CN108569900A - A kind of rapid shaping microwave-medium ceramics and preparation method thereof - Google Patents
A kind of rapid shaping microwave-medium ceramics and preparation method thereof Download PDFInfo
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- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
The invention discloses a kind of rapid shaping microwave-medium ceramics and preparation method thereof,Cross-linked scaffold as gel injection-moulding is mixed to get by using biomolecule material and plasticiser and deionized water,Biomolecule material can form hydrogen bond with plasticiser in the solution,Green strength is improved as plasticiser,Ceramic powder is individually mixed with remaining deionized water,It avoids ceramic powder from directly being mixed with the cross-linked scaffold as gel injection-moulding and gluing phenomenon occurs,The full cross-linked skeleton of ceramic powder is set to be uniformly mixed,It glues and is sintered finally by row,At a certain temperature rapidly at porcelain,It is avoided while greatly reducing the sample preparation time due to the viscous defect not exclusively generated of organic matter row,It is hereby achieved that the microwave-medium ceramics of function admirable,Microwave-medium ceramics sample made from this method possesses more excellent performance compared to using sample made from identical powder conventional solid-state method,Its dielectric loss reduces 26.01%,Q-unloaded improves 35.6%,QF values improve 76.85%.
Description
Technical field
The invention belongs to microwave-medium ceramics manufacturing fields, and in particular to a kind of rapid shaping microwave-medium ceramics and its system
Preparation Method.
Background technology
Microwave-medium ceramics (MWDC) refer to be applied to microwave frequency band (mainly UHF, SHF frequency range, 300MHz~
300GHz) as dielectric material and the ceramics of one or more functions are completed in circuit, be recent domestic to microwave-medium
One hot spot direction in investigation of materials field.But it in order to meet the microwave parameters requirement of device, generally requires ceramics sample
It is processed into special shape such as round platform etc., entire manufacturing process can be caused time-consuming if being continuing with conventional solid technique.
Gelcasting Technique (Gel-casting) is the last century 90's by U.S.'s Oak Ridge National Laboratory rate
The advanced ceramic forming technique of one kind first proposed.Its basic principle is the cross-linked network by using organic matter as skeleton pair
Ceramic powder is wrapped, then viscous by organic matter removal by arranging, so that ceramic powder completes formed in situ after sintering.
The technique has many advantages, such as that molding is fast, simple process, can make complex shape appearance sample.But exist simultaneously following problem：
Organic monomer have certain toxicity, sample homogeneity it is poor, it is interior have bubble hole etc., so not yet applying in microwave-medium ceramics system
Standby field.
Invention content
The purpose of the present invention is to provide a kind of rapid shaping microwave-medium ceramics and preparation method thereof, to overcome existing skill
The deficiency of art.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of rapid shaping microwave-medium ceramics, are prepared by the raw material based on following quality parts ratio：Ceramic powder：
Deionized water=(18-22)：(23-27).
Further, wherein ceramic powder grain size is 100-500nm.
Further, ceramic powder is low using titanium dioxide ceramic powder, lithium molybdate bismuth low-temp ceramics powder or potassium molybdate
Warm ceramic powder.
A kind of preparation method of rapid shaping microwave-medium ceramics, includes the following steps：
Step 1) takes raw material based on quality parts ratio：Ceramic powder：Deionized water=(18-22)：(23-27)；
Step 2), the 0.5-1% for taking biomolecule crosslinking agent, plasticiser and lubricant to be respectively deionized water quality,
Biomolecule crosslinking agent and plasticiser are added in portions of de-ionized water 0.06-0.16% and 0.1-0.4% simultaneously, and stirring is equal
It pH adjusting agent is added after even adjusts pH value and obtain mixture A to 8-10；
Mixture A is cooled to 60 DEG C -65 DEG C by step 3), and lubricant is added and is uniformly mixing to obtain mixture B；
Step 4), by ceramic powder with remaining deionized water after mixing, be added in mixture B, be uniformly mixed and obtain
Mixture C；
Mixture C is stirred continuously until thick by step 5), is subsequently poured into mold dry；
Green body after drying arrange viscous sintering and can be obtained microwave-medium ceramics by step 6).
Further, biomolecule crosslinking agent uses agarose, carragheen, gelatin or pectin.
Further, plasticiser uses ethylene glycol；Lubricant uses ethyl alcohol.
Further, pH adjusting agent is not chemically reacted with ceramic powder.
Further, in step 2), dissolving biomolecule crosslinking agent in deionized water when under condition of water bath heating into
Row, water bath heating temperature are 75 DEG C -90 DEG C.
