CN109020499A - A kind of preparation process of high performance piezoelectric ceramics - Google Patents
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Abstract
The invention discloses a kind of preparation processes of high performance piezoelectric ceramics, include the following steps: 1) pressure electroceramics raw material；2) piezoelectric ceramics raw material loading ball grinder is sufficiently mixed ball milling, the slurry obtained after ball milling is placed in drying box and is dried, powder is obtained；3) water is added to powder, adds one of ammonium hydroxide, citric acid or oxalic acid or any several composition, then heating carries out hydro-thermal process, and the powder drying after hydro-thermal process obtains piezoelectric ceramics material powder；4) piezoelectric ceramics material powder made from step 3) is handled using the treatment process of conventional piezoelectric ceramics, obtains high performance piezoelectric ceramics.The present invention has piezoelectric ceramics performance obtained good, and raw material dosage is few, at low cost, and pollution is small, and technique is simpler, the good feature of technology stability.
Description
Technical field
The present invention relates to a kind of processing method of ceramics doping material, especially a kind of preparation works of high performance piezoelectric ceramics
Skill.
Background technique
Piezoelectric ceramics is a kind of informational function ceramic material that can convert mutually mechanical energy and electric energy.Piezoelectric ceramics benefit
With its material under mechanical stress effect, causes the relative displacement of internal positive and negative charge center and polarize, lead to material ends
There is the opposite bound charge of symbol i.e. piezoelectric effect and makes in surface, and has sensitive characteristic, and piezoelectric ceramics is mainly used for making
Ultrasonic transducer, underwater acoustic transducer, electroacoustic transducer, ceramic filter, ceramic transformer, ceramic discriminator, high pressure is made to occur
Device, infrared detector, SAW device, electro-optical device, ignition and blasting device and piezolectric gyroscope etc., in addition to being led for high-tech
Domain, it is more to service in daily life for people, the effort for people's creation more good days.
The granularity of piezoelectric ceramics raw material is substantially at several microns to tens microns.How the element of each component to be evenly spread to
It is the key factor for improving voltage-sensitive ceramic performance in ceramics.
Now currently, usually being handled raw material using ball-milling method, but ball milling in the actual production process of piezoelectric ceramics
Method be only capable of for raw material being milled to 1 microns, although the requirements of most of applications are met, some high-end
Under application, the requirement of client is also not achieved using the performance of the ceramics of these raw materials.Recent years has using chemical coprecipitation
The means such as shallow lake, dissolution-gel method, freeze-drying synthesize ultra-fine feed stock oxide, to promote the performance of ceramics.But
Still ideal effect is not obtained.And hydro-thermal method is method new for one kind of ceramic raw material processing at present, it can be into one
Step improves the treatment effect of raw material.But now current hydro-thermal method still has defect, is mainly reflected in: 1, now current water
Thermal method must be raw material using the soluble-salt (predominantly nitrate) of raw material, reacted with alkali, oxide is finally made, but
The price of soluble-salt is much more expensive than oxide, increases the cost of material of ceramics；2, the soluble-salt of raw material is most
The amount of oxide made from end is that the sub-fraction of the amount of soluble-salt (is hydrated nitre with the soluble nitrate-five of zirconium oxide
For sour zirconium, zirconium dioxide is 29% after the completion of processing, remaining 71% is nitrate anion and the crystallization water), therefore, when preparing oxide
It needs a large amount of soluble-salt and alkali to be reacted, further increases the cost of material of ceramics, meanwhile, containing a large amount of in waste liquid
Acid group, environmental pollution is larger；3, the reaction system of soluble-salt and alkali is more complicated, and condition is harsher, treatment process
In technique the more difficult assurance of stability.
Summary of the invention
The object of the present invention is to provide a kind of preparation processes of high performance piezoelectric ceramics.The present invention has pressure obtained
Electroceramics performance is good, and raw material dosage is few, at low cost, and pollution is small, and technique is simpler, the good feature of technology stability.
