CN103044033A - Method for preparing NaSbO3 powder for lead-free piezoelectric ceramics by adopting hydrothermal method - Google Patents
Method for preparing NaSbO3 powder for lead-free piezoelectric ceramics by adopting hydrothermal method Download PDFInfo
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- CN103044033A CN103044033A CN2012104996629A CN201210499662A CN103044033A CN 103044033 A CN103044033 A CN 103044033A CN 2012104996629 A CN2012104996629 A CN 2012104996629A CN 201210499662 A CN201210499662 A CN 201210499662A CN 103044033 A CN103044033 A CN 103044033A
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Abstract
The invention discloses a method for preparing NaSbO3 powder for lead-free piezoelectric ceramics by adopting a hydrothermal method. The method comprises the following steps of: (1) adding NaOH and Sb2O5 into H2O, and adding water so as to prepare liquid with the total volume of A ml, wherein the added quantity of the NaOH is 3-5 Ammol, and the added quantity of the Sb2O5 is 0.1-0.5 Ammol; (2) stirring to enable the liquid to be uniform, thereby obtaining precursor liquid for hydrothermal reaction; (3) setting the reaction temperature of a hydrothermal reaction temperature control instrument to be 200-230 DEG C and the reaction time to be 12-24 hours; and (4) after the reaction temperature is reduced to room temperature, taking out a reaction kettle, washing precipitates by using deionized water and anhydrous ethanol until the precipitates are neutral, and drying, thereby obtaining the powder. The method simultaneously has the advantages of simple device, low temperature, high efficiency, high reaction activity of prepared powder, and sintering temperature lower than that of powder prepared by traditional solid-phase sintering, thereby being simple in process, high in efficiency, low in energy consumption, low in cost, and environment-friendly.
Description
Technical field
The invention belongs to field of functional materials, relate to a kind of hydrothermal method and prepare NaSbO
3The method of lead-free piezoelectric ceramic powder.
Background technology
NaSbO
3It is a kind of widely used fine chemical product.It is mainly used in translucent enamel, pottery, glass material, picture tube glass bulb and electron tube industry as finings and discoloring agent.In the glass industry traditionally the finings of usefulness be arsenic oxide arsenoxide, the huge exploitation of arsenic oxide arsenoxide toxicity and purification have limitation, and for practitioner and environment protection certain impact are arranged also.Use NaSbO
3Replace after the arsenic oxide arsenoxide, these problems will be readily solved.Industrial preparation NaSbO
3Raw material be generally the needle antimony ore deposit, adopt chlorine or hydrogen peroxide as oxygenant, prepare NaSbO with the sodium hydroxide reaction simultaneously
3Because inevitably sneaked into nonferrous metal ion and other impurity in the raw material, the NaSbO that produces
3Also needing to carry out complicated removal of impurities processes.
In recent years, for potassium niobate sodium-based leadless piezoelectric ceramic, has larger electronegative Sb
5+To B position Nb
+Part replace the piezoelectric property can improve pottery.In pottery, introduce Sb
5+The method usual method be to use Sb
2O
5But there is the shortcoming that feed particles is thick, purity is not high in this method, and NaSbO
3Middle SbO
3 -Ion is compared to the Sb of oxide compound state
2O
5Higher reactive behavior is arranged, therefore adopt hydrothermal treatment consists with Sb
2O
5The oxide compound refining is NaSbO
3Join that to improve piezoelectric property in the potassium niobate sodium-based leadless piezoelectric ceramic be commonplace method.Therefore prepare high-purity N aSbO
3Has extremely important meaning.
Summary of the invention
The purpose of this invention is to provide a kind of hydrothermal method and prepare NaSbO
3The method of lead-free piezoelectric ceramic powder is to solve NaSbO
3Purity is low, the problem of complicated process of preparation.
