate firming agent is one or more of calcium iodate, Magnesium iodate., strontium iodate, zinc iodate, barium iodate, nickelous iodate and iodic acid yttrium.
7. the method for fast setting ceramic size according to claim 6 is it is characterised in that glass in described step (3)
Glass rod mixing time is 10～30s, is slowly stirred to esters ph regulator and is uniformly dispersed and does not bring bubble into in slurry.
8. the method for the fast setting ceramic size according to any one of claim 1-7 is it is characterised in that described iodate
Concentration be preferably 6.0g/l～7.5g/l, esters ph regulator add volume be preferably ceramic size volume 1.5%～
2.5%.
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| CN109879665A (en) * | 2019-03-15 | 2019-06-14 | 安徽金岩高岭土科技有限公司 | A kind of high price counter ion Coagulation Casting technique prepares mullite ceramic method |
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