CN110316758A - It is a kind of that potassium-sodium niobate raw powder's production technology is prepared using microwave operational principle - Google Patents
It is a kind of that potassium-sodium niobate raw powder's production technology is prepared using microwave operational principle Download PDFInfo
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- CN110316758A CN110316758A CN201910741821.3A CN201910741821A CN110316758A CN 110316758 A CN110316758 A CN 110316758A CN 201910741821 A CN201910741821 A CN 201910741821A CN 110316758 A CN110316758 A CN 110316758A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01G33/00—Compounds of niobium
- C01G33/006—Compounds containing, besides niobium, two or more other elements, with the exception of oxygen or hydrogen
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses a kind of potassium sodium niobate ceramic powders, and mainly preparing raw material includes niobium pentaoxide, potassium oxide and sodium oxide molybdena.The present invention is efficiently combined by microwave material research-on-research station with high energy ball mill, and material powder is obtained KNN ceramic powder by calcining, ball milling, secondary clacining and secondary ball milling technique.Solve the problems, such as prepare the defective workmanship of KNN ceramic powder using conventional solid-state method or liquid phase method, and can obtain that component is uniform, crystallinity is high and average particle diameter size for 87 ~ 106nm high quality KNN ceramic powder.High quality KNN ceramic powder is calcined synthesis within half an hour and is obtained, have the characteristics that energy conservation with it is efficient, have very big potentiality in preparation precision leadless piezoelectric ceramics component, have broad application prospects.
Description
Technical field
The present invention relates to lead-free piezoelectric ceramic powder and its preparation fields, specially use microwave material research-on-research station system
A kind of method of standby potassium sodium niobate ceramic powder.
Background technique
Recent years, the states such as China, the U.S. and European Union or tissue have all been put into effect limitation heavy metal ion in succession and have been ceased with people
Cease the application in associated electrical ceramic components.Limitation especially to the lead and cadmium ion that destroy human or animal's nerve, display
Promotions of the people to environmental consciousness.However, all the time leaded solid solution is accounted for its excellent electric property and stability
According to absolute advantage and market, develops lead-free piezoceramic material and be faced with huge challenge.In lead-free piezoceramic material
Research in, by it is concerned by people be potassium sodium niobate ceramic (referred to as KNN ceramics), be on the one hand due to its residence with higher
In temperature so that its near room temperature have excellent thermal stability；On the other hand, it can be significantly improved by suitable technique
Its dielectric properties and piezoelectric property, to reach the electric property to match in excellence or beauty with leaded solid solution phase.
Currently, the preparation process of KNN ceramics generally requires higher sintering temperature and longer soaking time, thus can
Potassium in components system, sodium element volatilization is brought to increase so as to cause the defects of structure, electric property decline.In order to overcome system
The segregation of middle component and its electric property is promoted, when scientist uses many processes to reduce sintering temperature and heat preservation
Between, such as sintering aid and low temperature solid solution etc. is added.But the component of addition can often bring again different structure change with
Impurity phase, so that the electric property of ceramics cannot be promoted effectively.Therefore, in order to overcome the defect of process above or method, from
The source powder of the ceramics of preparation high quality sets about becoming the emphasis of research KNN ceramics at present.
The high quality powder that component is uniform, crystal property is good and particle diameter distribution is narrow and close to Nano grade is in sintering process
In can reduce sintering temperature, reduce fault of construction and promoted KNN ceramics dielectric and piezoelectric properties.Traditional solid reaction process
Phase structure of the long period and powder that need etc. is difficult to control；The process is more complicated is difficult to control for liquid phase method, and preceding
The phase cost of investment is excessively high, to be unfavorable for the industrialized production of KNN ceramic powder.It would therefore be highly desirable to which it is suitable to find one kind
Preparation process meets unleaded KNN ceramic powder to environmental protection and the requirements of energy-saving leadless piezoelectron ceramic components.
