CN108083839A - A kind of preparation method of high intensity, porous piezoelectric ceramics - Google Patents
A kind of preparation method of high intensity, porous piezoelectric ceramics Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of high intensity, porous piezoelectric ceramics, belong to field of ceramic preparation technology.The present invention is with strontium carbonate,Barium carbonate and titanium dioxide mixing are as matrix,The substances such as the tert-butyl alcohol are mixed with plant extraction liquid is prepared high intensity as reinforcing agent,The piezoelectric ceramics of high porosity and high tension performance,Since the tert-butyl alcohol has high saturated vapor pressure and low surface tension,The highly volatile during body drying,Compactness between adjacent particle is not interfered with,So that the intensity of green body is improved,In addition monomer is introduced in the tert-butyl alcohol,In green body macromolecule is obtained using monomer polymerization reactions,And construct three-dimensional net structure,To support ceramic body,Maintain high porosity,In sintering process,Uniform pore structure is formd using home position polymerization reaction,The breakdown being avoided that in polarization process,Be conducive to the transmission of stress and energy,So as to improve the piezoelectric property of piezoelectric ceramics,It is with a wide range of applications.
Description
Technical field
The invention discloses a kind of preparation methods of high intensity, porous piezoelectric ceramics, belong to field of ceramic preparation technology.
Background technology
Piezoelectric ceramics is a kind of ceramic material that can convert mechanical energy and electric energy mutually, belongs to inorganic non-metallic
Material.Piezoelectric ceramics has sensitive characteristic, can extremely faint mechanical oscillation be converted into electric signal, available for sonar system
System, meteorological detection, telemetering environmental protection, household electrical appliance etc..Piezoelectric ceramics allows it to sense more than ten meters the sensitivity of external force
Outer winged insect pats disturbance of the wing to air, makes piezoelectricity seismic detector with it, can accurately measure earthquake intensity, indicate ground
The azimuth-range of shake, this can't but be a big outstanding service of piezoelectric ceramics.Common piezoelectric ceramics has barium titanate series, zirconium metatitanic acid
Lead binary system and the third compound is added in binary system, the deformation quantity very little that piezoelectric ceramics generates under electric field action, most
It is no more than thousand a ten thousandths of size itself more, does not look down upon this small variation, the accurate control machine manufactured based on this principle
Structure piezoelectric actuator is all a big Gospel for fields such as control, microelectric technique, the bioengineering of precision instrument and machinery.
The frequency control apparatus such as resonator, wave filter are the Primary Components for determining communication equipment performance, and piezoelectric ceramics is at this
Aspect has apparent superiority.Its frequency stability is good, and precision is high and applicable wide frequency range, and small, nonhygroscopic,
Long lifespan can improve anti-interference particularly in multiple communicating apparatus, make previous electromagnetic equipment can not unmatch and face
Face the destiny substituted.
Acoustic transducer acoustic transducer is one of most common application.As sound pick-up, microphone, earphone, buzzer, super
Sound wave depth sounding instrument, sonar, the supersonic detector etc. of material can do acoustic transducer with piezoelectric ceramics.On toy for children
Buzzer to be exactly electric current generate vibration by the inverse piezoelectric effect of piezoelectric ceramics, and send the sound that human ear can be audible.
Piezoelectric ceramics can generate the vibration of different frequency, so as to send a variety of sound by the control of electronic circuit.Such as electricity
AC audio electric signal is exactly converted to voice signal by sub- music greeting card by inverse piezoelectric effect.Piezoelectricity trigger is since
Tank has been invented by the British army in world war, and after being used for the first time in the fight in French rope nurse river and having inflicted heavy losses on German army, it is smooth
It gram exhibits one's skill to the full in multiple fight.However to the 1960s and 1970s, due to the invention of antitank weapon, tank loses
Splendidness in the past.The armor-piercing bullet contact tank that antitank gun is launched, will explode, tank, which is fried, to be crushed at once.This is
Because equipped with piezoelectric ceramics on bullet, it can be changed into powerful mechanical force when colliding instant high-voltage, break out spark and draw
Bursting charge.A kind of modern electronic lighter on piezoelectric lighter gas stove, is exactly using made of piezoelectric ceramics.
