CN104446521A - Process for lowering calcination temperature of PZT piezoelectric material powder - Google Patents

Process for lowering calcination temperature of PZT piezoelectric material powder Download PDF

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CN104446521A
CN104446521A CN201410620605.0A CN201410620605A CN104446521A CN 104446521 A CN104446521 A CN 104446521A CN 201410620605 A CN201410620605 A CN 201410620605A CN 104446521 A CN104446521 A CN 104446521A
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material powder
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powder
piezoelectricity
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CN104446521B (en
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田永光
严红光
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Guangdong wisdom intelligent Polytron Technologies Inc
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DONGGUAN SWEET SOUND ELECTRONICS Co Ltd
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Abstract

The invention discloses a process for lowering calcination temperature of PZT piezoelectric material powder, and relates to a piezoelectric ceramic technology. The process comprises the following steps: baking, and burdening; carrying out ball-mill mixing to obtain the PZT piezoelectric material powder; carrying out pre-press forming on the PZT piezoelectric material powder to obtain blocks; synthesizing at low temperature: calcining and synthesizing the blocks which are formed by pre-press forming in a tunnel furnace at 850-950 DEG C; carrying out ball-milling again; drying: vaporizing the moisture in the material; 7 sieving through a 200mesh sieve to prepare formed powder; molding: adding hydroxypropyl methyl cellulose, glycerinum, ethyl alcohol and water to the powder, mixing, rolling, staling, and carrying out extrusion forming; discharging rubber and sintering; and polarizing by virtue of an electrode. The process has the advantages that calcining at low temperature is performed after pre-pressing; the reaction is rapid and full; the sintering energy source is saved; the equipment loss is lowered; the production cost is reduced; and the quality is improved.

