CN104556240A - Preparation method of bismuth titanate (BT) ferroelectric film - Google Patents
Preparation method of bismuth titanate (BT) ferroelectric film Download PDFInfo
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Abstract
The invention relates to the field of the preparative technology of ferroelectric films and devices and in particular relates to a preparation method of a bismuth titanate (BT) ferroelectric film. Solution modification and ultraviolet radiation are combined to reduce the sintering temperature of the film to be below 500 DEG C, the defects that the existing bismuth titanate ferroelectric film has high sintering temperature and the Bi element can be volatized easily are overcome and the purpose of compatibility with a Si integration circuit is achieved. The preparation method comprises the following steps: (1) preparing precursor solution; (2) preparing a BT gel film; (3) carrying out pretreatment on the BT gel film; and (4) performing ultimate treatment on a BT precursor film.
Description
one, technical field
The present invention relates to ferroelectric membranc and device preparing technical field, be specifically related to a kind of preparation method of bismuth titanate ferro-electricity membrane.
two, background technology
Due to dielectric, electric light, acousto-optic, Preset grating, nonlinear optics, pyroelectricity and piezoelectric property that ferroelectrics is special, be a kind of material having commercial application prospect, therefore ferroelectric application causes the attention of community of physicists and material supply section educational circles very early.Nineteen fifties just once started the climax to ferroelectrics applied research.Since the seventies, due to going deep into of being familiar with ferroelectrics, the expansion of artificial ferroelectric material kind, the progress of microelectronics integrated technology, particularly along with a series of breakthroughs of ferroelectric membranc technology of preparing, successfully prepare the ferroelectric membranc of excellent property, operating voltage can at 3-5V, can be integrated with Si or GaAs circuit, ferroelectric membranc preparation technology and ic process compatibility become possibility, greatly facilitate the preparation of ferroelectric membranc and the development of device application research, make it in microtronics, photoelectronics, the field such as integrated optics and microelectromechanical systems has a wide range of applications, become one of focus of new function material research in the world.
But how to obtain the ferroelectric membranc of high-quality, how to allow the preparation of ferroelectric membranc and the process compatible of unicircuit, be the difficult problem that annoying people, which greatly limits the application & development of ferroelectric material.Recent two decades come, along with the development of micro & nano technology and the needs of practical application, adopt low cost, be easy to the wet chemistry methods such as business-like collosol and gel or chemical solution deposition, preparation there is various magnetic, the film of optical, electrical characteristic be subject to gradually people pay attention to.Adopt sol-gel technique to prepare oxide nano-film, and form corresponding device, become research and development focus in recent years gradually.
But traditional sol-gel method is prepared sull and be there is an important difficult problem and do not overcome, namely the Tc of this kind of film prepared of sol-gel method is higher, generally all more than 600 DEG C.And this temperature is with current Si base semiconductor Technology and incompatible (requiring less than 500 DEG C).The low-temperature sol-gel technology of preparing that development is novel is the key that this kind of perovskite oxide material is able in microelectronic application.
In ferroelectric material, PZT no doubt has excellent ferroelectric properties, but because containing poisonous Pb, cause certain pollution to environment, the World Health Organization clearly proposes the use that will limit this kind of material.For this reason, new ferroelectric material must be developed, this wherein, Bi
4ti
3o
12(being abbreviated as BT) material attracts wide attention.This material has high residual polarization value, good resistent fatigue characteristic, therefore, will have very large using value in the nonvolatile memory in future.But Bi prepared by collosol and gel
4ti
3o
12film, generally all needs the Tc of more than 600 DEG C, how to improve solution composition, or by other measures, reduce sintering temperature, making it to merge with Si unicircuit, is Bi
4ti
3o
12film is applied the problem that must solve.