Common piezoelectric ceramics intensity is relatively low, porosity is relatively low and piezoelectric property is poor at present, can not meet wanting for market
It asks, therefore, invent the porous piezoceramics that a kind of intensity is high and the porosity is high has positive effect to field of ceramic preparation technology.
The content of the invention
The technical problems to be solved by the invention：For current common piezoelectric ceramics, there are intensity is relatively low, porosity is relatively low
And piezoelectric property is poor, the defects of can not meet the requirement in market, provides a kind of preparation of high intensity, porous piezoelectric ceramics
Method.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of high intensity, porous piezoelectric ceramics, it is characterised in that specifically preparation process is：
（1）By acrylamide, N, N- methylene-bisacrylamides and the tert-butyl alcohol are mixed, and obtain mixture, by mixture and
Deionized water mixing is placed in beaker, is continued to stir, is obtained Self-made mixture；
（2）Weigh 10~12g citruses and the mixing of 16~20g spinach be placed in pulper and blend, obtain blending object, will blend object and
Distilled water mixing is put into beaker, and beaker is placed in ultrasonic extraction in ultrasonic oscillation device, is filtered after extraction, collects filtrate,
Filtrate is evaporated under reduced pressure, obtains self-control plant extraction liquid, finally mixes self-control plant extraction liquid with the self-control of above-mentioned gained
Liquid mixing is ultrasonically treated, stratification, and separation removal lower water phase obtains premix；
（3）Strontium carbonate, barium carbonate and titanium dioxide are mixed to be put into kiln and calcined, grind again after calcination and crosses 100 mesh
Sieve collects sieving calcined powder, and sieving calcined powder, dextrin and amber powder are mixed, obtain modified porous powder；
（4）Modified porous powder, premix and silane resin acceptor kh-550 are mixed and reacted, obtains self-control stirring slurry
Self-control stirring slurry is poured into four-hole boiling flask and continues to stir, and vacuumized by material, is removed the bubble in slurry, then is burnt to four mouthfuls
The sodium peroxydisulfate polymerisation of the hydrogen peroxide of addition self-control stirring stock quality 10% and self-control stirring stock quality 3% in bottle,
Obtain self-control polymeric size；
（5）Self-control polymeric size is injected into mold, and is positioned in drier, under nitrogen protection air drying, it is dry
After be put into baking oven and dry, obtain self-control green body, and be removed from the molds self-control green body, self-control green body be put into crucible furnace and is burnt
Knot, cooled to room temperature, dry discharging, you can high intensity, porous piezoelectric ceramics is made.
Step（1）The mass ratio of the acrylamide, N, N- methylene-bisacrylamides and the tert-butyl alcohol is 2：1：3, it stirs
The time is mixed as 10~12min, the mass ratio of mixture and deionized water is 1：3, continuation mixing time is 11~15min.
Step（2）Described blends the time as 16~20min, and the mass ratio for blending object and distilled water is 1：5, ultrasonic extraction
Temperature is 60~80 DEG C, and ultrasonic extraction power is 180~200W, and the ultrasonic extraction time is 45~60min, makes plant extraction liquid by oneself
Volume ratio with Self-made mixture is 1：1, sonification power is 200~260W, and sonication treatment time is 10~12min.
Step（3）The mass ratio of the strontium carbonate, barium carbonate and titanium dioxide is 1：1：2, calcining heat for 800~
1000 DEG C, calcination time is 1~2h, and milling time is 10~12min, and the mass ratio of sieving calcined powder, dextrin and amber is
3：2：1, mixing time is 16~20min.
Step（4）The mass ratio of the modified porous powder, premix and silane resin acceptor kh-550 is 5：3：1,
The time is stirred to react as 2~4h, continuation mixing time is 10~12min, and the mass fraction of hydrogen peroxide is 20%, and reaction temperature is
45~55 DEG C, the reaction time is 1~2h.