Technical solution of the present invention: a kind of preparation process of high performance piezoelectric ceramics includes the following steps:
1) Pb is taken3O4、TiO2、ZrO2、Nb2O5It is mixed with NiO, obtains piezoelectric ceramics raw material；
2) piezoelectric ceramics raw material is packed into ball grinder, is added after alcohol and raw material is sufficiently mixed ball milling, will be obtained after ball milling
Slurry be placed in drying box and dry, obtain powder；
3) water is added to powder, adds one of ammonium hydroxide, citric acid or oxalic acid or any several composition, then
Heating carries out hydro-thermal process, and the powder after hydro-thermal process is dried in drying box, obtains piezoelectric ceramics material powder；
4) piezoelectric ceramics material powder made from step 3) is handled using the treatment process of conventional piezoelectric ceramics, obtains high property
It can piezoelectric ceramics.
The preparation process of high performance piezoelectric ceramics above-mentioned, in step 2), the slurry is the drying box at 60-120 DEG C
Middle drying.
The preparation process of high performance piezoelectric ceramics above-mentioned, the slurry are dried in 70 DEG C of drying box.
The preparation process of high performance piezoelectric ceramics above-mentioned, in step 3), in the reaction system of the hydro-thermal process, ammonia
The concentration of one of water, citric acid or oxalic acid or any several composition is 0.5-2mol/L.
The preparation process of high performance piezoelectric ceramics above-mentioned, in the reaction system of the hydro-thermal process, ammonium hydroxide, citric acid or
The concentration of one of oxalic acid or any several composition is 1mol/L.
The preparation process of high performance piezoelectric ceramics above-mentioned, in step 3), the treatment temperature of the hydro-thermal process is 200-
400℃；The processing time of the hydro-thermal process is 5-25h.
The preparation process of high performance piezoelectric ceramics above-mentioned, the treatment temperature of the hydro-thermal process are 300 DEG C；The hydro-thermal
The processing time of processing is 15h.
The preparation process of high performance piezoelectric ceramics above-mentioned, in step 3), the powder after the hydro-thermal process is in 60-80
DEG C drying box in dry.
The preparation process of high performance piezoelectric ceramics above-mentioned, the powder after the hydro-thermal process is in 70 DEG C of drying box
Drying.
Beneficial effects of the present invention
1, the present invention handles material powder by improved hydro-thermal treatment method, and powder obtained is more evenly distributed, powder
Partial size is smaller, particle size distribution is narrower, specific surface area is more, activity is stronger, and the performance of piezoelectric ceramics obtained is more preferable.
2, the present invention using oxide as raw material by directly being handled, with use soluble-salt as raw material phase
Than cost of material can be greatly reduced；Simultaneously as being directly to be handled oxide to obtain oxide, almost
There is no the loss of raw material, but how many amounts needed just to be handled with how many raw material, greatly reduces the dosage of material,
It further reduces costs；In addition, inorganic agent dosage is few in treatment process of the present invention, the waste liquid of generation is few, greatly reduces pair
The pollution level of environment；In addition, the present invention is directly handled using oxide, technique is simpler, and the stability of technique is more
It is good.
To further illustrate beneficial effects of the present invention, applicant devises following experiment:
Experimental example
1, experimental method: this experimental example is arranged four groups of experiments altogether, first group of piezoelectric ceramic piece for traditional handicraft preparation, the
Two groups of piezoelectric ceramic pieces prepared for the embodiment of the present invention 1, third group are piezoelectric ceramic piece prepared by the embodiment of the present invention 2, the
Four groups of piezoelectric ceramic pieces prepared for the embodiment of the present invention 3, respectively to the piezoelectric constant of four groups of potsherds, dielectric constant, dielectric
Loss, electromechanical coupling factor, Curie temperature measure.