three, summary of the invention
The present invention is in order to solve the weak point in above-mentioned background technology, a kind of preparation method of bismuth titanate ferro-electricity membrane is provided, its way be combined with uv irradiation by solution modification, the sintering temperature of film is made to be reduced to less than 500 DEG C, solve existing bismuth titanate ferro-electricity membrane sintering temperature high, the defects such as Bi element easily volatilizees, and reach the object with Si unicircuit compatibility.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of bismuth titanate ferro-electricity membrane, is characterized in that: described preparation method comprises the following steps:
1) preparation of precursor aqueous solution
Bismuth trinitrate (hereinafter referred to as BT) to be dissolved in the solution containing solvent and acetic acid by 1.1, obtains solution A after stirring clarification; In solution A, the mol ratio of acetic acid and Bismuth trinitrate is 15 ~ 20:1;
Butyl (tetra) titanate solution to be poured in the mixing solutions containing solvent and methyl ethyl diketone by 1.2, and after stirring clarification, obtain solution B, in solution B, the molar ratio of methyl ethyl diketone and butyl (tetra) titanate is 1 ~ 2:1;
Solution A and solution B mix according to mol ratio Bi:Ti=4:3 by 1.3, obtain mixing solutions;
By regulating solvent load, the total concn of Bi and Ti ion in mixing solutions is made to control within the scope of 0.2 ~ 0.5mol/l;
The mixing solutions of acquisition after standing 24 ~ 48 hours, according to Ti: ammoniacal liquor: the mol ratio of nitric acid=1:3:3 adds ammoniacal liquor and nitric acid, is namely obtained BT precursor aqueous solution by 1.4;
2) preparation of BT gel-film
The BT precursor aqueous solution utilizing step 1) to obtain, is being coated with Pt, ITO or LaNiO
3in the Si substrate of conductive layer, by lift or spin-coating method, obtained BT gel-film;
3) pre-treatment of BT gel-film
By step 2) the BT gel-film that obtains, be placed on the hot-plate of 250-300 DEG C, the uv light irradiation BT gel-film 20-50min utilizing wavelength to be 184-254nm, obtains BT precursor thin film;
4) process at end of BT precursor thin film
Step 3) is obtained BT precursor thin film, insert in infrared induction process furnace, be rapidly heated to 440-460 DEG C, and be incubated 30 minutes, obtain BT film;
In order to increase film thickness, need repeating step 2), step 3) and step 4) are about 5-6 time, can obtain the BT film of crystallization.
Ammoniacal liquor in BT precursor aqueous solution in described step 1), the molar ratio of nitric acid and methyl ethyl diketone is: ammoniacal liquor: nitric acid: methyl ethyl diketone=3:3:1 ~ 2.
Step 1) described in solvent be methyl alcohol or ethylene glycol monomethyl ether.
Step 3) medium ultraviolet lamp launch UV-light in, the ultraviolet of wavelength 184nm accounts for more than 10%, and the ultraviolet of wavelength 254nm accounts for more than 80%.
Step 3) described in ultraviolet lamp and the distance of BT gel-film remain within the scope of 1-5cm.
Step 4) described in BT precursor thin film be rapidly heated speed control within p.s. 25-50 DEG C.
Compared with prior art, the advantage that has of the present invention and effect as follows:
1, add methyl ethyl diketone in the solution, and ammoniacal liquor is stablizer, with butyl (tetra) titanate complexing, defines the titanium metal complex compound of not easily hydrolytie polycondensation, thus make solution-stabilized, do not precipitate.In addition, the ultraviolet of this complex compound to 254nm wavelength has strong sorption, and the energy of absorption facilitates the decomposition of metallorganics, and forms metal-oxygen-metal frame, for follow-up low-temperature sintering provides the foundation.Meanwhile, by adding nitric acid in the solution as oxygenant, avoid the generation of the film anoxia phenomenon after decomposition.Define corresponding oxide compound.In a word, this patent passes through the accurate control of chemical solution component and additive, there is provided energy with ultraviolet auxiliary irradiation, make originally to need the sintering temperature of the bismuth titanate film of more than 600oC crystallization to be reduced to below 500oC, namely achieve below the patient temperature of Si semi-conductor institute.Like this, for Si based ferroelectric film device in future provides a kind of new approaches.
2, due to the ultraviolet irradiation effect of short wavelength, with gel film generation photochemical reaction, decompose the oxonium ion in gel-film, and form ozone, there is strong activity and oxygenizement, thus react with the carbon in gel-film, form CO
2take film out of, reduce the residual of carbon in film dramatically, thus ensured the ferroelectric properties of film.