Step（5）The die size be 180mm × 16mm × 2mm, drying time be 10~12min, drying temperature
For 50~60 DEG C, drying time is 1~2h, and sintering temperature is 1000~1200 DEG C, and sintering time is 1~3h.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is mixed as substances such as matrix, the tert-butyl alcohols using strontium carbonate, barium carbonate and titanium dioxide and mixed with plant extraction liquid
Cooperate to be prepared the piezoelectric ceramics of high intensity, high porosity and high tension performance for reinforcing agent, matrix calcined first,
Intrinsic silicon impurity is removed, dextrin is recycled to be modified the matrix after calcining, in sintering process, dextrin can slowly disappear
It loses, intrinsic silicon hole is promoted gradually to increase therewith, then by acrylamide, N, N- methylene-bisacrylamides and the tert-butyl alcohol
Self-made mixture is mixed to get, it is continued supersound process with plant extraction liquid is prepared premix, utilizes premix
Modified matrix is further modified with silane coupling agent, since the tert-butyl alcohol has high saturated vapor pressure and low surface tension,
The highly volatile during body drying does not interfere with compactness between adjacent particle, so that the intensity of green body is improved,
In addition monomer is introduced in the tert-butyl alcohol, macromolecule is obtained using monomer polymerization reactions in green body, and constructs three-dimensional network
Structure to support ceramic body, maintains high porosity so that piezoelectric ceramics with high porosity simultaneously with higher
Mechanical strength；
（2）The present invention forms uniform pore structure in sintering process, using home position polymerization reaction, is avoided that polarization process
In breakdown so that polarization is abundant, is conducive to piezoelectric property and is optimized, wherein interconnect similar to the crystal grain of stone arch bridge,
Construct a firm spacial framework, and under the action of electromechanical Coupling and plus load, be conducive to stress and
The transmission of energy so as to improve the piezoelectric property of piezoelectric ceramics, is with a wide range of applications.
Specific embodiment
It is 2 in mass ratio：1：3 by acrylamide, N, and N- methylene-bisacrylamides and the tert-butyl alcohol be mixed 10~
12min obtains mixture, is 1 in mass ratio by mixture and deionized water：3 mixing be placed in beaker, continue stirring 11~
15min obtains Self-made mixture；Weigh 10~12g citruses and the mixing of 16~20g spinach be placed in pulper blend 16~
20min obtains blending object, and will blend object and distilled water is 1 in mass ratio：5 mixing are put into beaker, and beaker is placed in ultrasound
In ripple oscillator, 45~60min of ultrasonic extraction under conditions of temperature is 60~80 DEG C, power is 180~200W, mistake after extraction
Filter, collect filtrate, filtrate is evaporated under reduced pressure, obtain self-control plant extraction liquid, finally will self-control plant extraction liquid with it is above-mentioned
Gained Self-made mixture is 1 by volume：1 mixing, and with 200~260W power ultrasonics handle 10~12min, stratification,
Separation removal lower water phase, obtains premix；It is 1 in mass ratio：1：2 put the mixing of strontium carbonate, barium carbonate and titanium dioxide
Enter in kiln, 1~2h calcined in the case where temperature is 800~1000 DEG C, grind 10~12min again after calcination and cross 100 mesh sieves,
Sieving calcined powder is collected, is 3 in mass ratio by sieving calcined powder, dextrin and amber powder：2：1 is mixed 16~20min,
Obtain modified porous powder；It is 5 in mass ratio by modified porous powder, premix and silane resin acceptor kh-550：3：1 mixing
2~4h is stirred to react, obtains self-control stirring slurry, self-control stirring slurry is poured into four-hole boiling flask and continues 10~12min of stirring,
And vacuumize, the bubble in slurry is removed, then the mass fraction of addition self-control stirring stock quality 10% is into four-hole boiling flask
20% hydrogen peroxide and the sodium peroxydisulfate of self-control stirring stock quality 3%, 1~2h of polymerisation in the case where temperature is 45~55 DEG C,
Obtain self-control polymeric size；Polymeric size will be made by oneself to be injected into the mold that size is 180mm × 16mm × 2mm, and be positioned over
In drier, 10~12min of air drying, is put into after dry in baking oven under nitrogen protection, is dried in the case where temperature is 50~60 DEG C
Dry 1~2h obtains self-control green body, and is removed from the molds self-control green body, and self-control green body is put into crucible furnace, is in temperature
1~3h, cooled to room temperature, dry discharging, you can high intensity, porous piezoelectric ceramics is made are sintered at 1000~1200 DEG C.