Summary of the invention
In order to overcome conventional solid-state method and liquid phase method to prepare the defect of unleaded KNN ceramic powder technique, the present invention provides one
It is primary raw material, using microwave material research-on-research station preparation high quality KNN that kind, which utilizes niobium pentaoxide, potassium oxide, sodium oxide molybdena,
The method of ceramic powder.
The purpose of the present invention is what is be achieved by the steps of:
A kind of KNN ceramic powder, main synthesis material include niobium pentaoxide, potassium oxide and sodium oxide molybdena；
The niobium pentaoxide: potassium oxide: the molal weight ratio of sodium oxide molybdena is 1:0.32 ~ 0.80:0.20 ~ 0.68；
A kind of KNN ceramic powder is uniformly mixed primary raw material by high energy ball mill, will be put after mixed powder tabletting
Enter in corundum crucible, by the calcining of microwave material research-on-research station, grinding, microwave material research-on-research station secondary clacining and secondary
Grinding obtains；The structure and object phase of powder are characterized by modern method for testing and analyzing.
A kind of KNN ceramic powder, the powder at being grouped as are as follows: K x Na(1−x)NbO3, whereinx=0.32~0.80；
A kind of KNN ceramic powder is prepared using microwave material research-on-research station, the specific process steps are as follows:
1) according to niobium pentaoxide: potassium oxide: sodium oxide molybdena molal weight ratio is the precise powder of 1:0.32 ~ 0.80:0.20 ~ 0.68
Body raw material；
2) lapping liquid 2 ~ 3 hours of ball milling in high energy ball mill again are added in the powder for weighing step 1), then 1 ~
The pressure sampling machine lower sheeting of 2MPa；
3) green body for obtaining step 2 is put into corundum crucible, is forged at 850 ~ 900 DEG C by microwave material research-on-research station
It burns 20 ~ 30 minutes；
4) green body calcined in step 3) is ground to obtain primary calcining KNN ceramic powder.
5) primary calcining KNN ceramic powder repetition step 2 and step 3) and step 4) that step 4) obtains are obtained secondary
KNN ceramic powder is calcined, final KNN ceramic powder is as prepared.
Positive beneficial effect: the present invention is efficiently combined by microwave material research-on-research station with high energy ball mill, by raw material
Powder obtains KNN ceramic powder by calcining, ball milling, secondary clacining and secondary ball milling technique.It solves using conventional solid-state method
Or liquid phase method prepares the defective workmanship problem of KNN ceramic powder, and can obtain that component is uniform, crystallinity is high and average particle diameter size
For the high quality KNN ceramic powder of 87 ~ 106nm.High quality KNN ceramic powder is calcined synthesis within half an hour and is obtained, and has section
There can be very big potentiality with efficient feature in preparing accurate leadless piezoelectric ceramics component, there is wide answer
Use prospect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of KNN ceramic nano-powder body prepared by the present invention.
Specific embodiment
Combined with specific embodiments below, the present invention will be further explained and explanation:
Embodiment 1
A kind of KNN ceramic powder, main synthesis material include niobium pentaoxide, potassium oxide and sodium oxide molybdena；
The niobium pentaoxide: potassium oxide: the molal weight ratio of sodium oxide molybdena is 1:0.52:0.48；
A kind of KNN ceramic powder is uniformly mixed primary raw material by high energy ball mill, will be put after mixed powder tabletting
Enter in corundum crucible, by the calcining of microwave material research-on-research station, grinding, microwave material research-on-research station secondary clacining and secondary
Grinding obtains；The structure and object phase of powder are characterized by modern method for testing and analyzing.