For achieving the above object, the technical solution used in the present invention may further comprise the steps:
Step 1: with NaOH and Sb
2O
5Join H
2Among the O, wherein add water and be mixed with the solution that cumulative volume is 50mL, wherein the NaOH add-on is 3A～5Ammol, Sb
2O
5Add-on is 0.1A～0.5Ammol;
Step 2: the room temperature magnetic agitation, NaOH is dissolved fully, solution is mixed, get the precursor liquid of hydro-thermal reaction;
Step 3: the precursor liquid of step 2 gained is moved in the teflon-lined reactor, the control packing ratio is 70%, again polytetrafluoroethyllining lining is put into stainless steel cauldron, design temperature controller temperature of reaction is 200～230 ℃, and the reaction times is 12～24h;
Step 4: after the question response temperature is down to room temperature, reactor is taken out, use deionized water and absolute ethanol washing to neutrality, at 70 ℃ of lower freeze-day with constant temperature 2h, obtain powder.
The present invention further improves and is, the packing ratio of reactor is 70%.
The present invention further improves and is, hydrothermal temperature is 230 ℃, and the reaction times is 24h.
The present invention further improves and is, drying temperature is 70 ℃ in the step 4, and the time is 2h.
The present invention further improves and is A=50.
With respect to prior art, beneficial effect of the present invention is: adopt Sb
2O
5With NaOH be raw material, wherein sodium hydroxide is not only as reactant but also as mineralizer, hydrothermal temperature is low, reaction times is short, and synthetic nanometer grade powder purity is higher, good crystallinity, and reaction unit powder reactive behavior simple, efficient and preparation is high, sintering temperature is lower than the powder of traditional solid state sintering preparation, is that a kind of technique is simple, less energy-consumption, environmentally friendly preparation method with low cost.
Description of drawings
Fig. 1 is the NaSbO of the embodiment of the invention 3 preparations
3The XRD figure of powder;
Fig. 2 is the NaSbO of the embodiment of the invention 3 preparations
3The SEM figure of powder.
Embodiment
Step 1: with NaOH and Sb
2O
5Join H
2Among the O, wherein add water and be mixed with the solution that cumulative volume is 50mL, wherein the NaOH add-on is 150mmol, Sb
2O
5Add-on is 5mmol;
Step 2: the room temperature magnetic agitation, NaOH is dissolved fully, solution is mixed, get the precursor liquid of hydro-thermal reaction;
Step 3: the precursor liquid of step 2 gained is moved in the teflon-lined reactor, and the control packing ratio is 70%, again polytetrafluoroethyllining lining is put into stainless steel cauldron, and design temperature controller temperature of reaction is 200 ℃, and the reaction times is 12h;
Step 4: after the question response temperature is down to room temperature, reactor is taken out, use deionized water and absolute ethanol washing to neutrality throw out, at 70 ℃ of lower freeze-day with constant temperature 2h, obtain powder;
Embodiment 2
Step 1: with NaOH and Sb
2O
5Join H
2Among the O, wherein add water and be mixed with the solution that cumulative volume is 50mL, wherein NaOH concentration is 200mmol, Sb
2O
5Consumption is 15mmol;
Step 2: the room temperature magnetic agitation, NaOH is dissolved fully, solution is mixed, get the precursor liquid of hydro-thermal reaction;
Step 3: the precursor liquid of step 2 gained is moved in the teflon-lined reactor, and the control packing ratio is 70%, again polytetrafluoroethyllining lining is put into stainless steel cauldron, and design temperature controller temperature of reaction is 200 ℃, and the reaction times is 24h;
Step 4: after the question response temperature is down to room temperature, reactor is taken out, use deionized water and absolute ethanol washing to neutrality throw out, at 70 ℃ of lower freeze-day with constant temperature 2h, obtain powder;
Embodiment 3
Step 1: with NaOH and Sb
2O
5Join among the H2O, wherein add water and be mixed with the solution that cumulative volume is 50mL, wherein the NaOH add-on is 250mmol, Sb
2O
5Add-on is 25mmol;
Step 2: the room temperature magnetic agitation, NaOH is dissolved fully, solution is mixed, get the precursor liquid of hydro-thermal reaction;
Step 3: the precursor liquid of step 2 gained is moved in the teflon-lined reactor, is 70% with the water management packing ratio, again polytetrafluoroethyllining lining is put into stainless steel cauldron, and design temperature controller temperature of reaction is 230 ℃, and the reaction times is 24h;
Step 4: after the question response temperature is down to room temperature, reactor is taken out, use deionized water and absolute ethanol washing to neutrality throw out, at 70 ℃ of lower freeze-day with constant temperature 2h, obtain powder.