Further, in step 5), solution C is stirred continuously until in 84 DEG C -86 DEG C of water-bath thick, be subsequently poured into
It is dry in mold；It is thick provoke not drip after slurry with glass bar be advisable, the mold for pouring into sticky mass is positioned over perseverance
It is dried in constant temperature and humidity case；Climatic chamber temperature is 22-28 DEG C, and 35-45% humidity is dried 5-7 hours.
Further, in step 6), during row is viscous：It is slowly increased to from room temperature with 2 DEG C -4 DEG C of heating rate per minute
550 DEG C -555 DEG C and 1.8-2.2 hours are kept the temperature, is down to room temperature naturally with stove later；High temperature sintering：Heating rate be set as 3 DEG C-
4 DEG C per minute, is warming up to ceramic powder into porcelain temperature and keeps the temperature 4 hours, cools down later with stove.
Compared with prior art, the present invention has technique effect beneficial below：
A kind of rapid shaping microwave-medium ceramics of the present invention, there are hole in microwave-medium ceramics, size 10 microns with
Under, be not in scattering phenomenon inside microwave-medium ceramics much smaller than the wavelength for the electromagnetic wave propagated in the medium, due to this
The increase of product Hole directly reduces the dielectric constant of sample, and resonant frequency is higher than existing structure resonant frequency, this product
QF values also above existing product QF values, this product is pure, no other impurities element.
A kind of preparation method of rapid shaping microwave-medium ceramics, by using biomolecule material and plasticiser and go from
Sub- water is mixed to get the cross-linked scaffold as gel injection-moulding, and biomolecule material can form hydrogen bond with plasticiser in the solution, make
Green strength is improved for plasticiser, ceramic powder is individually mixed with remaining deionized water, avoids ceramic powder directly and conduct
Gluing phenomenon occurs for the cross-linked scaffold mixing of gel injection-moulding, finally mixes the two mixture, enables ceramic powder
It fully mixes with biomolecule material, plasticiser and deionization and is uniformly mixed as the cross-linked scaffold of gel injection-moulding, finally by
Row is viscous and sintering is avoided while greatly reducing the sample preparation time at a certain temperature rapidly at porcelain since organic matter row is viscous not
The defect generated completely, it is hereby achieved that the microwave-medium ceramics of function admirable, microwave-medium ceramics sample made from this method
Compared with using sample made from identical powder conventional solid-state method to possess more excellent performance, dielectric loss reduces condition
26.01%, Q-unloaded improves 35.6%, QF values and improves 76.85%, better than sample obtained by conventional method.
Further, this method greatly reduces the sample preparation time without Complicated Flows such as granulation, secondary ball milling, tablettings,
The sample preparation period can be greatly shortened, and since slurry has mobility, it is possible to very easily make according to mold
Go out the sample of labyrinth.
Further, this method uses ethylene glycol as plasticiser, forms hydrogen bond in the solution, improves sample green compact
Intensity；Using ethyl alcohol as lubricant, sample is greatly reduced from the loss during mold abjection.
Further, nontoxic biological molecular material such as agarose, carragheen, gelatin, fruit are used in this method preparation process
Glue forms matrix skeleton, environment-friendly and green as crosslinking agent.
Description of the drawings
Fig. 1 is finished product titanium dioxide pictorial diagram prepared by 1 rapid shaping microwave-medium ceramics method of embodiment；
Fig. 2 is finished product titanium dioxide SEM electron microscopes prepared by 1 rapid shaping microwave-medium ceramics method of embodiment；
Fig. 3 is finished product titanium dioxide EDS element spectrograms prepared by 1 rapid shaping microwave-medium ceramics method of embodiment；
Fig. 4 is lithium molybdate bismuth sample XRD diagram prepared by 2 rapid shaping microwave-medium ceramics method of embodiment；
Fig. 5 is finished product lithium molybdate bismuth pictorial diagram prepared by 2 rapid shaping microwave-medium ceramics method of embodiment；
Fig. 6 is potassium molybdate sample XRD diagram prepared by 3 rapid shaping microwave-medium ceramics method of embodiment.
