CN109650443A - A kind of preparation method of the potassium sodium niobate film of height preferred orientation - Google Patents
A kind of preparation method of the potassium sodium niobate film of height preferred orientation Download PDFInfo
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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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Abstract
The present invention discloses a kind of preparation method of the potassium sodium niobate film of height preferred orientation, this method step are as follows: weighs niobium oxide and is dissolved in hydrofluoric acid and obtains NbF5Ammonium oxalate is then added as stabilizer in solution, and alkalinity PH is finally added dropwise and debugs agent, obtains white precipitate Nb (OH)5；Washing filtering is carried out to white precipitate, citric acid, which is added, makes it obtain citric acid niobium in generation complex reaction, is then further filtered to citric acid niobium again；Sylvite and sodium salt powder is added, adds a certain amount of ethylene glycol, solution left standstill is finally obtained into uniform clear KNN precursor solution；Then it spin coating precursor solution and is made annealing treatment in the silicon base Jing Guo the pre-heat treatment, repeatedly spin coating anneals to obtain ideal KNN film.Non- alkoxide process of the present invention by improving sol-gel method and processing to silicon substrate, prepare the good KNN film of crystallinity on common (100) Si substrate, and obtained KNN film be (001) crystal orientation height preferentially.
Description
Technical field
The present invention relates to a kind of preparation methods of the potassium sodium niobate film of height preferred orientation, belong to piezoelectric material technology neck
Domain.
Background technique
Piezoelectric material is a kind of important functional material, and the functional characteristic that it has is in electronic technology, sensor, energy storage
It deposits and is widely used with driver etc..With grinding for MEMS (Micro Electro Mechanical Systems)
Study carefully development, piezoelectricity function element miniaturization and micromation and in terms of propose requirement.It is compared to block pressure
Electric material, piezoelectric membrane is easy to process, degree of regulation is high, light weight, driving voltage are low and can be excellent in terms of Planar integration
Point is more able to satisfy requirement of the MEMS to piezoelectricity functional material.
There are mainly four types of the methods for producing KNN system film, sputtering method, sol-gal process, chemical vapour deposition technique and pulse
Laser deposition, relative to other methods, sol-gal process: it is required that equipment is simple, and it is at low cost, large area film can be prepared.It is molten
Sol-gel preparation KNN system film is distinguished by raw material is subdivided into metal alkoxide method and non-alkoxide process.Metal alkoxide method is produced
The material ethyl alcohol niobium relative price of KNN system film is expensive, constrains the demand of volume production.It is cheap that non-alkoxide method prepares material price,
The cost of material can be substantially reduced.However, the thin-film material crystal that general non-alkoxide legal system takes is mostly polycrystalline, and KNN film with
Silicon substrate poor adhesion needs to carry out plating SiO to silicon substrate2Layer, preparation cost are high.
Summary of the invention
Goal of the invention: being that polycrystalline, KNN film and silicon serve as a contrast for crystal existing for existing non-alkoxide method preparation KNN system film
The problems such as bottom poor adhesion, the present invention provide a kind of preparation method of the potassium sodium niobate film of height preferred orientation.
Technical solution: a kind of preparation method of the potassium sodium niobate film of height preferred orientation of the present invention, including such as
Lower step:
(1) it weighs niobium oxide and is dissolved in hydrofluoric acid and obtain NbF5Solution, to NbF5Ammonium oxalate is first added in solution, it is molten to its
Alkalinity PH is added dropwise after solution and debugs agent, obtains white precipitate Nb (OH)5, Nb (OH) is washed with deionized5It precipitates and filters；
(2) by filtered Nb (OH)5It is mixed and added into deionized water with citric acid, and is stirred to clarify；
(3) clear solution obtained by step (2) is filtered, obtains clear filtering solution；
(4) sylvite and sodium salt is first added into filtering solution obtained by step (3), adjusts pH value after its dissolution, second is added
Glycol stands, obtains the potassium-sodium niobate precursor solution of clear；
(5) the pre-heat treatment is carried out to silicon wafer substrate, then potassium-sodium niobate forerunner described in spin coating in silicon base after preheat
Liquid solution obtains to surface and is covered with the silicon wafer of wet film, be put into vacuum oven and keep the temperature, then make annealing treatment, obtains potassium-sodium niobate
Film.