3, the bismuth in bismuth titanate film has very strong volatility, thermal treatment temp is higher, what volatilize is more, the present invention reduces sintering temperature by the effect of the ultraviolet irradiation of short wavelength, thus reduce the volatility of bismuth, effectively ensure that the stoichiometric ratio of bismuth and titanium in bismuth titanates, thus ensure that gained bismuth titanate film has good characteristic.
Four, accompanying drawing explanation
The XRD figure of Fig. 1 bismuth titanate film;
The polarizability of Fig. 2 bismuth titanate film and the relation of extra electric field;
The fatigue characteristic graphic representation of Fig. 3 bismuth titanate film.
Five, embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
1), the preparation of precursor aqueous solution
Bismuth trinitrate (hereinafter referred to as BT) is dissolved in the solution containing methyl alcohol and acetic acid, after stirring clarification, obtains solution A; In solution A, the mol ratio of acetic acid and Bismuth trinitrate is 15:1.
Butyl (tetra) titanate solution is poured in the mixing solutions containing methyl alcohol and methyl ethyl diketone, after stirring clarification, obtain solution B; In solution B, the molar ratio of methyl ethyl diketone and butyl (tetra) titanate is 1:1.
Solution A and solution B are mixed according to mol ratio Bi:Ti=4:3, obtains mixing solutions;
By regulating methanol usage, the total concn of Bi and Ti ion in mixing solutions is controlled at 0.3mol/l.
After the mixing solutions obtained is left standstill 24 ~ 48 hours, according to Ti: ammoniacal liquor: the mol ratio of nitric acid=1:3:3 adds ammoniacal liquor and nitric acid, namely obtain BT precursor aqueous solution;
2) preparation of BT gel-film
The BT precursor aqueous solution utilizing step 1) to obtain, in the Si substrate being coated with Pt conductive layer, by lift or spin-coating method, obtained BT gel-film;
3), the pre-treatment of BT gel-film
By step 2) the BT gel-film that obtains, be placed on the hot-plate of 300 DEG C, the uv light irradiation BT gel-film 50min utilizing wavelength to be 184-254nm, obtains BT precursor thin film;
4), the process at end of BT precursor thin film
Step 3) is obtained BT precursor thin film, insert in infrared induction process furnace, be rapidly heated to 450 DEG C, and be incubated 30 minutes, obtain BT film;
In order to increase film thickness, repeating step 2), step 3) and step 4) totally 5 times, can obtain the crystallization BT film that 350nm is thick.
The BT film XRD figure that embodiment 1 prepares is see Fig. 1, and as can be seen from Figure 1, BT film prepared by embodiment 1 produces without other dephasigns.In XRD except substrate Pt, exist without other dephasigns, illustrate that gained film is pure bismuth titanate film; The electric polarization curve of BT film prepared by embodiment 1 as shown in Figure 2.Film is under DC Electric Field as shown in Figure 2, has good ferroelectric hysteresis loop feature, and when extra electric field reaches 25V, the residual polarization value of film can reach 10 μ C/cm
2, show good ferroelectric properties; As shown in Figure 3, the BT film that as shown in Figure 3 prepared by embodiment 1 reaches 10 in cycle index to the Fatigue Test result of BT film prepared by embodiment 1
8time above, just show certain fatigability, therefore, BT film prepared by embodiment 1 has good resistent fatigue characteristic, namely has very long work-ing life.
Embodiment 2
1) preparation of precursor aqueous solution
Bismuth trinitrate (hereinafter referred to as BT) is dissolved in the solution containing methyl alcohol and acetic acid, after stirring clarification, obtains solution A.In solution A, the mol ratio of acetic acid and Bismuth trinitrate is 20:1.
Butyl (tetra) titanate solution is poured in the mixing solutions containing methyl alcohol and methyl ethyl diketone, after stirring clarification, obtain solution B; In solution B, the molar ratio of methyl ethyl diketone and butyl (tetra) titanate is 1.5:1.
Solution A and solution B are mixed according to 4:3, according to mol ratio Bi:Ti=4:3 mixing, obtains mixing solutions;
By regulating methanol usage, the total concn of Bi and Ti ion in mixing solutions is controlled at 0.4mol/l.
