CN104332250A - Preparation method for electrode silver palladium slurry in laminated piezoelectric ceramic loudspeaker - Google Patents
Preparation method for electrode silver palladium slurry in laminated piezoelectric ceramic loudspeaker Download PDFInfo
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- CN104332250A CN104332250A CN201410526757.4A CN201410526757A CN104332250A CN 104332250 A CN104332250 A CN 104332250A CN 201410526757 A CN201410526757 A CN 201410526757A CN 104332250 A CN104332250 A CN 104332250A
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Abstract
The invention discloses a preparation method for electrode silver palladium slurry in a laminated piezoelectric ceramic loudspeaker. The preparation method comprises the following steps that 1) raw material, including silver palladium alloy powder, porcelain powder or glass powder and organic carriers, is weighed, silver palladium alloy powder is prepared by adopting a chemical co-reduction method, ratio of silver to palladium is 1/99-9/91, and the three types of raw material is evenly stirred by a high-speed stirring machine so that silver palladium slurry is obtained, wherein the content of silver palladium alloy powder is 40wt.%-70wt.%, the content of porcelain powder or glass powder is 1wt.%-10wt.%, the content of organic carriers is 30wt.%-60wt.%, and the content of addition agent is 0.1wt.%-10wt.%, based on which the total content of silver palladium slurry is 100wt.%; and 2) the evenly stirred silver palladium slurry is rolled by a three-roll grinder with fineness of being lower than 5 microns, and then the finished product of slurry is obtained via 30min stirring by the high-speed stirring machine. The prepared silver palladium slurry has great technological property, a piezoelectric ceramic membrane is not corroded in printing, drying can be completed after 30min at temperature of 70 DEG C, and great separating of the piezoelectric ceramic membrane and a PET membrane can be realized. After sintering at temperature of 930 DEG C, the electrode is bright, great in solderability and high in sound intensity, and does not deform.
Description
Technical field
The present invention relates to stacked piezoelectric ceramic loudspeaker field, be specifically related to the preparation method of electrode silver palladium slurry in a kind of stacked piezoelectric ceramic loudspeaker.
Background technology
Electric slurry is a kind of functional material, mainly for the manufacture of thick film hybrid integrated circuit, resistor, multilayer ceramic capacitor, resistor network, sensitive components and other electronic devices and components, is the base electronic material of electronics and information industry.Electric slurry is generally made up of parts such as metal dust, inorganic bond phase, organic carrier and additives.Metal dust forms conduction after sintering and connects, metallic particles firmly bonds together by inorganic adhesive mutually after sintering, and give rete mechanical performance and the adhesive force to ground, organic carrier by mutually dispersed to metal dust and inorganic bond become paste, give mobility, thixotropy that slurry is certain, make slurry be suitable for printing.Additive comprises thixotropic agent, levelling agent, plasticizer and surfactant etc.Conventional metal dust is silver, because it has good conduction, heat conductivility, again because its price is relatively cheap, in a large number for electronics and information industry, but there is silver ion migration in silver paste, soldering resistance is poor, the shortcomings such as fusing point is low, in some high stability, high reliability, and sintering temperature high when, silver paste can not meet requirement.The performances such as palladium just in time has anti-silver ion migration, and soldering resistance is strong, and fusing point is high, therefore silver-colored palladium slurry is applicable to the occasion being applied in high-end electronic components and parts and high sintering temperature very much.
Piezoelectric ceramic loudspeaker utilizes piezoelectric effect, audio voltage signal is inputted to the piezoceramics film oscillator be attached on plate diaphragm (interior electrode), make ceramic membrane oscillator produce stretching vibration, thus drive the vibration of plate diaphragm generation mechanical bend to promote air sounding.Because the sintering temperature of piezoceramics film is higher, silver paste cannot obtain complete electrode, and silver-colored palladium slurry is most suitable material.CN101697317B discloses a kind of preparation method of unleaded silver-palladium inner electrode slurry used for multilayer ceramic capacitor, the silver-colored palladium slurry that this patent relates to is applied to multilayer ceramic capacitor, silver palladium ratio is up to 10/90, and conducting function is the mixture of silver powder and palladium powder mutually, and the non-chemically palladium-silver alloy powder that obtains of co-reducing process.