In above-mentioned steps (1), it is preferred that will niobium oxide be added hydrofluoric acid in, under 60~90 DEG C of water bath conditions heat 7~
12h makes it dissolve, and ammonium oxalate is then added, and continues the heating under water bath condition until ammonium oxalate dissolves.Preferably in 80 DEG C of water-baths
Under the conditions of elder generation heating stirring 10h be dissolved in niobium oxide in hydrofluoric acid, then proceed under 80 DEG C of water bath conditions heating stirring 1h,
Dissolve ammonium oxalate.Wherein, the dosage of niobium oxide and hydrofluoric acid preferably meets following ratio: dissolving 1g in the hydrofluoric acid of every 5mL
Niobium oxide.
Further, in step (1), it is 9 that ammonium hydroxide, which is added dropwise, and adjusts solution pH value, obtains white precipitate Nb (OH)5, by gained
White precipitate Nb (OH)5In 60 DEG C of 0.5~2h of ageing.When washing, it is generally available deionized water washing Nb (OH)5Precipitating 2~4 times
And it filters.
In step (3), citric acid and Nb (OH)5Molar ratio be preferably 3:1.
In step (4), the molar ratio of niobium element in filtering solution obtained by the potassium acetate and sodium acetate of addition and step (3)
(Nb5+):n(K+):n(Na+) it is preferably 2:1.1:1.1.Mole of citric acid additive amount in the additional amount of ethylene glycol and step (3)
Than being preferably 2:1.Wherein, the amount of niobium element can be calculated by following methods in filtering solution obtained by step (3): taking quality is m1
The step of (3) obtained by filtering solution, be put into calcination 1h in 900 DEG C of stove, obtain quality be m2White powder, calculate niobium
ConcentrationUnit is g/mol.
Preferably, carrying out the pre-heat treatment in step (5) to silicon wafer substrate and referring to silicon wafer substrate at 550 DEG C or more
At a temperature of preheat 10min, preferably in 600 DEG C of preheating 10min.Further, spincoating conditions are as follows: revolving speed 3500r/min, time
30s；The silicon wafer that surface can be covered with to wet film after spin coating keeps the temperature 6min in 150~250 DEG C of vacuum oven.
Further, it is the potassium sodium niobate film for obtaining ideal thickness, can be repeatedly revolved in silicon wafer substrate after preheat
It applies potassium-sodium niobate precursor solution and prepares potassium niobate thin film, made annealing treatment by the way of annealing layer by layer, i.e., every spin coating one
Secondary, annealing is primary, repeatedly, until obtaining ideal film thickness；The condition of annealing are as follows: at 650~850 DEG C
At a temperature of anneal 10min, annealing temperature is preferably 850 DEG C.It is typically repeated annealing 5~10 times preferably.
The utility model has the advantages that compared with the prior art, the advantages of the present invention are as follows: (1) method of the invention passes through to low cost
Non- alkoxide process improve, on the basis of non-alkoxide process, increase Nb (OH)5With acquired solution after citric acid hybrid reaction
The step of carrying out washing filtering, final obtained KNN system crystalline property is good, (001) crystal orientation height preferentially, relative to
Polycrystalline potassium sodium niobate film material, the KNN system film of (001) height preferred orientation are simple with higher quality characteristic and more
Structure-activity relationship, the more conducively Effective Regulation of performance；(2) this method is thin by improving KNN to the processing of silicon substrate high temperature preheating
The adhesiveness of film and silicon substrate solves the problems, such as KNN precursor liquid in silicon substrate poor adhesion, while reducing silicon substrate bottom
The cost of reason.
