CN1462761A - New method for preparing composite material of piezodielectric ceramics/polymer - Google Patents
New method for preparing composite material of piezodielectric ceramics/polymer Download PDFInfo
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- CN1462761A CN1462761A CN 03128078 CN03128078A CN1462761A CN 1462761 A CN1462761 A CN 1462761A CN 03128078 CN03128078 CN 03128078 CN 03128078 A CN03128078 A CN 03128078A CN 1462761 A CN1462761 A CN 1462761A
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Abstract
A composite piezoelectric ceramics/polymer material is prepared through adding acetate to polymer solution, stirring, stirring, heating to 60-120 deg.C, adding acetylacetone or glacial acetic acid, stirring, dropping titanate, reaction to obtain the nano ceramic sol containing polymer, distilling at 120-170 deg.C or depositing in solvent and drying, grinding to obtain the mother particles, mixing with ordinary piezoelectric ceramic powder, and die pressing.
Description
One, technical field:
The invention belongs to piezoelectric ceramics/polymer 1-3 thing matrix material category, a kind of new preparation process of piezoelectric ceramics/polymer 1-3 thing matrix material is provided, present method has solved the problem of piezoelectric ceramics/polymer 1-3 thing composite material interface in conjunction with difference, especially is suitable for preparation piezoelectric ceramics/polar polymer matrix material.
Two, background technology:
Utilizing polymer materials excellent mechanical property, film-forming properties and stupalith good electrical properties to carry out compound is a new way that is worth exploration.Synthetic gained matrix material has overcome the fragility of stupalith self and the temperature limitation of polymer materials, has improved some electrical property greatly.The recombining process of existing such matrix material of preparation mainly contains the hydrostomia method, pressure sintering and spin-coating method etc.
[1～6]All there is the problem in conjunction with difference of interface between polymkeric substance and the piezoelectric ceramics in above complex method, thereby has influenced the raising of composite property.
And have now when preparation polymkeric substance/piezo-electric ceramic composite material, the method for often using coupling agent that the piezoelectric ceramics surface is handled is improved two and is combined
[4～8], to obtain the matrix material of high-k, low-dielectric loss.But mostly used coupling agent is to increase the nonpolar of inorganic particulate surface usually, and for polar polymer, be difficult to improve the biphase bonding strength with coupling agent modified piezoelectric ceramics is compound, particularly when the recombining process that has shearing force to exist, coupling agent is difficult to play a role.Therefore the desired matrix material of difficult acquisition.
Sol-gel method is the main synthesis method of preparation nano material, and it has plurality of advantages such as goods purity and uniformity coefficient height, good moldability, is subjected to domestic and international material domain expert scholar's generally attention in recent years
[9～12]But do not see the report that utilizes sol-gel method to prepare piezoelectric ceramics/polymer 1-3 thing nanometer master batch as yet.
Reference: 1.M C W Lam, J Li.Linear pyroelectric sensor array based on PCLT/P (VDF/TrFE) composite Integrated.Ferroelectrics.2000,35:1817-18252.K C Cheng, H L W Chan.Mechanical quality factor of lead zirconate titanate/epoxycomposites.Materials Research Society Symposium-Proceedings.2000,628:24-283.E Venkatragavaraj, B Satish, P R Vinod et al.Piezoelectric properties offerroelectric PZT-polymer composites.Journal of Physics D.applied phyics, 2001,34 (4): 487-4924.C X Xiong, J Chen, L J Dong et al.Study on dielectric property and preparationmethod of BaTiO
3/ PVDF 0-3 composites.Journal of Wuhan University ofTechnology (Materials Science Edtion), 2002,17 (4): the 85-885. bear passes small stream, the outstanding .PVDF/ modification of Dong Li BaTiO
3The matrix material Dielectric Properties. polymer material science and engineering .2003, Vol.19 (1): 152-1556. Dong Li outstanding person, Xiong Chuanxi. scorification prepares PVDF/ modification BaTiO
3The matrix material Dielectric Properties. the matrix material journal. received 7.L Li, N R Sottos. Measurement of surface displacements in 1-3 and 1-1-3plezocomposites.Journal of Applied Physics.1996,79 (3): 1707-17128.T Hooshmand, R V Noort Bond durability of the resin-bonded and silane treatedceramic surface.Dental Materials.2002,18 (2): 179-1889.J Burs.k, R Kuzel, P Vanek.The textured PbTiO
3-Al
2O
3Composite films preparedby the sol-gel method.International Journal of Inorganic Materials.2001,3:485-49210.X R Fu, J H Li, Z T Song et al.Preparation of highly (100)-oriented PLCT thinfilms on Pt/Ti/SiO
2/ Si substrates by a simple sol-gel process.Materials Letters.2000,44:70-7411.W G Liu, J S Ko, W G Zhu.Preparation and properties of multilayer Pb (Zr, Ti) O
3/ PbTiO
3Thin films for pyroelectric application.Thin Solid Films.2000,371:254-25812.Y C Lai, J C Lin, C Lee.Nucleation and growth of highly oriented lead titanatethin films prepared by a sol-gel method.Applied Surface Science, 1998,125:51～57
Three, summary of the invention:
The invention provides the new preparation process of piezoelectric ceramics/polymer 1-3 thing matrix material, solving the problem of piezoelectric ceramics/polymer 1-3 thing composite material interface in conjunction with difference, and the compound problem of the coupling agent treatment piezoelectric ceramics commonly used surface polar polymer that is difficult to realize and coupling agent modified piezoelectric ceramics good interface.