A kind of KNN ceramic powder, the powder at being grouped as are as follows: K x Na(1−x)NbO3, whereinx=0.32~0.80；
A kind of KNN ceramic powder is prepared using microwave material research-on-research station, the specific process steps are as follows:
1) according to niobium pentaoxide: potassium oxide: sodium oxide molybdena molal weight ratio is 1:0.52:0.48 precise powder material；
2) lapping liquid 2.5 hours of ball milling under high energy ball mill again are added in the powder for weighing step 1), then in 1MPa
Pressure sampling machine lower sheeting；
3) green body for obtaining step 2 is put into corundum crucible, calcines 25 points at 850 DEG C by microwave material research-on-research station
Clock；
4) green body calcined in step 3) is ground to obtain primary calcining KNN ceramic powder；
5) 4) the primary calcining KNN ceramic powder obtained is repeated into step 2 and step 3) and step 4) obtains secondary clacining KNN
Ceramic powder as prepares final KNN ceramic powder.
Embodiment 2
A kind of KNN ceramic powder, main synthesis material include niobium pentaoxide, potassium oxide and sodium oxide molybdena；
The niobium pentaoxide: potassium oxide: the molal weight ratio of sodium oxide molybdena is 1:0.40:0.60；
A kind of KNN ceramic powder is uniformly mixed primary raw material by high energy ball mill, will be put after mixed powder tabletting
Enter in corundum crucible, by the calcining of microwave material research-on-research station, grinding, microwave material research-on-research station secondary clacining and secondary
Grinding obtains；The structure and object phase of powder are characterized by modern method for testing and analyzing.
A kind of KNN ceramic powder, the powder at being grouped as are as follows: K x Na(1−x)NbO3, whereinx=0.32~0.80；
A kind of KNN ceramic powder is prepared using microwave material research-on-research station, the specific process steps are as follows:
1) according to niobium pentaoxide: potassium oxide: sodium oxide molybdena molal weight ratio is 1:0.40:0.60 precise powder material；
2) lapping liquid 3 hours of ball milling under high energy ball mill again are added in the powder for weighing step 1), then in 1.5MPa
Pressure sampling machine lower sheeting；
3) green body for obtaining step 2 is put into corundum crucible, calcines 20 points at 900 DEG C by microwave material research-on-research station
Clock；
4) green body calcined in step 3) is ground to obtain primary calcining KNN ceramic powder；
5) the primary calcining KNN ceramic powder that step 4) obtains is repeated into step 2 and step 3) and step 4) obtains secondary clacining
KNN ceramic powder as prepares final KNN ceramic powder.
Embodiment 3
Prepare K0.50Na0.50NbO3Ceramic powder: niobium pentaoxide 10.6324g, potassium oxide 1.8841g, oxidation sodium powder are taken respectively
Body 1.2402g material powder；It is mixed 3 hours through high energy ball mill, by mixed powder tabletting under the pressure sampling machine of 1.5MPa
It is placed in corundum crucible；Corundum crucible is placed in the cavity at microwave material research-on-research station, is forged at being 880 DEG C in temperature
It burns 23 minutes, then green body is crushed and obtains once calcining K0.50Na0.50NbO3Ceramic powder；Each to repeat the above steps
Part obtains secondary clacining K0.50Na0.50NbO3Ceramic powder.
K0.50Na0.50NbO3Ceramic powder particle has sharp-featured structure, it is shown that higher crystallinity；Average grain
Diameter is having a size of 94nm.
Embodiment 4
Prepare K0.60Na0.40NbO3Ceramic powder: niobium pentaoxide 10.6324g, potassium oxide 2.2609g, oxidation sodium powder are taken respectively
Body 0.9922g material powder；It is mixed 2.5 hours through high energy ball mill, by mixed powder tabletting under the pressure sampling machine of 2MPa
It is placed in corundum crucible；Corundum crucible is placed in the cavity at microwave material research-on-research station, is forged at being 900 DEG C in temperature
It burns 27 minutes, then green body is crushed and obtains once calcining K0.60Na0.40NbO3Ceramic powder；Each to repeat the above steps
Part obtains secondary clacining K0.60Na0.40NbO3Ceramic powder.