Example 1
It is 2 in mass ratio：1：10min is mixed in acrylamide, N, N- methylene-bisacrylamides and the tert-butyl alcohol by 3, is obtained
Mixture and deionized water are 1 in mass ratio by mixture：3 mixing are placed in beaker, continue to stir 11min, it is mixed to obtain self-control
Close liquid；It weighs 10g citruses and the mixing of 16g spinach is placed in pulper and blends 16min, obtain blending object, object and distillation will be blended
Water is 1 in mass ratio：5 mixing are put into beaker, and beaker are placed in ultrasonic oscillation device, temperature be 60 DEG C, power is
Ultrasonic extraction 45min under conditions of 180W is filtered after extraction, collects filtrate, filtrate is evaporated under reduced pressure, and obtains self-control plant
Extracting solution, it is 1 by volume that will finally make plant extraction liquid by oneself with above-mentioned gained Self-made mixture：1 mixing, and with 200W power
10min, stratification are ultrasonically treated, separation removal lower water phase obtains premix；It is 1 in mass ratio：1：2 by strontium carbonate,
Barium carbonate and titanium dioxide mixing are put into kiln, are calcined 1h in the case where temperature is 800 DEG C, are ground 10min again simultaneously after calcination
100 mesh sieves are crossed, collect sieving calcined powder, are 3 in mass ratio by sieving calcined powder, dextrin and amber powder：2：1 is mixed
16min obtains modified porous powder；It is 5 in mass ratio by modified porous powder, premix and silane resin acceptor kh-550：
3：1 is mixed reaction 2h, obtains self-control stirring slurry, and self-control stirring slurry is poured into four-hole boiling flask and continues to stir 10min,
And vacuumize, the bubble in slurry is removed, then the mass fraction of addition self-control stirring stock quality 10% is into four-hole boiling flask
20% hydrogen peroxide and the sodium peroxydisulfate of self-control stirring stock quality 3%, the polymerisation 1h in the case where temperature is 45 DEG C are made by oneself
Polymeric size；Polymeric size will be made by oneself to be injected into the mold that size is 180mm × 16mm × 2mm, and be positioned in drier,
Air drying 10in under nitrogen protection is put into after dry in baking oven, and 1h is dried in the case where temperature is 50 DEG C, obtains self-control green body,
And self-control green body is removed from the molds, self-control green body is put into crucible furnace, 1h, natural cooling are sintered in the case where temperature is 1000 DEG C
To room temperature, dry discharging, you can high intensity, porous piezoelectric ceramics is made.
Example 2
It is 2 in mass ratio：1：11min is mixed in acrylamide, N, N- methylene-bisacrylamides and the tert-butyl alcohol by 3, is obtained
Mixture and deionized water are 1 in mass ratio by mixture：3 mixing are placed in beaker, continue to stir 13min, it is mixed to obtain self-control
Close liquid；It weighs 11g citruses and the mixing of 18g spinach is placed in pulper and blends 18min, obtain blending object, object and distillation will be blended
Water is 1 in mass ratio：5 mixing are put into beaker, and beaker are placed in ultrasonic oscillation device, temperature be 70 DEG C, power is
Ultrasonic extraction 55min under conditions of 190W is filtered after extraction, collects filtrate, filtrate is evaporated under reduced pressure, and obtains self-control plant
Extracting solution, it is 1 by volume that will finally make plant extraction liquid by oneself with above-mentioned gained Self-made mixture：1 mixing, and with 230W power
11min, stratification are ultrasonically treated, separation removal lower water phase obtains premix；It is 1 in mass ratio：1：2 by strontium carbonate,
Barium carbonate and titanium dioxide mixing are put into kiln, are calcined 1.5h in the case where temperature is 900 DEG C, are ground 11min again after calcination
And 100 mesh sieves are crossed, sieving calcined powder is collected, is 3 in mass ratio by sieving calcined powder, dextrin and amber powder：2：1 mixing is stirred
18min is mixed, obtains modified porous powder；It is in mass ratio by modified porous powder, premix and silane resin acceptor kh-550
5：3：1 is mixed reaction 3h, obtains self-control stirring slurry, and self-control stirring slurry is poured into four-hole boiling flask and continues to stir
11min, and vacuumize, the bubble in slurry is removed, then the quality of stock quality 10% is stirred in addition self-control into four-hole boiling flask
The hydrogen peroxide and the sodium peroxydisulfate of self-control stirring stock quality 3% that fraction is 20%, the polymerisation 1.5h in the case where temperature is 50 DEG C,
Obtain self-control polymeric size；Polymeric size will be made by oneself to be injected into the mold that size is 180mm × 16mm × 2mm, and be positioned over
In drier, air drying 11min, is put into after dry in baking oven under nitrogen protection, dries 1.5h in the case where temperature is 55 DEG C, obtains
To self-control green body, and self-control green body is removed from the molds, self-control green body is put into crucible furnace, be sintered in the case where temperature is 1100 DEG C
2h, cooled to room temperature, dry discharging, you can high intensity, porous piezoelectric ceramics is made.