Specific implementation mode
The present invention is described in further detail below in conjunction with the accompanying drawings：
A kind of rapid shaping microwave-medium ceramics, are prepared by the raw material based on following quality parts ratio：Ceramic powder：
Deionized water=(18-22)：(23-27)；Wherein ceramic powder grain size is 100-500nm；
The ceramic powder needed for sample preparation is obtained by the method for carrying out pre-burning ball milling to ceramic commodity powder；Ceramic powder is put
Enter in alumina crucible, lid lid after be put into high temperature furnace with 3 DEG C of heating rates per minute from room temperature rise to 1200 DEG C and
Two hours are kept the temperature at 1200 DEG C, is down to room temperature naturally with stove later；Ball milling condition is：By powder：Absolute alcohol：Zirconium ball is according to 1：
1：It is added in ball grinder after 2 mass ratio mixing, ball milling 4 hours, obtain ceramic powder under the rotating speed of 150r/min；
A kind of preparation method of rapid shaping microwave-medium ceramics, includes the following steps：
Step 1) takes raw material based on quality parts ratio：Ceramic powder：Deionized water=(18-22)：(23-27)；
Step 2), the 0.5-1% for taking biomolecule crosslinking agent, plasticiser and lubricant to be respectively deionized water quality,
Biomolecule crosslinking agent and plasticiser are added in portions of de-ionized water 0.06-0.16% and 0.1-0.4% simultaneously, 75 DEG C-
It it is stirring evenly and then adding into pH adjusting agent at 90 DEG C adjusts pH value and obtain mixture A to 8-10；
Mixture A is cooled to 60 DEG C -65 DEG C by step 3), and lubricant is added and is uniformly mixing to obtain mixture B；
Step 4), by ceramic powder with remaining deionized water after mixing, be added in mixture B, be uniformly mixed and obtain
Mixture C；
Mixture C is stirred continuously until thick by step 5), is subsequently poured into mold dry；
Green body after drying arrange viscous sintering and can be obtained microwave-medium ceramics by step 6).
Biomolecule crosslinking agent uses agarose, carragheen, gelatin or pectin；
Plasticiser uses ethylene glycol；
Lubricant uses ethyl alcohol；
PH adjusting agent uses ammonium hydroxide, lithium hydroxide or potassium hydroxide；PH adjusting agent is not chemically reacted with ceramic powder；
Ceramic powder uses titanium dioxide ceramic powder, lithium molybdate bismuth low-temp ceramics powder or potassium molybdate low-temp ceramics powder；
In step 1), the ceramic powder needed for sample preparation is obtained by the method for carrying out pre-burning ball milling to ceramic commodity powder；It will
Ceramic powder is put into alumina crucible, is put into high temperature furnace with 2 DEG C -4 DEG C heating rates per minute from room temperature liter after lid lid
Two hours are kept the temperature to 1100 DEG C -1300 DEG C and at 1100 DEG C -1300 DEG C, later with stove Temperature fall；Ball milling condition is：By powder
Body：Absolute alcohol：Zirconium ball is according to 1：1：It is added in ball grinder after 2 mass ratio mixing, in turning for 140r/min-160r/min
Speed lower ball milling 3-5 hours, obtains ceramic powder.
In step 2), carried out under condition of water bath heating when dissolving biomolecule crosslinking agent is in deionized water, water-bath adds
Hot temperature is 75 DEG C -90 DEG C；Using asepsis environment-protecting biomolecule crosslinking agent as the cross-linked scaffold of gel injection-moulding, with ceramic powder
Body is as filler.
In step 5), solution C is stirred continuously until in 84 DEG C -86 DEG C of water-bath thick, is subsequently poured into mold and does
It is dry；It is thick provoke not drip after slurry with glass bar be advisable, the mold for pouring into sticky mass is positioned over climatic chamber
In be dried；Climatic chamber temperature is 22-28 DEG C, and 35-45% humidity is dried 5-7 hours；
In step 6), during row is viscous：It is slowly increased to 550 DEG C -555 from room temperature with 2 DEG C -4 DEG C of heating rate per minute
DEG C and keep the temperature 1.8-2.2 hours, be down to room temperature naturally with stove later；High temperature sintering：Heating rate is set as 3 DEG C -4 DEG C every point
Clock is warming up to ceramic powder into porcelain temperature and keeps the temperature 4 hours, cools down later with stove.
Embodiment 1：
(1) it takes 25g deionization moisture 14g and 11g two bottled, 0.16g agaroses and 0.025g ethylene glycol is then taken to be added
It is placed on magnetic stirring apparatus and heats in 14g deionized waters, temperature is set as 75 DEG C, takes 0.025g ethylene glycol reagents to add with dropper
Enter in small beaker, load weighted agarose powder is then added, avoids being sticked on wall of cup；Ethylene glycol in the solution can be with agarose
Hydrogen bond is formed, green strength is improved as plasticiser, ammonium hydroxide is eventually adding and adjusts mixed liquor to pH=9, and be placed on magnetic agitation
On device, set temperature is 85 DEG C, and rotating speed 200r/min makes agarose be completely dissolved, and obtains mixture A；
(2) when little particle therein obviously disappears, illustrate that agarose has been completely dissolved at this time, mixture A coolings are worked as
Temperature is added 0.05g ethyl alcohol after reaching 65 DEG C and continues to be stirred until homogeneous to obtain mixture B, and ethyl alcohol can be in sample as lubricant
It plays a protective role when demoulding；
(3) the 20g titanium dioxide ceramic powders after pre-burning ball milling will be weighed to be added in residue 11g deionized waters, was added
Journey should slow down as far as possible, avoid titanium dioxide from occurring to reunite and splash, be added in mixture B after mixing, mixing is equal again
It is even to obtain mixture C；
(4) etc. after ceramic powders have been thoroughly dispersed among slurry, mixture C is persistently stirred at 85 DEG C, makes water
Divide rapid evaporation, it is rapid to improve slurry viscosity；
(5) when magnetite can not continue stirring when be drawn off, use stirring rod hand operated mixing instead, when the slurry in stirring rod compared with
For it is sticky slowly fall when illustrate slurry tanning finish, be poured into mold, be put in after another piece of glass slide is covered above
It is flattened under weight, time 15min later slowly removes both sides glass slide, and the sample handled well is connected to mold
It is put in climatic chamber and is dried, temperature is set as 25 DEG C, and humidity 40% is dried 6 hours；Lower temperature and centainly wet
Degree avoids the problem that dry too fast generation cracking and water transport channel closed interior moisture can not be discharged.