Description

A kind of technique reducing PZT piezoelectricity material powder calcining temperature
Technical field
The present invention relates to piezoelectric ceramic technology, espespecially a kind of technique reducing PZT piezoelectricity material powder calcining temperature.So-called PZT piezoelectricity material powder is generate PZT piezoelectric raw material powder used.
Background technology
The main component of PZT piezoelectric is zirconium phthalandione lead (Pb (Ti, Zr) O 3.It is made up through techniques such as calcinings of the raw material powder (PZT piezoelectricity material powder) generating PZT piezoelectric used.In existing calcining process, PZT piezoelectricity material powder is dispensed into the high-temperature calcination through 1100 DEG C ~ 1300 DEG C in crucible.The problem that existing technique is brought is:
The first, temperature is wayward, and temperature is too low, reacts insufficient, principal crystalline phase poor quality; Temperature is high, burns block hardening, not easily pulverizes, active reduction, makes firing temperature raise or narrow; Generally according to test, suitable synthesis temperature need be determined.
The second, calcine at 1100 DEG C ~ 1300 DEG C temperature, waste energy.
3rd, crucible repeatedly through high-temperature calcination, generally through 7 times, will be damaged, consumptive material increases.
4th, at 1100 DEG C ~ 1300 DEG C temperature lower calcinations, equipment loss is comparatively large, increases production cost, as: the loss of heating carbon-point is large, and the replacing of body of heater refractory brick is frequent.
Summary of the invention
The technical issues that need to address of the present invention overcome the calcining of existing PZT piezoelectricity material powder to need temperature higher, and energy dissipation, frock, equipment loss are comparatively large, and the deficiency that production cost is higher, provides a kind of technique reducing PZT piezoelectricity material powder calcining temperature.The technique of this technique to calcining is optimized, and reduces calcining temperature, can ensure product performance, can realize again saving energy and reduce the cost, reduce costs.
For this reason, a kind of technique reducing PZT piezoelectricity material powder calcining temperature of the present invention adopts following technical proposals:
Reduce a technique for PZT piezoelectricity material powder calcining temperature, comprising:
Step 1, baking, batching, to the baking of used raw material, make the moisture content in absorption raw material discharge, and calculates required each raw material and weigh according to general formula;
Step 2, ball milling mixes, and makes its granularity reach≤1.5um, mixes, and obtains PZT piezoelectricity material powder;
Step 3, pre-molding, by described PZT piezoelectricity material powder briquetting, before compacting in described PZT piezoelectricity material powder, stir and add the water that its weight is described PZT piezoelectricity material powder 4 ~ 6%, and weight is the polyvinyl alcohol solution of described PZT piezoelectricity material powder 1 ~ 3%, concentration 4 ~ 6%, and weight is the dehydrated alcohol of described PZT piezoelectricity material powder 1 ~ 3%, pressure-controlling, at 6MPa ~ 8MPa, adopts impact briquetting mode;
Step 4, low temperature synthesizes, and is synthesized by the material block of pre-molding in tunnel stove in 850 DEG C ~ 950 DEG C calcinings;
Step 5, again ball milling, implement ball mill pulverizing to the material block synthesized through low temperature, cause granularity to reach≤0.09um;
Step 6, dry, by the moisture content vaporization in material, adopt electrothermal drying, put into baking oven baking, 140 DEG C ~ 160 DEG C, 20h ~ 25h;
Step 7, sieves, and by the material toasted, is down to normal temperature, crosses 200 mesh sieves; Be prepared into molding mass powder;
Step 8, shaping, add Vltra tears, glycerine, alcohol and water, mixing, roll off, old and extrusion molding in material powder;
Step 9, binder removal and sintering, in circulation tunnel stove, binder removal, sinter ceramic plate into, sintering temperature 1280 DEG C ~ 1300 DEG C;
Step 10, by electrode, by the silver slurry of required diameter, thickness 0.01mm in the ceramic plate two surface silk screen printing of preparation, in tunnel stove, 340 DEG C ~ 360 DEG C oven dry, load in square crucible, put into tunnel stove 775 DEG C ~ 785 DEG C silver ink firings, Temperature fall, to room temperature, is made by silver-colored ceramic plate;
Step 11, polarization, will be put into automatic tunnel polarization machine by silver-colored ceramic plate and be warmed up to 145 DEG C ~ 155 DEG C, 3kv/mm ~ 5kv/mm voltage polarizing 15 minutes to 25 minutes, make the piezoelectricity pottery silver strip with piezoelectricity.
Further, described general formula is
0.02Pb(Sb 1/3.Nb 2/3)O 3- 0.47(Pb 0.7Sr 0.3)TiO 3- 0.51PbZrO 3
The mechanism of present invention process is described below:
1, the raw material mixed is pressed into block, makes interparticle contact area as far as possible large, be beneficial to the carrying out of solid state reaction.Pressure can not be too large, general pressure-controlling at about 6MPa ~ 8MPa, impact briquetting.Material powder is too dry, the easy layering of briquetting, cracked; Usually add water the water of heavily about 5% (reinforced) mix
2, the main purpose of calcining is that raw material generates lead titanate piezoelectric ceramics through chemical reaction, and in the reaction generating Pb-based lanthanumdoped zirconate titanates, mainly the lead ion of plumbous oxide spreads in titanium oxide, zirconium white; Pressurization object make each raw material energy close contact, mutual diffusion ratio is easier to, reaction carry out comparatively fast, more abundant.
3, the selection of temperature makes being obtained by reacting of generation lead titanate piezoelectric ceramics fully carry out, and temperature is too low, and react insufficient, degradation, firing range is narrow.Calcining temperature is too high, and PbO volatilizees, and makes the material block after calcining too hard, is difficult to pulverize, brings adverse consequences to performance and technique.For lead titanate piezoelectric ceramics, wherein the fusing point of red lead is 880 DEG C, has larger activity, can react with other materials at a lower temperature, is conducive to pottery synthesis.Plumbous oxide has obvious volatilization when more than 1050 DEG C, needs sealing during high-temperature calcination.