Example 3
It is 2 in mass ratio：1：12min is mixed in acrylamide, N, N- methylene-bisacrylamides and the tert-butyl alcohol by 3, is obtained
Mixture and deionized water are 1 in mass ratio by mixture：3 mixing are placed in beaker, continue to stir 15min, it is mixed to obtain self-control
Close liquid；It weighs 12g citruses and the mixing of 20g spinach is placed in pulper and blends 20min, obtain blending object, object and distillation will be blended
Water is 1 in mass ratio：5 mixing are put into beaker, and beaker are placed in ultrasonic oscillation device, temperature be 80 DEG C, power is
Ultrasonic extraction 60min under conditions of 200W is filtered after extraction, collects filtrate, filtrate is evaporated under reduced pressure, and obtains self-control plant
Extracting solution, it is 1 by volume that will finally make plant extraction liquid by oneself with above-mentioned gained Self-made mixture：1 mixing, and with 260W power
12min, stratification are ultrasonically treated, separation removal lower water phase obtains premix；It is 1 in mass ratio：1：2 by strontium carbonate,
Barium carbonate and titanium dioxide mixing are put into kiln, are calcined 2h in the case where temperature is 1000 DEG C, are ground 12min again simultaneously after calcination
100 mesh sieves are crossed, collect sieving calcined powder, are 3 in mass ratio by sieving calcined powder, dextrin and amber powder：2：1 is mixed
20min obtains modified porous powder；It is 5 in mass ratio by modified porous powder, premix and silane resin acceptor kh-550：
3：1 is mixed reaction 4h, obtains self-control stirring slurry, and self-control stirring slurry is poured into four-hole boiling flask and continues to stir 12min,
And vacuumize, the bubble in slurry is removed, then the mass fraction of addition self-control stirring stock quality 10% is into four-hole boiling flask
20% hydrogen peroxide and the sodium peroxydisulfate of self-control stirring stock quality 3%, the polymerisation 2h in the case where temperature is 55 DEG C are made by oneself
Polymeric size；Polymeric size will be made by oneself to be injected into the mold that size is 180mm × 16mm × 2mm, and be positioned in drier,
Air drying 12min under nitrogen protection is put into after dry in baking oven, and 2h is dried in the case where temperature is 60 DEG C, obtains self-control green body,
And self-control green body is removed from the molds, self-control green body is put into crucible furnace, 3h, natural cooling are sintered in the case where temperature is 1200 DEG C
To room temperature, dry discharging, you can high intensity, porous piezoelectric ceramics is made.
Comparative example
With the high intensity, porous piezoelectric ceramics of Sichuan company as a comparison case
High intensity, porous piezoelectric ceramics in high intensity, porous piezoelectric ceramics produced by the present invention and comparative example is subjected to performance inspection
It surveys, testing result is as shown in table 1：
1st, test method：
Porosity test is detected using mercury injection apparatus；
Intensity test is detected by 4740 standards of GB/T；
Vickers hardness test is detected using hardness-testing device；
Piezoelectric constant test is detected using D33 piezoelectricity testers；
Table 1
According to data in table 1, high intensity, porous piezoelectric ceramics intensity produced by the present invention is high, and the porosity is high, reaches 49%,
Piezoelectric property is good, and piezoelectric constant has reached 17pC/N, has broad application prospects.