The complicated process of preparation of electrode in stacked piezoelectric ceramic loudspeaker, very high to the requirement of silver-colored palladium slurry, requirement in demand fulfillment operation, such as print disposed slurry and do not corrode ceramic membrane, ceramic membrane can from good separation PET film after drying, and in after sintering, electrode is indeformable, the complete densification of interior electrode, solderability is good, and the sound intensity is high.
Summary of the invention
The object of the present invention is to provide the preparation method of electrode silver palladium slurry in a kind of stacked piezoelectric ceramic loudspeaker, silver-colored palladium slurry combination property prepared by this method is superior, cost performance is high, well can be applied to the making of electrode in stacked piezoelectric ceramic loudspeaker, the import silver palladium slurry of alternative same domain.In stacked piezoelectric ceramic loudspeaker provided by the invention, the preparation method of electrode silver palladium slurry comprises the following steps:
1) raw material is taken: palladium-silver alloy powder, porcelain powder or glass dust and organic carrier, described palladium-silver alloy powder adopts chemical co-reducing process to prepare, wherein silver-colored palladium ratio is 1/99 ~ 9/91, adopt homogenizer to stir described three kinds of raw materials and obtain silver-colored palladium slurry, wherein said silver palladium alloy powder content is 40wt.% ~ 70wt.%, porcelain powder or glass dust content are 1wt.% ~ 10wt.%, organic carrier content is 30wt.% ~ 60wt.%, additive level is 0.1wt.% ~ 10wt.%, in described silver-colored palladium slurry total amount for 100wt.%;
2) by the silver-colored palladium slurry that stirs by three-roll grinder rolling, fineness reaches less than 5 μm, then stirs 30min by homogenizer and obtains slurry finished product.
According to some embodiment of the present invention, described palladium-silver alloy powder adopts and dries higher than the temperature of normal temperature, and the average grain diameter of described palladium-silver alloy powder is 1 ~ 5 μm, and apparent density is 0.8 ~ 1.5g/cm
3, tap density is 1.5 ~ 3.0 g/cm3, and specific area is 2.0 ~ 6.0m/g.
According to some embodiment of the present invention, described organic carrier comprises ethyl cellulose-terpinol system and water-soluble resin-ol kind solvent, described ethyl cellulose mass fraction is 10 ~ 15wt.%, the mass fraction of described water-soluble resin is 15 ~ 50wt.%, in the mass fraction of described organic carrier for 100wt.%, described ethyl cellulose-terpinol and described water-soluble resin-ol kind solvent mass ratio 90/10 ~ 40/60.
According to some embodiment of the present invention, described water-soluble resin be selected from following in one or more: polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol and alkyd resins.
According to some embodiment of the present invention, described additive be selected from following in one or more: castor oil, tributyl citrate, dibutyl phthalate and phosphate.
According to some embodiment of the present invention, described porcelain powder is piezoelectric ceramic powder.
Foregoing invention content is not intended to each disclosed embodiment describing often kind of execution mode of the present invention.More specifically illustrate exemplary embodiment below in conjunction with embodiment, the Characteristics and advantages of above-mentioned and further embodiment of the present invention can be made more obvious.
Embodiment
Should be appreciated that when do not depart from the scope of the present invention or spirit, those skilled in the art can imagine other various embodiment can modifying to it according to the instruction of this specification.Therefore, following embodiment does not have restrictive, sense.