After the mixing solutions obtained is left standstill 24 ~ 48 hours, according to Ti: ammoniacal liquor: the mol ratio of nitric acid=1:3:3 adds ammoniacal liquor and nitric acid, namely obtain BT precursor aqueous solution;
2), the preparation of BT gel-film
The BT precursor aqueous solution utilizing step 1) to obtain, is being coated with LaNiO
3in the Si substrate of conductive layer, by lift or spin-coating method, obtained BT gel film;
3), the pre-treatment of BT gel film
By step 2) the BT gel film that obtains, be placed on the hot-plate of 300 DEG C, the uv light irradiation BT gel film 40min utilizing wavelength to be 184-254nm, obtains BT precursor thin film;
4), the process at end of BT precursor thin film
Step 3) is obtained BT precursor thin film, insert in infrared induction process furnace, be rapidly heated to 450 DEG C, and be incubated 20 minutes, obtain BT film;
In order to increase film thickness, repeating step 2), step 3) and step 4) totally 5 times, can obtain the crystallization BT film that 320nm is thick.
BT film excess polarization value prepared by embodiment 2 can reach 8 μ C/cm
2, fatigue life cycle can reach 10
8above.
Embodiment 3
1) preparation of precursor aqueous solution
Bismuth trinitrate is dissolved in the solution containing ethylene glycol monomethyl ether and acetic acid, after stirring clarification, obtains solution A; In solution A, the mol ratio of acetic acid and Bismuth trinitrate is 20:1.
Butyl (tetra) titanate solution is poured in the mixing solutions containing ethylene glycol monomethyl ether and methyl ethyl diketone, after stirring clarification, obtain solution B; In solution B, the molar ratio of methyl ethyl diketone and butyl (tetra) titanate is 2:1;
Solution A and solution B are mixed according to mol ratio Bi:Ti=4:3, obtains mixing solutions;
By regulating methanol usage, the total concn of Bi and Ti ion in solution is controlled at 0.5mol/l.
After the mixing solutions obtained is left standstill 24 ~ 48 hours, according to Ti: ammoniacal liquor: the mol ratio of nitric acid=1:3:3 adds ammoniacal liquor and nitric acid, namely obtain BT precursor aqueous solution;
2), the preparation of BT gel-film
The BT precursor aqueous solution utilizing step 1) to obtain, in the Si substrate being coated with Pt conductive layer, by lift or spin-coating method, obtained BT gel-film;
3), the pre-treatment of BT gel-film
By step 2) the BT gel-film that obtains, be placed on the hot-plate of 250 DEG C, the uv light irradiation BT gel-film 40min utilizing wavelength to be 184-254nm, obtains BT precursor thin film;
4), the process at end of BT precursor thin film
Step 3) is obtained BT precursor thin film, insert in infrared induction process furnace, be rapidly heated to 460 DEG C, and be incubated 30 minutes, obtain BT film;
In order to increase the thickness of film, repeating step 2), step 3) and step 4) totally 6 times, can obtain the crystallization BT film that 400nm is thick.
BT film excess polarization value prepared by embodiment 3 can reach 9 μ C/cm
2, fatigue life cycle can reach 10
8above.
Step 3 in above-mentioned 3 embodiments) medium ultraviolet lamp launch UV-light in, the ultraviolet of wavelength 184nm accounts for more than 10%, and the ultraviolet of wavelength 254nm accounts for more than 80%, and the distance of described ultraviolet lamp and BT gel-film remains within the scope of 1-5cm.
Step 4 in above-mentioned 3 embodiments) described in BT precursor thin film be rapidly heated speed control within p.s. 25-50 DEG C.