K0.60Na0.40NbO3Ceramic powder particle has sharp-featured structure, it is shown that higher crystallinity；Average grain
Diameter is having a size of 106nm.
Embodiment 5
Prepare K0.32Na0.68NbO3Ceramic powder: niobium pentaoxide 10.6324g, potassium oxide 1.2059g, oxidation sodium powder are taken respectively
Body 1.6867g material powder；Through high energy ball mill mix 3 hours, under the pressure sampling machine of 1MPa by mixed powder tabletting after
It is placed in corundum crucible；Corundum crucible is placed in the cavity at microwave material research-on-research station, is calcined at being 850 DEG C in temperature
20 minutes, then green body is crushed and obtains once calcining K0.32Na0.68NbO3Ceramic powder；The each condition to repeat the above steps,
Obtain secondary clacining K0.32Na0.68NbO3Ceramic powder.
K0.32Na0.68NbO3Ceramic powder particle has sharp-featured structure, it is shown that higher crystallinity；Average grain
Diameter is having a size of 87nm.
Embodiment 6
Prepare K0.75Na0.25NbO3Ceramic powder: niobium pentaoxide 10.6324g, potassium oxide 2.8262g, oxidation sodium powder are taken respectively
Body 0.6201g material powder；It is mixed 2.5 hours through high energy ball mill, by mixed powder pressure under the pressure sampling machine of 1.5MPa
Piece is placed in corundum crucible；Corundum crucible is placed in the cavity at microwave material research-on-research station, in the case where temperature is 870 DEG C
Green body is then crushed and obtains once calcining K by calcining 25 minutes0.75Na0.25NbO3Ceramic powder；What is repeated the above steps is each
Condition obtains secondary clacining K0.75Na0.25NbO3Ceramic powder.
K0.75Na0.25NbO3Ceramic powder particle has sharp-featured structure, it is shown that higher crystallinity；Average grain
Diameter is having a size of 102nm.
Embodiment 7
Prepare K0.45Na0.55NbO3Ceramic powder: niobium pentaoxide 10.6324g, potassium oxide 1.6957g, oxidation sodium powder are taken respectively
Body 1.3642g material powder；Through high energy ball mill mix 2 hours, under the pressure sampling machine of 2MPa by mixed powder tabletting after
It is placed in corundum crucible；Corundum crucible is placed in the cavity at microwave material research-on-research station, is calcined at being 890 DEG C in temperature
19 minutes, then green body is crushed and obtains once calcining K0.45Na0.55NbO3Ceramic powder；The each condition to repeat the above steps,
Obtain secondary clacining K0.45Na0.55NbO3Ceramic powder.
K0.45Na0.55NbO3Ceramic powder particle has sharp-featured structure, it is shown that higher crystallinity；Average grain
Diameter is having a size of 98nm.
The present invention is efficiently combined by microwave material research-on-research station with high energy ball mill, material powder process is calcined,
Ball milling, secondary clacining and secondary ball milling technique obtain KNN ceramic powder.It solves and is prepared using conventional solid-state method or liquid phase method
The defective workmanship problem of KNN ceramic powder, and can obtain that component is uniform, crystallinity is high and average particle diameter size is 87 ~ 106nm's
High quality KNN ceramic powder.High quality KNN ceramic powder is calcined synthesis within half an hour and is obtained, and has energy saving and efficient spy
Point has very big potentiality in preparing accurate leadless piezoelectric ceramics component, has broad application prospects.
Above embodiments are merely to illustrate the preferred embodiment of the present invention, but the present invention is not limited to above-mentioned embodiment party
Formula, the field those of ordinary skill within the scope of knowledge, it is made any within the spirit and principles in the present invention
Modification, equivalent substitute and improvement etc. should all be covered within the claimed technical proposal scope of the present invention.
Claims (5)
1. a kind of KNN ceramic powder, it is characterised in that: its main synthesis material includes niobium pentaoxide, potassium oxide and sodium oxide molybdena.