Except as otherwise noted, otherwise all numerals of the representation feature size, quantity and the physical characteristic that use in this specification and claim be all construed as and all modified by term " about " in all cases.Therefore, unless indicated to the contrary, otherwise the numerical parameter listed in above-mentioned specification and appended claims is all approximations, those skilled in the art can utilize instruction content disclosed herein to seek the desirable characteristics obtained, these approximations of appropriate change.The use of the number range represented with end points comprises all numerals within the scope of this and any scope within the scope of this, and such as, 1,2,3,4 and 5 comprise 1,1.1,1.3,1.5,2,2.75,3,3.80,4 and 5 etc.
embodiment 1:
1) 0.6Kg palladium sponge is dissolved with the red fuming nitric acid (RFNA) that 4.5L concentration is 65%, use 150 L deionized water dissolving 46.3Kg silver nitrates in a kettle., the palladium nitrate solution dissolved is transferred in reactor, adds deionized water and make overall solution volume be 250L, open stirring and solution is mixed.Add alkali precipitation agent, until pH value in solution is 10.In reactor, add 0.3Kg lauryl sodium sulfate, open heating, design temperature 60 DEG C, treats that temperature stabilization is 60 DEG C, in solution, slowly adds 10Kg hydrazine hydrate solution, adds completely and continues reaction 30min.Filter after washing 5 times, then silver-colored palladium powder is dried 24h under 80 DEG C of conditions.
2) take 5Kg ethyl cellulose, add 45Kg terpinol, stir 8h through homogenizer and obtain ethyl cellulose-terpinol carrier (1# carrier) that mass fraction is 10%.Take 15Kg polyvinylpyrrolidone, add 35Kg ethylene glycol, obtain through high-speed stirred 4h polyvinylpyrrolidone-ethylene glycol carrier (2# carrier) that mass fraction is 30%.
3) raw material is taken according to one batch of 30Kg silver palladium slurry: palladium-silver alloy powder (55%): 16.5Kg; Porcelain powder (2%): 0.6Kg; 1# carrier (34%): 10.2Kg; 2# carrier (8.5%): 2.55Kg; Castor oil (0.5%): 0.15Kg.Mix with homogenizer.
4) three rollers grindings: by the silver-colored palladium slurry that stirs by three-roll grinder rolling 4 times, fineness reaches less than 5 μm, then stirs 30min by homogenizer and obtains slurry finished product.
embodiment 2:
1) 1.5Kg palladium sponge is dissolved with the red fuming nitric acid (RFNA) that 12L concentration is 68%, use 150L deionized water dissolving 44.9Kg silver nitrate in a kettle., the palladium nitrate solution dissolved is transferred in reactor, adds deionized water and make overall solution volume be 250L, open stirring and solution is mixed.Add alkali precipitation agent, until pH value in solution is 12.In reactor, add 0.3Kg polyvinylpyrrolidone, open heating, design temperature 60 DEG C, treats that temperature stabilization is 60 DEG C, in solution, slowly adds 10Kg hydrazine hydrate solution, adds completely and continues reaction 30min.Filter after washing 5 times, then silver-colored palladium powder is dried 24h at 80 DEG C.
2) take 5Kg ethyl cellulose, add 45Kg terpinol, stir 8h through homogenizer and obtain ethyl cellulose-terpinol carrier (1# carrier) that mass fraction is 10%.Take 15Kg polyvinylpyrrolidone, add 35Kg ethylene glycol, obtain through high-speed stirred 4h polyvinylpyrrolidone-ethylene glycol carrier (2# carrier) that mass fraction is 30%.
3) raw material is taken according to one batch of 30Kg silver palladium slurry: palladium-silver alloy powder (55%): 16.5Kg; Porcelain powder (3%): 0.9Kg; 1# carrier (33.2%): 9.96Kg; 2# carrier (8.3%): 2.49Kg; Dibutyl phthalate (0.5%): 0.15Kg.Mix with homogenizer.
4) three rollers grindings: by the silver-colored palladium slurry that stirs by three-roll grinder rolling 6 times, fineness reaches less than 5 μm, then stirs 30min by homogenizer and obtains slurry finished product.
embodiment 3:
1) 0.6Kg palladium sponge is dissolved with the red fuming nitric acid (RFNA) that 4.5L concentration is 66%, use 150 L deionized water dissolving 46.3Kg silver nitrates in a kettle., the palladium nitrate solution dissolved is transferred in reactor, adds deionized water and make overall solution volume be 250L, open stirring and solution is mixed.Add alkali precipitation agent, until pH value in solution is 11.In reactor, add 0.3Kg alcohol amine compound, open heating, design temperature 60 DEG C, treats that temperature stabilization is 60 DEG C, in solution, slowly adds 10Kg hydrazine hydrate solution, adds completely and continues reaction 30min.Filter after washing 5 times, then silver-colored palladium powder is dried 24h at 80 DEG C.