Claims (6)
1. a preparation method for bismuth titanate ferro-electricity membrane, is characterized in that: described preparation method comprises the following steps:
1) preparation of precursor aqueous solution
Bismuth trinitrate (hereinafter referred to as BT) to be dissolved in the solution containing solvent and acetic acid by 1.1, obtains solution A after stirring clarification; In solution A, the mol ratio of acetic acid and Bismuth trinitrate is 15 ~ 20:1;
Butyl (tetra) titanate solution to be poured in the mixing solutions containing solvent and methyl ethyl diketone by 1.2, and after stirring clarification, obtain solution B, in solution B, the molar ratio of methyl ethyl diketone and butyl (tetra) titanate is 1 ~ 2:1;
Solution A and solution B mix according to mol ratio Bi:Ti=4:3 by 1.3, obtain mixing solutions;
By regulating solvent load, the total concn of Bi and Ti ion in mixing solutions is made to control within the scope of 0.2 ~ 0.5mol/l;
The mixing solutions of acquisition after standing 24 ~ 48 hours, according to Ti: ammoniacal liquor: the mol ratio of nitric acid=1:3:3 adds ammoniacal liquor and nitric acid, is namely obtained BT precursor aqueous solution by 1.4;
2) preparation of BT gel-film
The BT precursor aqueous solution utilizing step 1) to obtain, is being coated with Pt, ITO or LaNiO
3in the Si substrate of conductive layer, by lift or spin-coating method, obtained BT gel-film;
3) pre-treatment of BT gel-film
By step 2) the BT gel-film that obtains, be placed on the hot-plate of 250-300 DEG C, the uv light irradiation BT gel-film 20-50min utilizing wavelength to be 184-254nm, obtains BT precursor thin film;
4) process at end of BT precursor thin film
Step 3) is obtained BT precursor thin film, insert in infrared induction process furnace, be rapidly heated to 440-460 DEG C, and be incubated 30 minutes, obtain BT film;
In order to increase film thickness, need repeating step 2), step 3) and step 4) are about 5-6 time, can obtain the BT film of crystallization.
2. according to the preparation method of a kind of bismuth titanate ferro-electricity membrane described in claim 1, it is characterized in that: ammoniacal liquor in BT precursor aqueous solution in described step 1), the molar ratio of nitric acid and methyl ethyl diketone is: ammoniacal liquor: nitric acid: methyl ethyl diketone=3:3:1 ~ 2.
3. the preparation method of a kind of bismuth titanate ferro-electricity membrane according to claim 1 and 2, is characterized in that: step 1) described in solvent be methyl alcohol or ethylene glycol monomethyl ether.
4. the preparation method of a kind of bismuth titanate ferro-electricity membrane according to claim 3, is characterized in that: step 3) medium ultraviolet lamp launch UV-light in, the ultraviolet of wavelength 184nm accounts for more than 10%, and the ultraviolet of wavelength 254nm accounts for more than 80%.
5. the preparation method of a kind of bismuth titanate ferro-electricity membrane according to claim 4, is characterized in that: step 3) described in ultraviolet lamp and the distance of BT gel-film remain within the scope of 1-5cm.
6. the preparation method of a kind of bismuth titanate ferro-electricity membrane according to claim 5, is characterized in that: step 4) described in BT precursor thin film be rapidly heated speed control within p.s. 25-50 DEG C.
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Cited By (4)
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|---|---|---|---|---|
| CN105870123A (en) * | 2016-03-25 | 2016-08-17 | 广西大学 | Tungsten bismuth titanate ferroelectric film and preparation method thereof |
| CN106915771A (en) * | 2017-02-27 | 2017-07-04 | 江苏大学 | One kind is with C3N4The method that mesoporous wire bismuth titanates is prepared for template |
| CN110078131A (en) * | 2019-05-30 | 2019-08-02 | 西安理工大学 | Using Si as substrate c-axis oriented growth Bi4Ti2.95Co0.05O12More iron thin films and preparation method thereof |
| CN113264550A (en) * | 2021-05-18 | 2021-08-17 | 攀枝花学院 | Preparation method of lithium titanate negative electrode material |
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| CN106915771A (en) * | 2017-02-27 | 2017-07-04 | 江苏大学 | One kind is with C3N4The method that mesoporous wire bismuth titanates is prepared for template |
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| CN113264550A (en) * | 2021-05-18 | 2021-08-17 | 攀枝花学院 | Preparation method of lithium titanate negative electrode material |
| CN113264550B (en) * | 2021-05-18 | 2023-04-07 | 攀枝花学院 | Preparation method of lithium titanate negative electrode material |
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