(6) sample taken off is put on potsherd to be then fed into low temperature oven and arrange and is glued, room temperature rises with 2 DEG C per minute
Heating rate rise to 550 DEG C and keep the temperature 2 hours, cool down later with stove, ensure being completely exhausted out for organic matter；It puts it into later
Sintering process is completed in high temperature furnace, heating rate is set as 3 DEG C per minute, is warming up to 1450 DEG C and keeps the temperature 4 hours, later with stove
Cooling, you can obtain microwave-medium ceramics.
The sample drawing of titanium dioxide ceramic green body is prepared using the present embodiment as shown in Figure 1, left side is using by pre-
Sample drawing made from ball milling powder body is burnt, right side is then untreated powder.Use sample made from powder after treatment
Product surface more flat smooth is lost caused by avoiding unnecessary scattered reflection；Schemed using the sample SEM that this method is produced
Spectrum is as shown in Figure 2, the results showed that there are hole in sample, size is at 10 microns hereinafter, much smaller than the electromagnetism propagated in the medium
The wavelength of wave, so being not in apparent scattering phenomenon in inside, conversely, because the increase of sample Hole directly reduces
The dielectric constant of sample, and the half power of the resonant frequency of sample and dielectric constant is inversely proportional, so the resonance of sample
Frequency can improve, and then improve the QF values of sample, and the EDS elements collection of illustrative plates of sample is as shown in figure 3, the result shows that sample
Middle organic matter completely removes, can be with by the method in addition to adjusting pH and a small amount of nitrogen for introducing, then without other impurities element
Obtain very pure titanium dioxide microwave dielectric ceramic sample.The sample microwave dielectric property that embodiment obtains is as shown in table 1：
Sample microwave dielectric property table in 1 embodiment 1 of table
Embodiment 2：
(1) it takes 25g deionization moisture 14g and 11g two bottled, then takes 0.16g gelatin and 0.025g ethylene glycol that 14g is added
It is placed on magnetic stirring apparatus and heats in deionized water, temperature is set as 80 DEG C, takes 0.025g ethylene glycol reagents to be added with dropper
In small beaker, load weighted gelatin powder is then added, avoids being sticked on wall of cup；Ethylene glycol can form hydrogen with gelatin in the solution
Key improves green strength as plasticiser, is eventually adding lithium hydroxide and adjusts mixed liquor to pH=9, and is placed on magnetic stirring apparatus
On, set temperature is 85 DEG C, and rotating speed 200r/min makes gelatin be completely dissolved, and obtains mixture A；
(2) when little particle therein obviously disappears, illustrate that gelatin has been completely dissolved at this time, by mixture A coolings when temperature
0.05g lithium hydroxides, which are added, after reaching 65 DEG C in degree continues to be stirred until homogeneous to obtain mixture B, and ethyl alcohol can be in sample as lubricant
It plays a protective role when pint mould；
(3) the 20g lithium molybdate bismuth low-temp ceramics powders after pre-burning ball milling will be weighed to be added in residue 11g deionized waters, is added
Entering process should slow down as far as possible, be added in mixture B after mixing, be uniformly mixed obtain mixture C again；
(4) etc. after ceramic powders have been thoroughly dispersed among slurry, mixture C is persistently stirred at 85 DEG C, makes water
Divide rapid evaporation, it is rapid to improve slurry viscosity；
(5) when magnetite can not continue stirring when be drawn off, use stirring rod hand operated mixing instead, when the slurry in stirring rod compared with
For it is sticky slowly fall when illustrate slurry tanning finish, be poured into mold, be put in after another piece of glass slide is covered above
It is flattened under weight, time 15min later slowly removes both sides glass slide, and the sample handled well is connected to mold
It is put in climatic chamber and is dried, temperature is set as 25 DEG C, and humidity 40% is dried 6 hours；Lower temperature and centainly wet
Degree avoids the problem that dry too fast generation cracking and water transport channel closed interior moisture can not be discharged.