Mechanism of the present invention: in polymers soln, utilize sol-gel method to prepare the piezoelectric ceramics nano particle, make the inorganic particulate original position be grown in the surface of polymkeric substance equably, obtain original position composite piezoelectric ceramic/polymer nanometer master batch.The nano-ceramic particle growth in situ that generates in the sol-gel method is on the surface of polymkeric substance, composite master batch and conventional ceramic powder compound tense, nano-ceramic particle in the composite master batch combines as binding site and conventional ceramic powder, making the conventional ceramic powder be aggregated thing fully wraps up, nano-ceramic particle has improved interface combination between piezoelectric ceramics and the polymkeric substance as coupling agent, has improved composite property.
The present invention adopts following technical proposal to realize:
1. add acetate and mix in polymers soln, be warming up to 60 ℃～120 ℃ after mixing and add methyl ethyl diketone or Glacial acetic acid, the back that stirs drips a certain amount of titanic acid ester, reacts the nano ceramics colloidal sol that obtained containing polymkeric substance in 1～4 hour.Directly under 120 ℃～170 ℃, distill then or pour into and carry out sedimentation in the solvent that is insoluble to used polymkeric substance, dry 1～10 day, behind the complete drying mixture is ground into fine powder and promptly gets piezoelectric ceramics/polymer 1-3 thing original position composite master batch.
2. original position composite master batch and common piezoelectric ceramic powder adding mixing equipment are mixed,, prepare piezoelectric ceramics/polymer 1-3 thing matrix material of the present invention according to method compression moulding in homemade mould of forming polymer.
Four, description of drawings:
Fig. 1 is preparation technology's schema of piezoelectric ceramics/polymer 1-3 thing matrix material, introduced the new preparation process of piezoelectric ceramics/polymer 1-3 thing matrix material, utilize sol-gel method at first in polymers soln, to prepare the original position composite master batch, the more compound interface of preparing of original position composite master batch and conventional ceramic powder is combined good piezoelectric ceramics/polymer 1-3 thing matrix material.
Fig. 2 is PbTiO
3The SEM photo of/PVDF matrix material under 10000 times can find that from photo spheroidal particle is the nano-PbTiO that generates in the sol-gel method
3, particle diameter is at 20～200nm, and growth in situ is on the surface of polymkeric substance, the nano-PbTiO in the composite master batch
3Combine common PbTiO as binding site and conventional ceramic powder
3By PbTiO
3/ PVDF nanometer master batch all coats, and the interface is in conjunction with good.
Five, embodiment:
Embodiment 1: add plumbic acetate and mix in PVDF solution, be warming up to 60 ℃～120 ℃ after mixing and add methyl ethyl diketone, the back that stirs drips a certain amount of titanic acid ester, reacts to obtain PVDF/nano-PbTiO in 1～4 hour
3Colloidal sol.Pour into then and carry out sedimentation in the water, sediment washs repeatedly, is placed in the air and dries, and behind the complete drying mixture is ground into fine powder and obtains composite master batch.Again with composite master batch and common PbTiO
3Powder mixes, and suppresses 10～30min down in 150 ℃～200 ℃ and makes matrix material.Test under 1000kHz, when the PVDF volume content had 40%, the specific inductivity of matrix material was higher than 50, and tangent of the dielectric loss angle tan δ is less than 0.07, and SEM observes the nano-PbTiO that generates in the discovery sol-gel method
3Growth in situ is on the surface of polymkeric substance, common PbTiO
3All coated by PVDF nanometer master batch, the interface is in conjunction with good, as shown in Figure 2.
Embodiment 2: add barium acetate and mix in PVC solution, be warming up to 60 ℃～120 ℃ after mixing and add acetic acid, the back that stirs drips a certain amount of titanic acid ester, reacts to obtain PVC/nano-BaTiO in 1～4 hour
3Colloidal sol is placed on after 120 ℃～170 ℃ are distilled down and dries in the air, behind the complete drying mixture is ground into fine powder and obtains composite master batch.Again with composite master batch and common BaTiO
3Powder mixes, and compacting 10～30min makes matrix material in the time of 140 ℃～180 ℃.
Claims (1)
1, a kind of new preparation process of piezoelectric ceramics/polymer 1-3 thing matrix material, it is characterized in that: a: in polymers soln, add acetate and mix, be warming up to 60 ℃～120 ℃ after mixing and add methyl ethyl diketone or Glacial acetic acid, drip a certain amount of titanic acid ester after stirring, react the nano ceramics colloidal sol that obtained containing polymkeric substance in 1～4 hour.Directly under 120 ℃～170 ℃, distill then or pour into and carry out sedimentation in the solvent that is insoluble to used polymkeric substance, dry 1～10 day, behind the complete drying mixture is ground into fine powder and promptly gets piezoelectric ceramics/polymer 1-3 thing original position composite master batch.B: original position composite master batch and common piezoelectric ceramic powder adding mixing equipment are mixed,, prepare piezoelectric ceramics/polymer 1-3 thing matrix material of the present invention according to method compression moulding in homemade mould of forming polymer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1314747C (en) * | 2005-01-27 | 2007-05-09 | 武汉理工大学 | Piezoelectric ceramic and pioloform composite materials |
| CN100436529C (en) * | 2005-01-25 | 2008-11-26 | 武汉理工大学 | Interface modifier of organic polymer and iron inorganic composite materials and its preparation |
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2003
- 2003-05-30 CN CN 03128078 patent/CN1213094C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100436529C (en) * | 2005-01-25 | 2008-11-26 | 武汉理工大学 | Interface modifier of organic polymer and iron inorganic composite materials and its preparation |
| CN1314747C (en) * | 2005-01-27 | 2007-05-09 | 武汉理工大学 | Piezoelectric ceramic and pioloform composite materials |
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