Experimental result: table 1 is four groups of potsherd experimental data contrast tables, as can be seen from Table 1: being implemented through the present invention
The piezoelectric constant of the piezoelectric ceramic piece of example the method processing improves 10%, and dielectric constant improves 20%, and dielectric loss omits
Micro- consumption reduces, and Curie temperature is increased to 137 DEG C or so.Illustrate that the performance of piezoelectric ceramics produced by the present invention has obtained greatly
While raising, it is also greatly reduced ceramic cost, reduce environmental pollution and ensure that technology stability.
1: four group of potsherd experimental data contrast table of table
Detailed description of the invention
Attached drawing 1 is the granularity cumulative distribution table of the ceramic powder of conventional solid-state method and hydro-thermal method of the present invention preparation；
Attached drawing 2 is the scanning electron microscope (SEM) photograph of the ceramic powder of conventional solid-state method preparation；
Attached drawing 3 is the scanning electron microscope (SEM) photograph of the ceramic powder of hydro-thermal method of the present invention preparation.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
The embodiment of the present invention
Embodiment 1: a kind of preparation process of high performance piezoelectric ceramics, steps are as follows:
1) Pb by mass percentage, is taken3O465%, TiO210%, ZrO25%, Nb2O515% and NiO 5% is mixed
It closes, obtains piezoelectric ceramics raw material；
2) piezoelectric ceramics raw material is packed into ball grinder, is added after alcohol and raw material is sufficiently mixed ball milling, will be obtained after ball milling
Slurry be placed on and dried in 70 DEG C of drying box, obtain powder；
3) water is added to powder, adds ammonium hydroxide, then heating progress hydro-thermal process, in the reaction system of hydro-thermal process,
The concentration of ammonium hydroxide is 1mol/L, and the treatment temperature of hydro-thermal process is 300 DEG C, and the processing time of hydro-thermal process is 15h, hydro-thermal process
Powder afterwards is dried in 70 DEG C of drying box, obtains piezoelectric ceramics material powder；
4) 300g deionized water is added into piezoelectric ceramics material powder made from 1kg step 3), adding concentration is
10% polyvinyl alcohol 550g, dispersing agent dispersing agent 8g, defoaming agent 4g, tape casting after ball milling mixing 2 hours are quiet by lamination etc.
Then pressure, punching, dumping, sintering, surface metalation, polarization process obtain high performance piezoelectric ceramics.
Embodiment 2: a kind of preparation process of high performance piezoelectric ceramics, steps are as follows:
1) Pb by mass percentage, is taken3O465%, TiO210%, ZrO25%, Nb2O515% and NiO 5% is mixed
It closes, obtains piezoelectric ceramics raw material；
2) piezoelectric ceramics raw material is packed into ball grinder, is added after alcohol and raw material is sufficiently mixed ball milling, will be obtained after ball milling
Slurry be placed on and dried in 60 DEG C of drying box, obtain powder；
3) water is added to powder, adds citric acid, then heating progress hydro-thermal process, in the reaction system of hydro-thermal process
The concentration of citric acid is 0.5mol/L, and the treatment temperature of hydro-thermal process is 200 DEG C, and the processing time of hydro-thermal process is 25h, hydro-thermal
Treated, and powder is dried in 60 DEG C of drying box, obtains piezoelectric ceramics material powder；
4) 250g deionized water is added into piezoelectric ceramics material powder made from 1kg step 3), adding concentration is
10% polyvinyl alcohol 500g, dispersing agent dispersing agent 6g, defoaming agent 2g, tape casting after ball milling mixing 1 hour are quiet by lamination etc.
Then pressure, punching, dumping, sintering, surface metalation, polarization process obtain high performance piezoelectric ceramics.