(6) sample taken off is put on potsherd to be then fed into high temperature Muffle furnace and arrange and is glued, room temperature rises with every point
The heating rate that 2 DEG C of clock rises to 450 DEG C and keeps the temperature 4 hours, cools down later with stove, ensures being completely exhausted out for organic matter；Later will
It, which is put into high temperature furnace, completes sintering process, and heating rate is set as 3 DEG C per minute, is warming up to 560 DEG C and keeps the temperature 4 hours, it
Cool down afterwards with stove, you can obtain microwave-medium ceramics.
The XRD diagram for the sample that embodiment 2 obtains is as shown in figure 4, as can be seen from the figure test gained powder collection of illustrative plates and text
The reference chart for offering middle offer is essentially identical, and number, position, the intensity at peak match.Illustrate that obtained sample is exactly lithium molybdate bismuth.
Simultaneously without apparent miscellaneous peak in collection of illustrative plates, show that obtained sample purity is higher；Sample is schemed as shown in figure 5, flat smooth in fact.
Embodiment 3：
(1) it takes 25g deionization moisture 14g and 11g two bottled, 0.16g carragheens and 0.025g ethylene glycol is then taken to be added
It is placed on magnetic stirring apparatus and heats in 14g deionized waters, temperature is set as 85 DEG C, takes 0.025g ethylene glycol reagents to add with dropper
Enter in small beaker, load weighted carragheen powder is then added, avoids being sticked on wall of cup；Ethylene glycol in the solution can be with carragheen
Hydrogen bond is formed, green strength is improved as plasticiser, potassium hydroxide is eventually adding and adjusts mixed liquor to pH=10, and be placed on magnetic force
On blender, set temperature is 85 DEG C, and rotating speed 200r/min makes agarose be completely dissolved, and obtains mixture A；
(2) when little particle therein obviously disappears, illustrate that carragheen has been completely dissolved at this time, mixture A coolings are worked as
Temperature is added 0.05g potassium hydroxide and continues to be stirred until homogeneous to obtain mixture B after reaching 65 DEG C, ethyl alcohol can be as lubricant
Sample plays a protective role when demoulding；
(3) the 20g potassium molybdate low-temp ceramics powders after pre-burning ball milling will be weighed to be added in residue 11g deionized waters, addition
Process should slow down as far as possible, avoid potassium molybdate low-temp ceramics powder from occurring to reunite and splash, mixture B is added after mixing
In, it is uniformly mixed obtains mixture C again；
(4) etc. after ceramic powders have been thoroughly dispersed among slurry, mixture C is persistently stirred at 85 DEG C, makes water
Divide rapid evaporation, it is rapid to improve slurry viscosity；
(5) when magnetite can not continue stirring when be drawn off, use stirring rod hand operated mixing instead, when the slurry in stirring rod compared with
For it is sticky slowly fall when illustrate slurry tanning finish, be poured into mold, be put in after another piece of glass slide is covered above
It is flattened under weight, time 15min later slowly removes both sides glass slide, and the sample handled well is connected to mold
It is put in climatic chamber and is dried, temperature is set as 25 DEG C, and humidity 40% is dried 6 hours；Lower temperature and centainly wet
Degree avoids the problem that dry too fast generation cracking and water transport channel closed interior moisture can not be discharged.
(6) sample taken off is put on potsherd to be then fed into high temperature Muffle furnace and arrange and is glued, room temperature rises with every point
The heating rate that 2 DEG C of clock rises to 400 DEG C and keeps the temperature 4 hours, cools down later with stove, ensures being completely exhausted out for organic matter；Later will
It, which is put into high temperature furnace, completes sintering process, and heating rate is set as 3 DEG C per minute, is warming up to 460 DEG C and keeps the temperature 4 hours, it
Cool down afterwards with stove, you can obtain microwave-medium ceramics.
The XRD diagram for the sample that embodiment 3 obtains is as shown in fig. 6, as can be seen from the figure test gained powder collection of illustrative plates and text
The reference chart for offering middle offer is essentially identical, and number, position, the intensity at peak match substantially.Illustrate that obtained sample is exactly potassium molybdate.
Simultaneously without apparent miscellaneous peak in collection of illustrative plates, show that obtained sample purity is higher.