Detailed description of the invention
Fig. 1 is the XRD diagram of the KNN film of embodiment 1 (100) produced preferentially；
Fig. 2 is the comparison for the XRD diagram that embodiment 1 and comparative example produce KNN film；
Fig. 3 is the XRD diagram for producing KNN film in embodiment 2 under different pyrolysis temperatures；
Fig. 4 is the XRD diagram for producing KNN film in embodiment 3 under different annealing temperature.
Specific embodiment
Technical solution of the present invention is described further with reference to the accompanying drawing.
Embodiment 1
1) Nb of quality 5g is weighed with electronic balance2O5, 25ml hydrofluoric acid is added to it, the concentration of hydrofluoric acid is 40wt%,
Mixed liquor is heated to 10h to make it dissolve in 80 DEG C of water bath with thermostatic control, obtains clear solution.
2) stabilizer of the ammonium oxalate of 7g or so as niobium source is added dropwise to the clear solution 1) obtained, and continues in 80 DEG C of water
Bathe heating stirring 1h.
3) ammonium hydroxide is added dropwise to the clear solution 2) obtained and adjusts its PH to 9, determine the Nb (OH) for generating white5Precipitating, and
By the turbid solution containing precipitating in 60 DEG C of standing 2h.
4) the white Nb (OH) for filtering and 3) obtaining is washed repeatedly with deionized water5Then precipitating presses Nb (OH)5With citric acid
Molar ratio is 1:3 by citric acid and Nb (OH)5Mixing, and deionized water is added persistently stirs and dissolve it in volume for 24 hours and be
The reagent bottle of 60ml, obtains clear solution.
5) 4) clear solution obtained is filtered with filtering flask, and obtains clear filtering solution.
6) it takes a small amount of solution (quality m1) 5) obtained to be sintered at 900 DEG C, obtains white powder (quality m2),
And press formulaCalculate solution concentration, unit g/mol.
7) to the solution 5) obtained (Nb in molar ratio5+):n(K+):n(Na+Potassium acetate and second is added in)=2:1.1:1.1
Sour sodium powder end is simultaneously stirred continuously 2h, and it is 6 to 7 or so that ammonium hydroxide, which is then added dropwise, and adjusts its PH, and ethylene glycol is then added dropwise in molar ratio, and
It stands for 24 hours.
8) silicon substrate of (100) orientation is washed and preheats 10min in 600 DEG C of stove.
9) the KNN precursor liquid 7) obtained is added dropwise on silicon substrate after preheat, and is revolved in revolving speed 3500r/min spin coater
It applies 30s and obtains wet film, then the vacuum oven by wet film at 150 DEG C keeps the temperature 6min, finally the 10min in 850 DEG C of stove
It is crystallized, every spin coating is primary, just carries out annealing primary.It repeats spin coating 5 times, obtains desired film thickness.
Comparative example
1) Nb of quality 5g is weighed with electronic balance2O5, 25ml hydrofluoric acid is added to it, the concentration of hydrofluoric acid is 40wt%,
Mixed liquor is heated to 10h to make it dissolve in 80 DEG C of water bath with thermostatic control, obtains clear solution.
2) stabilizer of the ammonium oxalate of 7g or so as niobium source is added dropwise to the clear solution 1) obtained, and continues in 80 DEG C of water
Bath heating 1h.
3) ammonium hydroxide is added dropwise to the clear solution 2) obtained and adjusts its PH to 9, determine the Nb (OH) for generating white5Precipitating, and
By the turbid solution containing precipitating in 60 DEG C of standing 2h.
4) the white Nb (OH) for filtering and 3) obtaining is washed repeatedly with deionized water5Then precipitating presses Nb (OH)5With citric acid
Molar ratio is 1:3 by citric acid and Nb (OH)5Mixing, and deionized water is added persistently stirs and dissolve it in volume for 24 hours and be
The reagent bottle of 60ml, obtains clear solution.
5) it takes a small amount of solution (quality m1) 4) obtained to be sintered at 900 DEG C, obtains white powder (quality m2), and
By formulaCalculate solution concentration, unit g/mol.