Embodiment 3: a kind of preparation process of high performance piezoelectric ceramics, steps are as follows:
1) Pb by mass percentage, is taken3O465%, TiO210%, ZrO25%, Nb2O515% and NiO 5% is mixed
It closes, obtains piezoelectric ceramics raw material；
2) piezoelectric ceramics raw material is packed into ball grinder, is added after alcohol and raw material is sufficiently mixed ball milling, will be obtained after ball milling
Slurry be placed on and dried in 120 DEG C of drying box, obtain powder；
3) water is added to powder, adds oxalic acid, then heating progress hydro-thermal process, in the reaction system of hydro-thermal process,
The concentration of oxalic acid is 2mol/L, and the treatment temperature of hydro-thermal process is 400 DEG C, and the processing time of hydro-thermal process is 5h, hydro-thermal process
Powder afterwards is dried in 80 DEG C of drying box, obtains piezoelectric ceramics material powder；
4) 350g deionized water is added into piezoelectric ceramics material powder made from 1kg step 3), adding concentration is
10% polyvinyl alcohol 600g, dispersing agent dispersing agent 10g, defoaming agent 6g, tape casting after ball milling mixing 3 hours, by lamination etc.
Then static pressure, punching, dumping, sintering, surface metalation, polarization process obtain high performance piezoelectric ceramics.
Claims (9)
1. a kind of preparation process of high performance piezoelectric ceramics, which comprises the steps of:
1) Pb is taken3O4、TiO2、ZrO2、Nb2O5It is mixed with NiO, obtains piezoelectric ceramics raw material；
2) piezoelectric ceramics raw material is packed into ball grinder, is added after alcohol and raw material is sufficiently mixed ball milling, the slurry that will be obtained after ball milling
Material, which is placed in drying box, dries, and obtains powder；
3) water is added to powder, adds one of ammonium hydroxide, citric acid or oxalic acid or any several composition, then heats
Hydro-thermal process is carried out, the powder after hydro-thermal process is dried in drying box, obtains piezoelectric ceramics material powder；
4) piezoelectric ceramics material powder made from step 3) is handled using the treatment process of conventional piezoelectric ceramics, obtains high-performance pressure
Electroceramics.
2. the preparation process of high performance piezoelectric ceramics according to claim 1, it is characterised in that: in step 2), the slurry
Material is dried in 60-120 DEG C of drying box.
3. the preparation process of high performance piezoelectric ceramics according to claim 2, it is characterised in that: the slurry is at 70 DEG C
Drying box in dry.
4. the preparation process of high performance piezoelectric ceramics according to claim 1, it is characterised in that: in step 3), the water
In the reaction system of heat treatment, the concentration of one of ammonium hydroxide, citric acid or oxalic acid or any several composition is 0.5-
2mol/L。
5. the preparation process of high performance piezoelectric ceramics according to claim 4, it is characterised in that: the hydro-thermal process it is anti-
It answers in system, the concentration of one of ammonium hydroxide, citric acid or oxalic acid or any several composition is 1mol/L.
6. the preparation process of high performance piezoelectric ceramics according to claim 1, it is characterised in that: in step 3), the water
The treatment temperature of heat treatment is 200-400 DEG C；The processing time of the hydro-thermal process is 5-25h.
7. the preparation process of high performance piezoelectric ceramics according to claim 6, it is characterised in that: the place of the hydro-thermal process
Managing temperature is 300 DEG C；The processing time of the hydro-thermal process is 15h.
8. the preparation process of high performance piezoelectric ceramics according to claim 1, it is characterised in that: in step 3), the water
Powder after heat treatment is dried in 60-80 DEG C of drying box.
9. the preparation process of high performance piezoelectric ceramics according to claim 8, it is characterised in that: after the hydro-thermal process
Powder is dried in 70 DEG C of drying box.
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| CN101607823A (en) * | 2009-07-09 | 2009-12-23 | 南京航空航天大学 | A kind of hydrothermal high-temperature mixed synthetic method of piezoelectric ceramic powder |
| US20150364674A1 (en) * | 2013-02-26 | 2015-12-17 | Fujifilm Corporation | Oxide particles, piezoelectric element, and method for producing oxide particles |
| JP6414818B2 (en) * | 2015-02-24 | 2018-10-31 | 神島化学工業株式会社 | Nano composite oxide and method for producing the same |
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