Embodiment 4：
(1) it takes 23g deionization moisture 12g and 11g two bottled, 0.115g pectin and 0.0138g ethylene glycol is then taken to be added
It is placed on magnetic stirring apparatus and heats in 12g deionized waters, temperature is set as 90 DEG C, and 0.0138g ethylene glycol reagents are taken with dropper
It is added in small beaker, load weighted pectin powder is then added, avoids being sticked on wall of cup；Ethylene glycol in the solution can be with pectin shape
At hydrogen bond, green strength is improved as plasticiser, ammonium hydroxide is eventually adding and adjusts mixed liquor to pH=8, and be placed on magnetic stirring apparatus
On, set temperature is 85 DEG C, and rotating speed 200r/min makes pectin be completely dissolved, and obtains mixture A；
(2) when little particle therein obviously disappears, illustrate that pectin has been completely dissolved at this time, by mixture A coolings when temperature
0.023g ethyl alcohol, which is added, after reaching 60 DEG C in degree continues to be stirred until homogeneous to obtain mixture B, and ethyl alcohol can be in sample as lubricant
It plays a protective role when demoulding；
(3) the 18g titanium dioxide ceramic powders after pre-burning ball milling will be weighed to be added in residue 11g deionized waters, was added
Journey should slow down as far as possible, avoid titanium dioxide from occurring to reunite and splash, be added in mixture B after mixing, mixing is equal again
It is even to obtain mixture C；
(4) etc. after ceramic powders have been thoroughly dispersed among slurry, mixture C is persistently stirred at 84 DEG C, makes water
Divide rapid evaporation, it is rapid to improve slurry viscosity；
(5) when magnetite can not continue stirring when be drawn off, use stirring rod hand operated mixing instead, when the slurry in stirring rod compared with
For it is sticky slowly fall when illustrate slurry tanning finish, be poured into mold, be put in after another piece of glass slide is covered above
It is flattened under weight, time 15min later slowly removes both sides glass slide, and the sample handled well is connected to mold
It is put in climatic chamber and is dried, temperature is set as 22 DEG C, and humidity 35% is dried 5 hours；Lower temperature and centainly wet
Degree avoids the problem that dry too fast generation cracking and water transport channel closed interior moisture can not be discharged.
(6) sample taken off is put on potsherd to be then fed into low temperature oven and arrange and is glued, room temperature rises with 3 DEG C per minute
Heating rate rise to 555 DEG C and keep the temperature 1.8 hours, cool down later with stove, ensure being completely exhausted out for organic matter；It is put later
Enter and complete sintering process in high temperature furnace, heating rate is set as 4 DEG C per minute, is warming up to 1450 DEG C and keeps the temperature 4 hours, Zhi Housui
Stove cools down, you can obtains microwave-medium ceramics.
Embodiment 5：
(1) it takes 24g deionization moisture 13g and 11g two bottled, 0.114g carragheens and 0.0192g ethylene glycol is then taken to add
Enter to be placed in 13g deionized waters on magnetic stirring apparatus and heat, temperature is set as 84 DEG C, takes 0.0192g ethylene glycol to try with dropper
Agent is added in small beaker, and load weighted OK a karaoke club buffings is then added, avoids being sticked on wall of cup；Ethylene glycol in the solution can be with OK a karaoke club
Glue forms hydrogen bond, and green strength is improved as plasticiser, is eventually adding lithium hydroxide and adjusts mixed liquor to pH=10, and is placed on magnetic
On power blender, set temperature is 90 DEG C, and rotating speed 200r/min makes carragheen be completely dissolved, and obtains mixture A；
(2) when little particle therein obviously disappears, illustrate that carragheen has been completely dissolved at this time, mixture A coolings are worked as
Temperature is added 0.048g ethyl alcohol after reaching 62 DEG C and continues to be stirred until homogeneous to obtain mixture B, and ethyl alcohol can be in sample as lubricant
It plays a protective role when pint mould；
(3) the 22g lithium molybdate bismuth low-temp ceramics powders after pre-burning ball milling will be weighed to be added in residue 11g deionized waters, is added
Entering process should slow down as far as possible, be added in mixture B after mixing, be uniformly mixed obtain mixture C again；
(4) etc. after ceramic powders have been thoroughly dispersed among slurry, mixture C is persistently stirred at 86 DEG C, makes water
Divide rapid evaporation, it is rapid to improve slurry viscosity；
(5) when magnetite can not continue stirring when be drawn off, use stirring rod hand operated mixing instead, when the slurry in stirring rod compared with
For it is sticky slowly fall when illustrate slurry tanning finish, be poured into mold, be put in after another piece of glass slide is covered above
It is flattened under weight, time 15min later slowly removes both sides glass slide, and the sample handled well is connected to mold
It is put in climatic chamber and is dried, temperature is set as 28 DEG C, and humidity 45% is dried 7 hours；Lower temperature and centainly wet
Degree avoids the problem that dry too fast generation cracking and water transport channel closed interior moisture can not be discharged.