6) to the solution 4) obtained (Nb in molar ratio5+):n(K+):n(Na+Potassium acetate and second is added in)=2:1.1:1.1
Sour sodium powder end is simultaneously stirred continuously 2h, and it is 6 to 7 or so that ammonium hydroxide, which is then added dropwise, and adjusts its PH, and ethylene glycol is then added dropwise in molar ratio, and
It stands for 24 hours.
7) silicon substrate of (100) orientation is washed and preheats 10min in 600 DEG C of stove.
8) the KNN precursor liquid 6) obtained is added dropwise on silicon substrate after preheat, and is revolved in revolving speed 3500r/min spin coater
It applies 30s and obtains wet film, then the vacuum oven by wet film at 150 DEG C keeps the temperature 6min, finally the 10min in 850 DEG C of stove
It is crystallized, every spin coating is primary, with regard to once being annealed.And repeat spin coating 5 times, obtain desired film thickness.
Fig. 1 is the XRD diagram for the potassium-sodium niobate niobium system film that embodiment 1 is produced, and wherein substrate is common (100) orientation
Silicon substrate, heat treatment temperature are 600 DEG C.The pyrolysis temperature of KNN film is 150 DEG C, and annealing temperature is 850 DEG C.It can be with from Fig. 1
See, the KNN crystalline property produced is good, and KNN system film is orientated height preferentially in (001).
Fig. 2 is the XRD diagram for the potassium/sodium niobtae film that embodiment 1 and comparative example are produced, and line 1 and line 2 respectively represent implementation
Example 1 and comparative example products therefrom.Wherein substrate is the silicon substrate of common (100) orientation, and heat treatment temperature is 600 DEG C.KNN is thin
The pyrolysis temperature of film is 150 DEG C, and annealing temperature is 850 DEG C.As can be seen from Figure 2 line 1 is more sharp with respect to the peak of line 2, explanation
The crystalline property that embodiment 1 is produced is more preferable.Also, it may be seen that the film that comparative example is produced is polycrystalline, and containing some miscellaneous
Peak；And the film that embodiment 1 is produced is (001) height film preferentially, without miscellaneous peak, exactly because in this embodiment 1 we
Filtration treatment has been carried out to the clear solution that step 4) obtains, and without implementing filtration treatment in comparative example, what step 4) was produced
Solution may be containing impurity such as niobium oxide, this will will affect KNN system crystalline property and preferentially spend.
Embodiment 2
Referring to the method for embodiment 1, one group of parallel laboratory test is carried out, difference is, in step 9), by wet film at 150 DEG C
Vacuum oven keeps the temperature 6min, and finally 10min is crystallized in 850 DEG C of stove, by wet film obtained by spin coating respectively 150
DEG C, 200 DEG C, 250 DEG C, keep the temperature 6min, XRD diagram such as Fig. 3 institute of gained KNN film in the vacuum ovens of 300 DEG C and 350 DEG C
Show.
It can be seen that the KNN crystalline property that pyrolysis temperature obtains when being 150~250 DEG C is good, preferentially degree is high, and is pyrolyzed
The KNN crystalline property that temperature is obtained at 300~350 DEG C is poor, preferentially spend it is unobvious, this is because mentioning with pyrolysis temperature
Height, K and Na volatilization are more serious.
Embodiment 3
Referring to the method for embodiment 1, one group of parallel laboratory test is carried out, difference is, in step 9), wet film obtained by spin coating is existed
After keeping the temperature 6min in 150 DEG C of vacuum oven, respectively in 650 DEG C, 700 DEG C, 750 DEG C, 800 DEG C and 850 DEG C of stove
10min carries out annealing crystallization, and the XRD diagram of gained KNN film is as shown in Figure 4.
It can be seen that annealing temperature is within the scope of 650~850 DEG C, crystalline property is good, shows good
(001) preferred orientation.