2. KNN ceramic powder according to claim 1, it is characterised in that: the niobium pentaoxide: potassium oxide: oxygen
The molal weight ratio for changing sodium is 1:0.32 ~ 0.80:0.20 ~ 0.68.
3. a kind of KNN ceramic powder described in is uniformly mixed primary raw material by high energy ball mill, after mixed powder tabletting
It is put into corundum crucible, by the calcining of microwave material research-on-research station, grinding, microwave material research-on-research station secondary clacining and two
Secondary grinding obtains；The structure and object phase of powder are characterized by modern method for testing and analyzing.
4. KNN ceramic powder according to claim 1, it is characterised in that: its powder at being grouped into available chemical formula
K x Na(1−x)NbO3It indicates, whereinx=0.32~0.80。
5. a kind of preparation method of KNN ceramic powder as described in right 1-4 Arbitrary Term, it is characterised in that: use microwave material
The preparation of research-on-research station, the specific process steps are as follows:
1) according to niobium pentaoxide: potassium oxide: sodium oxide molybdena molal weight ratio is the precise powder of 1:0.32 ~ 0.80:0.20 ~ 0.68
Body raw material；
2) lapping liquid 2 ~ 3 hours of ball milling under high energy ball mill again are added in the powder for weighing step 1), then 1 ~
The pressure sampling machine lower sheeting of 2MPa；
3) green body for obtaining step 2 is put into corundum crucible, is forged at 850 ~ 900 DEG C by microwave material research-on-research station
It burns 20 ~ 30 minutes；
4) green body calcined in step 3) is ground to obtain primary calcining KNN ceramic powder；
5) the primary calcining KNN ceramic powder that step 4) obtains is repeated into step 2 and step 3) and step 4) obtains secondary clacining
KNN ceramic powder as prepares final KNN ceramic powder.
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| CN103588480A (en) * | 2013-11-19 | 2014-02-19 | 南昌航空大学 | Preparation method of secondary microwave sintering high-performance submicron zirconium oxide based tooth |
| CN104051606A (en) * | 2014-06-09 | 2014-09-17 | 北京派和科技股份有限公司 | Potassium niobate sodium-based multi-layer piezoelectric ceramic element and preparing method thereof |
| DE102013226715A1 (en) * | 2013-12-19 | 2015-06-25 | Robert Bosch Gmbh | Method for joining piezoceramic layers |
| CN106242568A (en) * | 2016-07-22 | 2016-12-21 | 郑州大学 | A kind of microwave synthesis method of potassium-sodium niobate leadless piezoelectric ceramic |
| CN108863360A (en) * | 2018-07-27 | 2018-11-23 | 福州大学 | A kind of preparation method of Er ions potassium-sodium niobate-strontium titanates crystalline ceramics |
-
2019
- 2019-08-12 CN CN201910741821.3A patent/CN110316758A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588480A (en) * | 2013-11-19 | 2014-02-19 | 南昌航空大学 | Preparation method of secondary microwave sintering high-performance submicron zirconium oxide based tooth |
| DE102013226715A1 (en) * | 2013-12-19 | 2015-06-25 | Robert Bosch Gmbh | Method for joining piezoceramic layers |
| CN104051606A (en) * | 2014-06-09 | 2014-09-17 | 北京派和科技股份有限公司 | Potassium niobate sodium-based multi-layer piezoelectric ceramic element and preparing method thereof |
| CN106242568A (en) * | 2016-07-22 | 2016-12-21 | 郑州大学 | A kind of microwave synthesis method of potassium-sodium niobate leadless piezoelectric ceramic |
| CN108863360A (en) * | 2018-07-27 | 2018-11-23 | 福州大学 | A kind of preparation method of Er ions potassium-sodium niobate-strontium titanates crystalline ceramics |
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Application publication date: 20191011 |