(6) sample taken off is put on potsherd to be then fed into low temperature oven and arrange and is glued, room temperature rises with 2 DEG C per minute
Heating rate rise to 552 DEG C and keep the temperature 2 hours, cool down later with stove, ensure being completely exhausted out for organic matter；It puts it into later
Sintering process is completed in high temperature furnace, heating rate is set as 3 DEG C per minute, is warming up to 1460 DEG C and keeps the temperature 4 hours, later with stove
Cooling, you can obtain microwave-medium ceramics.
Embodiment 6：
(1) it takes 26g deionization moisture 15g and 11g two bottled, 0.182g agaroses and 0.0312g ethylene glycol is then taken to add
Enter to be placed in 15g deionized waters on magnetic stirring apparatus and heat, temperature is set as 73 DEG C, takes 0.0312g ethylene glycol to try with dropper
Agent is added in small beaker, and load weighted agarose powder is then added, avoids being sticked on wall of cup；Ethylene glycol in the solution can be with fine jade
Lipolysaccharide forms hydrogen bond, and green strength is improved as plasticiser, is eventually adding potassium hydroxide and adjusts mixed liquor to pH=9, and is placed on
On magnetic stirring apparatus, set temperature is 85 DEG C, and rotating speed 200r/min makes agarose be completely dissolved, and obtains mixture A；
(2) when little particle therein obviously disappears, illustrate that agarose has been completely dissolved at this time, mixture A coolings are worked as
Temperature is added 0.078g ethyl alcohol after reaching 65 DEG C and continues to be stirred until homogeneous to obtain mixture B, and ethyl alcohol can be in sample as lubricant
It plays a protective role when pint mould；
(3) the 19g potassium molybdate low-temp ceramics powders after pre-burning ball milling will be weighed to be added in residue 11g deionized waters, addition
Process should slow down as far as possible, be added in mixture B after mixing, be uniformly mixed obtain mixture C again；
(4) etc. after ceramic powders have been thoroughly dispersed among slurry, mixture C is persistently stirred at 85 DEG C, makes water
Divide rapid evaporation, it is rapid to improve slurry viscosity；
(5) when magnetite can not continue stirring when be drawn off, use stirring rod hand operated mixing instead, when the slurry in stirring rod compared with
For it is sticky slowly fall when illustrate slurry tanning finish, be poured into mold, be put in after another piece of glass slide is covered above
It is flattened under weight, time 15min later slowly removes both sides glass slide, and the sample handled well is connected to mold
It is put in climatic chamber and is dried, temperature is set as 25 DEG C, and humidity 40% is dried 6 hours；Lower temperature and centainly wet
Degree avoids the problem that dry too fast generation cracking and water transport channel closed interior moisture can not be discharged.
(6) sample taken off is put on potsherd to be then fed into low temperature oven and arrange and is glued, room temperature rises with 2 DEG C per minute
Heating rate rise to 550 DEG C and keep the temperature 2 hours, cool down later with stove, ensure being completely exhausted out for organic matter；It puts it into later
Sintering process is completed in high temperature furnace, heating rate is set as 3 DEG C per minute, is warming up to 1450 DEG C and keeps the temperature 4 hours, later with stove
Cooling, you can obtain microwave-medium ceramics.
Embodiment 7：
(1) it takes 27g deionization moisture 14g and 13g two bottled, 0.27g gelatin and 0.0432g ethylene glycol is then taken to be added
It is placed on magnetic stirring apparatus and heats in 14g deionized waters, temperature is set as 86 DEG C, and 0.0432g ethylene glycol reagents are taken with dropper
It is added in small beaker, load weighted gelatin powder is then added, avoids being sticked on wall of cup；Ethylene glycol in the solution can be with gelatin shape
At hydrogen bond, green strength is improved as plasticiser, ammonium hydroxide is eventually adding and adjusts mixed liquor to pH=8, and be placed on magnetic stirring apparatus
On, set temperature is 85 DEG C, and rotating speed 200r/min makes gelatin be completely dissolved, and obtains mixture A；
(2) when little particle therein obviously disappears, illustrate that gelatin has been completely dissolved at this time, by mixture A coolings when temperature
0.098g ethyl alcohol, which is added, after reaching 65 DEG C in degree continues to be stirred until homogeneous to obtain mixture B, and ethyl alcohol can be in sample as lubricant
It plays a protective role when demoulding；
(3) the 21g titanium dioxide ceramic powders after pre-burning ball milling will be weighed to be added in residue 13g deionized waters, was added
Journey should slow down as far as possible, be added in mixture B after mixing, be uniformly mixed obtain mixture C again；
(4) etc. after ceramic powders have been thoroughly dispersed among slurry, mixture C is persistently stirred at 85 DEG C, makes water
Divide rapid evaporation, it is rapid to improve slurry viscosity；
(5) when magnetite can not continue stirring when be drawn off, use stirring rod hand operated mixing instead, when the slurry in stirring rod compared with
For it is sticky slowly fall when illustrate slurry tanning finish, be poured into mold, be put in after another piece of glass slide is covered above
It is flattened under weight, time 15min later slowly removes both sides glass slide, and the sample handled well is connected to mold
It is put in climatic chamber and is dried, temperature is set as 25 DEG C, and humidity 40% is dried 6 hours；Lower temperature and centainly wet
Degree avoids the problem that dry too fast generation cracking and water transport channel closed interior moisture can not be discharged.