4, after briquetting, at about 650 DEG C insulation 2h, can lead titanate be generated, be incubated about 2h about about 900 DEG C, can Pb-based lanthanumdoped zirconate titanates be generated.The length of soaking time, can determine according to the number of the size of briquetting and charging.
5, can not add a cover during calcining, when filling with substance can not fill too full, too crowded, and block and interblock need keep space, and under normal circumstances, after calcining, material block is long-pending increases, and crackle in length and breadth, even peels off.
The invention has the beneficial effects as follows:
1, after precompressed, low temperature calcination, reaction is carried out very fast, and more fully, material block is long-pending to be increased, and crackle in length and breadth, even peels off, and need not pulverize, and sintering range is broadened, and also can reduce temperature sintering; Save the sintering energy.
2, calcine at 800 DEG C ~ 1000 DEG C temperature, save energy.
3, without potcal pot calcination, use saggar after being pressed into briquetting in advance, can not add a cover, can repeatedly calcine, reduce frock loss..
4, at 800 DEG C ~ 1000 DEG C temperature lower calcinations, equipment loss reduces, and saves production cost, as: the loss of heating carbon-point reduces, and the high-temperature calcination of body of heater refractory brick is changed every year, reduces to 2 years and clears up in-furnace dust dirt 1 time, 5 years replacing stove bricks 1 time.
5, cost declines, 1) calcination reaction carries out very fast comparatively abundant, only need 800 DEG C ~ about 1000 DEG C calcinings, the corresponding calcining per kilogram material electricity charge 1.0 yuan/kg; 2) frock cost depletions per kilogram 0.10 yuan/kg; 3) equipment is reduced to maintenance in several years, per kilogram powder cost 0.05 yuan/kg.
High/low temperature calcines cost-saving comparison sheet
Specifeca tion speeification contrast table after high and low temperature calcining
In table: T DEG C, calcining temperature; Kp, electromechanical coupling factor; Qm, mechanical quality factor; ∑, specific inductivity; Tg δ, dielectric loss.
Embodiment
Below, specific embodiments of the invention are introduced.
Reduce a technique for PZT piezoelectricity material powder calcining temperature, comprising:
Step 1, baking, batching, its general formula is
0.02Pb(Sb 1/3.Nb 2/3)O 3- 0.47(Pb 0.7Sr 0.3)TiO 3- 0.51PbZrO 3
By above-mentioned general formula, desired raw material is toasted, the moisture content in absorption raw material is discharged, calculate required each raw material according to general formula and weigh; The main composition of its raw material is Pb 3o 4, ZrO 2, TiO 2, SrCO 3, Nb 2o 5, Sb 2o 3, weigh by the formula of chemical formula, above main composition gross weight is 100%, adds 0.001Wt%BiFeO 3;
Step 2, ball milling mixes, and makes its granularity reach≤1.5um, mixes, and obtains PZT piezoelectricity material powder;
Step 3, pre-molding, by described PZT piezoelectricity material powder briquetting, before compacting in described PZT piezoelectricity material powder, stir and add the water that its weight is described PZT piezoelectricity material powder 5%, and weight is the polyvinyl alcohol solution of described PZT piezoelectricity material powder 2%, concentration 5%, and weight is the dehydrated alcohol of described PZT piezoelectricity material powder 2%, pressure-controlling, at 6MPa ~ 8MPa, adopts impact briquetting mode;
Step 4, low temperature synthesizes, and is synthesized by the material block of pre-molding in tunnel stove in 850 DEG C ~ 950 DEG C calcinings;
Step 5, again ball milling, implement ball mill pulverizing to the material block synthesized through low temperature, cause granularity to reach≤0.09um;
Step 6, dry, by the moisture content vaporization in material, adopt electrothermal drying; Put into baking oven and toast 150 DEG C, 20h; Dry the length of material time, according to feeded number and determine;
Step 7, sieves, and by the material toasted, is down to normal temperature, crosses 200 mesh sieves; Be prepared into molding mass powder.
Step 8, shaping, Vltra tears, glycerine, alcohol and water is added in material powder, mixing, roll off, old and extrusion molding, as added weight 2%, the Gonak of concentration 15 ~ 20%, 1% glycerine, 5% alcohol and water (determining to add appropriate filtered water according to the dry wet situation of compound) in material powder;
Step 9, binder removal and sintering, in circulation tunnel stove, binder removal, sinter ceramic plate into, sintering temperature 1280 DEG C ~ 1300 DEG C, insulation 1h binder removal, and existing technique sintering temperature needs 1320 DEG C ~ 1340 DEG C;
Step 10, by electrode, by the silver slurry of required diameter, thickness 0.01mm in the ceramic plate two surface silk screen printing of preparation, in tunnel stove, 350 DEG C of oven dry, load in square crucible, put into 780 DEG C, tunnel stove, be incubated 10-15 minute silver ink firing, Temperature fall, to room temperature, is made by silver-colored ceramic plate;
Step 11, polarization, will be put into automatic tunnel polarization machine by silver-colored ceramic plate and be warmed up to 150 DEG C, 3kv/mm ~ 5kv/mm voltage polarizing 20 minutes, making general formula is
0.02Pb (Sb 1/3.Nb 2/3) O 3- 0.47(Pb 0.7sr 0.3) TiO 3- 0.51pbZrO 3have piezoelectricity piezoelectricity pottery silver strip.
The above is only preferred embodiment of the present invention, not imposes any restrictions technical scope of the present invention.The technician of the industry, under the inspiration of the technical program, some distortion and amendment can be made, every above embodiment is done according to technical spirit of the present invention any amendment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.