Claims (10)
1. a kind of preparation method of the potassium sodium niobate film of height preferred orientation, which comprises the steps of:
(1) it weighs niobium oxide and is dissolved in hydrofluoric acid and obtain NbF5Solution, to NbF5Ammonium oxalate is first added in solution, after its dissolution
Alkalinity PH is added dropwise and debugs agent, obtains white precipitate Nb (OH)5, Nb (OH) is washed with deionized5It precipitates and filters；
(2) by filtered Nb (OH)5It is mixed and added into deionized water with citric acid, is stirred to clarify；
(3) clear solution obtained by step (2) is filtered, obtains clear filtering solution；
(4) sylvite and sodium salt is first added into filtering solution obtained by step (3), adjusts pH value after its dissolution, ethylene glycol is added,
Stand, obtain the potassium-sodium niobate precursor solution of clear；
(5) the pre-heat treatment is carried out to silicon wafer substrate, then potassium-sodium niobate presoma described in spin coating is molten in silicon base after preheat
Liquid obtains to surface and is covered with the silicon wafer of wet film, be put into vacuum oven and keep the temperature, then make annealing treatment, obtains potassium sodium niobate film.
2. the preparation method of the potassium sodium niobate film of height preferred orientation according to claim 1, which is characterized in that step
(1) in, by niobium oxide be added hydrofluoric acid in, under 60~90 DEG C of water bath condition 7~12h of heating stirring until dissolution obtain it is clear
Then ammonium oxalate is added in clear solution, continue the heating stirring under water bath condition until ammonium oxalate dissolves.
3. the preparation method of the potassium sodium niobate film of height preferred orientation according to claim 1, which is characterized in that step
(1) in, 1g niobium oxide is dissolved in the hydrofluoric acid of every 5mL.
4. the preparation method of the potassium sodium niobate film of height preferred orientation according to claim 1, which is characterized in that step
(1) in, it is 9 that ammonium hydroxide, which is added dropwise, and adjusts the pH value of solution, obtains white precipitate Nb (OH)5, first by gained white precipitate Nb (OH)5?
60 DEG C of 0.5~2h of ageing, are then washed with deionized and filter.
5. the preparation method of the potassium sodium niobate film of height preferred orientation according to claim 1, which is characterized in that step
(2) in, the citric acid and Nb (OH)5Molar ratio be 3:1.
6. the preparation method of the potassium sodium niobate film of height preferred orientation according to claim 1, which is characterized in that step
(4) in, the molar ratio n (Nb of niobium element in the additional amount of potassium acetate and sodium acetate and the filtering solution5+):n(K+):n(Na+)
=2:1.1:1.1, and PH to 6 is adjusted, the molar ratio of citric acid additive amount is preferably 2 in the additional amount of ethylene glycol and step (2):
1。
7. the preparation method of the potassium sodium niobate film of height preferred orientation according to claim 1, which is characterized in that step
(5) in, it is described to silicon wafer substrate carry out the pre-heat treatment be by silicon wafer substrate 550 DEG C or more at a temperature of preheat 10min.
8. the preparation method of the potassium sodium niobate film of height preferred orientation according to claim 1, which is characterized in that step
(5) in, the spincoating conditions are as follows: revolving speed 3500r/min, time 30s.
9. the preparation method of the potassium sodium niobate film of height preferred orientation according to claim 1, which is characterized in that step
(5) in, the silicon wafer that the surface is covered with wet film is kept the temperature into 6min in 150~250 DEG C of vacuum oven.
10. the preparation method of the potassium sodium niobate film of height preferred orientation according to claim 1, which is characterized in that step
Suddenly in (5), multiple spin coating potassium-sodium niobate precursor solution prepares potassium sodium niobate film, every spin coating in silicon wafer substrate after preheat
Once, annealing is primary；The condition of the annealing are as follows: anneal 10min at a temperature of 650~850 DEG C.
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| CN116514546A (en) * | 2023-07-04 | 2023-08-01 | 乌镇实验室 | Potassium sodium niobate-based leadless piezoelectric ceramic powder and preparation method of leadless piezoelectric ceramic |
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