Claims (6)
1. a kind of preparation method of high intensity, porous piezoelectric ceramics, it is characterised in that specifically preparation process is：
（1）By acrylamide, N, N- methylene-bisacrylamides and the tert-butyl alcohol are mixed, and obtain mixture, by mixture and
Deionized water mixing is placed in beaker, is continued to stir, is obtained Self-made mixture；
（2）Weigh 10~12g citruses and the mixing of 16~20g spinach be placed in pulper and blend, obtain blending object, will blend object and
Distilled water mixing is put into beaker, and beaker is placed in ultrasonic extraction in ultrasonic oscillation device, is filtered after extraction, collects filtrate,
Filtrate is evaporated under reduced pressure, obtains self-control plant extraction liquid, finally mixes self-control plant extraction liquid with the self-control of above-mentioned gained
Liquid mixing is ultrasonically treated, stratification, and separation removal lower water phase obtains premix；
（3）Strontium carbonate, barium carbonate and titanium dioxide are mixed to be put into kiln and calcined, grind again after calcination and crosses 100 mesh
Sieve collects sieving calcined powder, and sieving calcined powder, dextrin and amber powder are mixed, obtain modified porous powder；（4）
Modified porous powder, premix and silane resin acceptor kh-550 are mixed and reacted, self-control stirring slurry is obtained, will make by oneself
Stirring slurry, which is poured into four-hole boiling flask, to be continued to stir, and is vacuumized, and is removed the bubble in slurry, then is added certainly into four-hole boiling flask
The hydrogen peroxide of system stirring stock quality 10% and the sodium peroxydisulfate polymerisation of self-control stirring stock quality 3%, it is poly- to obtain self-control
Close slurry；
（5）Self-control polymeric size is injected into mold, and is positioned in drier, under nitrogen protection air drying, it is dry
After be put into baking oven and dry, obtain self-control green body, and be removed from the molds self-control green body, self-control green body be put into crucible furnace and is burnt
Knot, cooled to room temperature, dry discharging, you can high intensity, porous piezoelectric ceramics is made.
2. a kind of preparation method of high intensity, porous piezoelectric ceramics according to claim 1, it is characterised in that：Step（1）
The mass ratio of the acrylamide, N, N- methylene-bisacrylamides and the tert-butyl alcohol is 2：1：3, mixing time for 10~
The mass ratio of 12min, mixture and deionized water is 1：3, continuation mixing time is 11~15min.
3. a kind of preparation method of high intensity, porous piezoelectric ceramics according to claim 1, it is characterised in that：Step（2）
Described blends the time as 16~20min, and the mass ratio for blending object and distilled water is 1：5, ultrasonic extraction temperature is 60~80 DEG C,
Ultrasonic extraction power is 180~200W, and the ultrasonic extraction time is 45~60min, makes plant extraction liquid and Self-made mixture by oneself
Volume ratio is 1：1, sonification power is 200~260W, and sonication treatment time is 10~12min.
4. a kind of preparation method of high intensity, porous piezoelectric ceramics according to claim 1, it is characterised in that：Step（3）
The mass ratio of the strontium carbonate, barium carbonate and titanium dioxide is 1：1：2, calcining heat is 800~1000 DEG C, and calcination time is
1~2h, milling time are 10~12min, and the mass ratio of sieving calcined powder, dextrin and amber is 3：2：1, mixing time 16
~20min.
5. a kind of preparation method of high intensity, porous piezoelectric ceramics according to claim 1, it is characterised in that：Step（4）
The mass ratio of the modified porous powder, premix and silane resin acceptor kh-550 is 5：3：1, the time is stirred to react as 2
~4h, continuation mixing time are 10~12min, and the mass fraction of hydrogen peroxide is 20%, and reaction temperature is 45~55 DEG C, during reaction
Between be 1~2h.
6. a kind of preparation method of high intensity, porous piezoelectric ceramics according to claim 1, it is characterised in that：Step（5）
The die size is 180mm × 16mm × 2mm, and drying time is 10~12min, and drying temperature is 50~60 DEG C, drying
Time is 1~2h, and sintering temperature is 1000~1200 DEG C, and sintering time is 1~3h.
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| CN108911738A (en) * | 2018-07-06 | 2018-11-30 | 西安工业大学 | porous barium titanate piezoelectric ceramics and preparation method thereof |
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