2) take 5Kg ethyl cellulose, add 45Kg terpinol, stir 8h through homogenizer and obtain ethyl cellulose-terpinol carrier (1# carrier) that mass fraction is 10%.Take 10Kg alkyd resins, add 40Kg ethylene glycol, obtain through high-speed stirred 4h alkyd resins-ethylene glycol carrier (3# carrier) that mass fraction is 20%.
3) raw material is taken according to one batch of 30Kg silver palladium slurry: palladium-silver alloy powder (60%): 18Kg; Porcelain powder (3%): 0.9Kg; 1# carrier (33.25%): 9.975Kg; 3# carrier (3.65%): 1.095Kg; Dibutyl phthalate (0.1%): 0.03Kg.Mix with homogenizer.
4) three rollers grindings: by the silver-colored palladium slurry that stirs by three-roll grinder rolling 5 times, fineness reaches less than 5 μm, then stirs 30min by homogenizer and obtains slurry finished product.
embodiment 4:
1) 1.5Kg palladium sponge is dissolved with the red fuming nitric acid (RFNA) that 12L concentration is 67%, use 150L deionized water dissolving 44.9Kg silver nitrate in a kettle., the palladium nitrate solution dissolved is transferred in reactor, adds deionized water and make overall solution volume be 250L, open stirring and solution is mixed.Add alkali precipitation agent, until pH value in solution is 11.In reactor, add 0.3Kg lauryl sodium sulfate, open heating, setting reaction temperature 60 DEG C, question response temperature stabilization is 60 DEG C, in solution, slowly add 10Kg hydrazine hydrate solution, adds completely and continues reaction 30min.Filter after washing 5 times, then silver-colored palladium powder is dried 24h at 80 DEG C.
2) take 7.5Kg ethyl cellulose, add 42.5Kg terpinol, stir 8h through homogenizer and obtain ethyl cellulose-terpinol carrier (4# carrier) that mass fraction is 15%.Taking 20Kg polyvinylpyrrolidone, add 30Kg alcohols solvent, obtaining through stirring 4h the alkyd resins-ol kind solvent carrier (5# carrier) that mass fraction is 40%.
3) raw material is taken according to one batch of 30Kg silver palladium slurry: palladium-silver alloy powder (50%): 15Kg; Porcelain powder (1%): 0.3Kg; 4# carrier (24%): 7.2Kg; 5# carrier (24%): 7.2Kg; Phosphate (1%): 0.3Kg.Mix with homogenizer.
4) three rollers grindings: by the silver-colored palladium slurry that stirs by three-roll grinder rolling 6 times, fineness reaches less than 5 μm, then stirs 30min by homogenizer and obtains slurry finished product.
Claims (6)
1. the preparation method of electrode silver palladium slurry in stacked piezoelectric ceramic loudspeaker, comprises the following steps:
1) raw material is taken: palladium-silver alloy powder, porcelain powder or glass dust and organic carrier, described palladium-silver alloy powder adopts chemical co-reducing process to prepare, wherein silver-colored palladium ratio is 1/99 ~ 9/91, adopt homogenizer to stir described three kinds of raw materials and obtain silver-colored palladium slurry, wherein said silver palladium alloy powder content is 40wt.% ~ 70wt.%, porcelain powder or glass dust content are 1wt.% ~ 10wt.%, organic carrier content is 30wt.% ~ 60wt.%, additive level is 0.1wt.% ~ 10wt.%, in described silver-colored palladium slurry total amount for 100wt.%;
2) by the silver-colored palladium slurry that stirs by three-roll grinder rolling, fineness reaches less than 5 μm, then stirs 30min by homogenizer and obtains slurry finished product.