Claims (2)

1. reduce a technique for PZT piezoelectricity material powder calcining temperature, it is characterized in that: comprising:
Step 1, baking, batching, to the baking of used raw material, make the moisture content in absorption raw material discharge, and calculates required each raw material and weigh according to general formula;
Step 2, ball milling mixes, and makes its granularity reach≤1.5um, mixes, and obtains PZT piezoelectricity material powder;
Step 3, pre-molding, by described PZT piezoelectricity material powder briquetting, before compacting in described PZT piezoelectricity material powder, stir and add the water that its weight is described PZT piezoelectricity material powder 4 ~ 6%, and weight is the polyvinyl alcohol solution of described PZT piezoelectricity material powder 1 ~ 3%, concentration 4 ~ 6%, and weight is the dehydrated alcohol of described PZT piezoelectricity material powder 1 ~ 3%, pressure-controlling, at 6MPa ~ 8MPa, adopts impact briquetting mode;
Step 4, low temperature synthesizes, and is synthesized by the material block of pre-molding in tunnel stove in 850 DEG C ~ 950 DEG C calcinings;
Step 5, again ball milling, implement ball mill pulverizing to the material block synthesized through low temperature, cause granularity to reach≤0.09um;
Step 6, dry, by the moisture content vaporization in material, adopt electrothermal drying, put into baking oven baking, 140 DEG C ~ 160 DEG C, 20h ~ 25h;
Step 7, sieves, and by the material toasted, is down to normal temperature, crosses 200 mesh sieves; Be prepared into molding mass powder;
Step 8, shaping, add Vltra tears, glycerine, alcohol and water, mixing, roll off, old and extrusion molding in material powder;
Step 9, binder removal and sintering, in circulation tunnel stove, binder removal, sinter ceramic plate into, sintering temperature 1280 DEG C ~ 1300 DEG C;
Step 10, by electrode, by the silver slurry of required diameter, thickness 0.01mm in the ceramic plate two surface silk screen printing of preparation, in tunnel stove, 340 DEG C ~ 360 DEG C oven dry, load in square crucible, put into tunnel stove 775 DEG C ~ 785 DEG C silver ink firings, Temperature fall, to room temperature, is made by silver-colored ceramic plate;
Step 11, polarization, will be put into automatic tunnel polarization machine by silver-colored ceramic plate and be warmed up to 145 DEG C ~ 155 DEG C, 3kv/mm ~ 5kv/mm voltage polarizing 15 minutes to 25 minutes, make the piezoelectricity pottery silver strip with piezoelectricity.
2. a kind of technique reducing PZT piezoelectricity material powder calcining temperature according to claim 1, is characterized in that: described general formula is
0.02Pb(Sb 1/3.Nb 2/3)O 3- 0.47(Pb 0.7Sr 0.3)TiO 3- 0.51PbZrO 3
CN201410620605.0A 2014-11-07 2014-11-07 A kind of technique that reduces PZT piezoelectricity material powder calcining heat Active CN104446521B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1339829A (en) * 2000-08-18 2002-03-13 株式会社村田制作所 Piezo-electric ceramic material, sintered piezo-electric ceramic pressed block and piezo-electric ceramic device
CN1958509A (en) * 2006-11-27 2007-05-09 浙江嘉康电子股份有限公司 Modified PZT piezoelectric ceramics with Nano powder being added directly, and preparation method
CN1958510A (en) * 2006-11-27 2007-05-09 浙江嘉康电子股份有限公司 Modified PZT piezoelectric ceramics with Nano powder being added to preburning material, and preparation method
CN101570430A (en) * 2009-06-09 2009-11-04 武汉理工大学 Piezoceramic material for high-quality ignition device

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1339829A (en) * 2000-08-18 2002-03-13 株式会社村田制作所 Piezo-electric ceramic material, sintered piezo-electric ceramic pressed block and piezo-electric ceramic device
CN1958509A (en) * 2006-11-27 2007-05-09 浙江嘉康电子股份有限公司 Modified PZT piezoelectric ceramics with Nano powder being added directly, and preparation method
CN1958510A (en) * 2006-11-27 2007-05-09 浙江嘉康电子股份有限公司 Modified PZT piezoelectric ceramics with Nano powder being added to preburning material, and preparation method
CN101570430A (en) * 2009-06-09 2009-11-04 武汉理工大学 Piezoceramic material for high-quality ignition device

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Address after: 523000 Guangdong province Dongguan wangniudunzhen Newton Hengli Village Industrial Park

Patentee after: Guangdong wisdom intelligent Polytron Technologies Inc

Address before: 523000 Guangdong province Dongguan wangniudunzhen Newton Hengli Village Industrial Park

Patentee before: Dongguan Sweet Sound Electronics Co., Ltd.