Phase with the powder of XRD determining embodiment 3 preparation forms structure, measures the microscopic appearance of powder with SEM, and its result therefrom as can be known, adopts hydrothermal method as shown in Figure 1 and Figure 2, can prepare NaSbO with this understanding
3Powder.
Hydrothermal method has prepared NaSbO
3Powder also is used for the Sb of potassium-sodium niobate lead-free piezoelectric ceramics doping vario-property
5+The introducing source.
The above only is one embodiment of the present invention, it or not whole or unique embodiment, the conversion of any equivalence that those of ordinary skills take the technology of the present invention bill by reading specification sheets of the present invention is claim of the present invention and contains.
Claims (5)
1. a hydrothermal method prepares NaSbO
3The method of lead-free piezoelectric ceramic powder is characterized in that: may further comprise the steps:
Step 1: with NaOH and Sb
2O
5Join among the H2O, wherein add water and be mixed with the solution that cumulative volume is AmL, wherein the NaOH add-on is 3A～5Ammol, Sb
2O
5Add-on is 0.1A～0.5Ammol;
Step 2: the room temperature magnetic agitation, NaOH is dissolved fully, solution is mixed, get the precursor liquid of hydro-thermal reaction;
Step 3: the precursor liquid of step 2 gained is moved in the teflon-lined reactor, again polytetrafluoroethyllining lining is put into stainless steel cauldron, design temperature controller temperature of reaction is 200～230 ℃, and the reaction times is 12～24h;
Step 4: after the question response temperature is down to room temperature, reactor is taken out, use deionized water and absolute ethanol washing to neutrality throw out, drying obtains powder.
2. a kind of hydrothermal method according to claim 1 prepares NaSbO
3The method of lead-free piezoelectric ceramic powder is characterized in that: the packing ratio of reactor is 70%.
3. a kind of hydrothermal method according to claim 1 prepares NaSbO
3The method of lead-free piezoelectric ceramic powder is characterized in that: hydrothermal temperature is 230 ℃, and the reaction times is 24h.
4. a kind of hydrothermal method according to claim 1 prepares NaSbO
3The method of lead-free piezoelectric ceramic powder is characterized in that: drying temperature is 70 ℃ in the step 4, and the time is 2h.
5. a kind of hydrothermal method according to claim 1 prepares NaSbO
3The method of lead-free piezoelectric ceramic powder is characterized in that: A=50.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110713383A (en) * | 2019-10-25 | 2020-01-21 | 四川大学 | Piezoelectric ceramic material and preparation method thereof |
| CN113461422A (en) * | 2021-08-03 | 2021-10-01 | 四川大学 | High-voltage anti-fatigue potassium-sodium niobate-based lead-free piezoelectric ceramic and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2012
- 2012-11-28 CN CN2012104996629A patent/CN103044033A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110713383A (en) * | 2019-10-25 | 2020-01-21 | 四川大学 | Piezoelectric ceramic material and preparation method thereof |
| CN110713383B (en) * | 2019-10-25 | 2020-07-31 | 四川大学 | Piezoelectric ceramic material and preparation method thereof |
| CN113461422A (en) * | 2021-08-03 | 2021-10-01 | 四川大学 | High-voltage anti-fatigue potassium-sodium niobate-based lead-free piezoelectric ceramic and preparation method thereof |
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Application publication date: 20130417 |