2. preparation method as claimed in claim 1, is characterized in that, described palladium-silver alloy powder adopts and dries higher than the temperature of normal temperature, the average grain diameter of described palladium-silver alloy powder is 1 ~ 5 μm, apparent density is 0.8 ~ 1.5g/cm3, and tap density is 1.5 ~ 3.0 g/cm3, and specific area is 2.0 ~ 6.0m/g.
3. preparation method as claimed in claim 1, it is characterized in that, described organic carrier comprises ethyl cellulose-terpinol system and water-soluble resin-ol kind solvent, described ethyl cellulose mass fraction is 10 ~ 15wt.%, the mass fraction of described water-soluble resin is 15 ~ 50wt.%, in the mass fraction of described organic carrier for 100wt.%, described ethyl cellulose-terpinol and described water-soluble resin-ol kind solvent mass ratio 90/10 ~ 40/60.
4. preparation method as claimed in claim 1, is characterized in that, described water-soluble resin be selected from following in one or more: polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol and alkyd resins.
5. preparation method as claimed in claim 1, is characterized in that, described additive be selected from following in one or more: castor oil, tributyl citrate, dibutyl phthalate and phosphate.
6. preparation method as claimed in claim 1, it is characterized in that, described porcelain powder is piezoelectric ceramic powder.
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| CN1103057A (en) * | 1993-07-29 | 1995-05-31 | 纳幕尔杜邦公司 | Lead-free thick film paste composition |
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| JPH11232926A (en) * | 1998-02-13 | 1999-08-27 | Murata Mfg Co Ltd | Paste for ceramic internal electrode |
| CN1571855A (en) * | 2001-10-18 | 2005-01-26 | 加拿大电子粉末公司 | Powder for laminated ceramic capacitor internal electrode |
| CN1832068A (en) * | 2006-03-10 | 2006-09-13 | 潮州三环（集团）股份有限公司 | Inner electrode size of ceramic capacitor and preparation method thereof |
| CN101697317A (en) * | 2009-10-27 | 2010-04-21 | 彩虹集团公司 | Preparation method for unleaded silver-palladium inner electrode slurry used for multilayer ceramic capacitor |
| CN102270513A (en) * | 2010-06-03 | 2011-12-07 | 西安宏星电子浆料科技有限责任公司 | Thick-film conductor paste used for alumina substrate and preparation method of thick-film conductor paste |
| US20120140375A1 (en) * | 2010-12-06 | 2012-06-07 | Samsung Electro-Mechanics Co., Ltd. | Conductive paste for inner electrode and multilayer ceramic electronic component having the same |
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2014
- 2014-10-09 CN CN201410526757.4A patent/CN104332250A/en active Pending
Patent Citations (8)
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| CN1103057A (en) * | 1993-07-29 | 1995-05-31 | 纳幕尔杜邦公司 | Lead-free thick film paste composition |
| CN1212441A (en) * | 1997-09-19 | 1999-03-31 | 广东肇庆风华电子工程开发有限公司 | Chip multilayer ceramic capacitor palladium-silver inside electrode size |
| JPH11232926A (en) * | 1998-02-13 | 1999-08-27 | Murata Mfg Co Ltd | Paste for ceramic internal electrode |
| CN1571855A (en) * | 2001-10-18 | 2005-01-26 | 加拿大电子粉末公司 | Powder for laminated ceramic capacitor internal electrode |
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| CN101697317A (en) * | 2009-10-27 | 2010-04-21 | 彩虹集团公司 | Preparation method for unleaded silver-palladium inner electrode slurry used for multilayer ceramic capacitor |
| CN102270513A (en) * | 2010-06-03 | 2011-12-07 | 西安宏星电子浆料科技有限责任公司 | Thick-film conductor paste used for alumina substrate and preparation method of thick-film conductor paste |
| US20120140375A1 (en) * | 2010-12-06 | 2012-06-07 | Samsung Electro-Mechanics Co., Ltd. | Conductive paste for inner electrode and multilayer ceramic electronic component having the same |
Non-Patent Citations (1)
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Application publication date: 20150204 |