(6) sample taken off is put on potsherd to be then fed into low temperature oven and arrange and is glued, room temperature rises with 2 DEG C per minute
Heating rate rise to 550 DEG C and keep the temperature 2 hours, cool down later with stove, ensure being completely exhausted out for organic matter；It puts it into later
Sintering process is completed in high temperature furnace, heating rate is set as 3 DEG C per minute, is warming up to 1450 DEG C and keeps the temperature 4 hours, later with stove
Cooling, you can obtain microwave-medium ceramics.
Claims (10)
1. a kind of rapid shaping microwave-medium ceramics, which is characterized in that be prepared by the raw material based on following quality parts ratio：
Ceramic powder：Deionized water=(18-22)：(23-27).
2. a kind of rapid shaping microwave-medium ceramics according to claim 1, which is characterized in that wherein ceramic powder grain size is
100-500nm。
3. a kind of rapid shaping microwave-medium ceramics according to claim 1, which is characterized in that ceramic powder uses titanium dioxide
Titanium ceramic powder, lithium molybdate bismuth low-temp ceramics powder or potassium molybdate low-temp ceramics powder.
4. a kind of preparation method of rapid shaping microwave-medium ceramics, which is characterized in that include the following steps：
Step 1) takes raw material based on quality parts ratio：Ceramic powder：Deionized water=(18-22)：(23-27)；
Step 2) takes biomolecule crosslinking agent, plasticiser and lubricant to be respectively 0.5-1%, 0.06- of deionized water quality
Biomolecule crosslinking agent and plasticiser are added in portions of de-ionized water 0.16% and 0.1-0.4% simultaneously, uniformly rear that pH is added
Conditioning agent adjusts pH value and obtains mixture A to 8-10；
Mixture A is cooled to 60 DEG C -65 DEG C by step 3), and lubricant is added and is uniformly mixing to obtain mixture B；
Step 4), by ceramic powder with remaining deionized water after mixing, be added in mixture B, mixed
Object C；
Mixture C is stirred continuously until thick by step 5), is subsequently poured into mold dry；
Green body after drying arrange viscous sintering and can be obtained microwave-medium ceramics by step 6).
5. a kind of preparation method of rapid shaping microwave-medium ceramics according to claim 4, which is characterized in that biology point
Sub- crosslinking agent uses agarose, carragheen, gelatin or pectin.
6. a kind of preparation method of rapid shaping microwave-medium ceramics according to claim 4, which is characterized in that plasticiser
Using ethylene glycol；Lubricant uses ethyl alcohol.
7. a kind of preparation method of rapid shaping microwave-medium ceramics according to claim 4, which is characterized in that pH is adjusted
Agent is not chemically reacted with ceramic powder.
8. a kind of preparation method of rapid shaping microwave-medium ceramics according to claim 4, which is characterized in that step 2)
In, it is carried out under condition of water bath heating when dissolving biomolecule crosslinking agent is in deionized water, water bath heating temperature is 75 DEG C -90
℃。
9. a kind of preparation method of rapid shaping microwave-medium ceramics according to claim 4, which is characterized in that step 5)
In, solution C is stirred continuously until in 84 DEG C -86 DEG C of water-bath thick, is subsequently poured into mold dry；It is thick with glass
Stick, which provokes not drip after slurry, to be advisable, and the mold for pouring into sticky mass is positioned in climatic chamber and is dried；Constant temperature
Constant humidity cabinet temperature is 22-28 DEG C, and 35-45% humidity is dried 5-7 hours.
10. a kind of preparation method of rapid shaping microwave-medium ceramics according to claim 4, which is characterized in that step
6) in, during row is viscous：550 DEG C -555 DEG C are slowly increased to 2 DEG C -4 DEG C of heating rate per minute and keep the temperature 1.8- from room temperature
2.2 hours, it is down to room temperature naturally with stove later；High temperature sintering：Heating rate be set as 3 DEG C -4 DEG C it is per minute, be warming up to ceramics
Powder is at porcelain temperature and keeps the temperature 4 hours, cools down later with stove.
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| CN111187062A (en) * | 2020-01-13 | 2020-05-22 | 杭州电子科技大学 | CaSnSiO5-K2MoO4Base composite ceramic microwave material and preparation method thereof |
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