CN100376506C - Non-plumbum series ferroelectric film with ingredient gradient distribution and its preparation method - Google Patents
Non-plumbum series ferroelectric film with ingredient gradient distribution and its preparation method Download PDFInfo
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- CN100376506C CN100376506C CNB2005100268425A CN200510026842A CN100376506C CN 100376506 C CN100376506 C CN 100376506C CN B2005100268425 A CNB2005100268425 A CN B2005100268425A CN 200510026842 A CN200510026842 A CN 200510026842A CN 100376506 C CN100376506 C CN 100376506C
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Abstract
The present invention relates to a leadless ferroelectric film with ingredient gradient distribution and a preparing method thereof. The Ba(Ti, Zr or Sn)O3 ferro-electricity film with ingredient gradient distribution of the present invention comprises Ba(Ti<1-x>, Zr or Sn<x>)O3, wherein x is from 0 to 0.70. The gradient film Ba(Zr, Ti)O3 (BZT) and Ba(Ti, Sn)O3 (BTS) of the present invention belongs to a leadless system. In a preparing process, particularly in the integration with a Si technology, lead pollution does not exist, and a temperature regulating range is wide. Compared with barium strontium titanate (BST), on the structure, Ba(Zr, Ti)O3 (BZT) materials and Ba(Ti, Sn)O3 (BTS) materials belong to B position substitution in an ABO3 perovskite structure, and the crystal grain size can be regulated in a large range; on the property, the leakage conductance of film materials is reduced, compressional resistance is improved, and the applied range of the gradient film is widened. Compared with BZT and BTS ferroelectric film with the components evenly distributed along the thickness, the Ba(Ti, Zr or Sn)O3 ferro-electricity film with ingredient gradient distribution of the present invention has large dielectric constant and improved temperature characteristic.
Description
Technical field
The invention belongs to and a kind ofly adopt chemical process preparation to have non-lead ferro-electric film that composition gradient distributes and preparation method thereof field.
Background technology
Generally speaking, near the transformation temperature of ferroelectric material, the variation of its dielectric constant with temperature and produce bigger change, especially obvious near its Curie temperature.For ferroelectric material, often near its transformation temperature, have higher dielectric constant, pyroelectric coefficient and piezoelectric property etc.But, limited its scope of application because its temperature profile is bad near transformation temperature.For ferroelectric thin-flim materials, in order to change its temperature profile, prepared (Ba, Sr) TiO
3(BST) ferroelectric membranc forms composition gradient along thickness, has improved the temperature profile of film to a certain extent.But because bst thin film has higher leakage conductance loss, thereby its application is subjected to certain limitation, and this just needs a kind of high-k, the thin-film material of low leakage conductance loss.
Equivalent material as BST has Ta
2O
5, (Ba
I-xSr
x) (Ti
1-yZr
y) O
3(BSTZ), Ba (Zr, Ti) O
3(BZT) and Ba (Ti, Sn) O
3(BTS) etc.Zirconium barium titanate Ba (ZrTi) O
3(BZT) and Ba (Ti, Sn) O
3(BTS) be to BaTiO
3(ABO
3) perovskite structure carries out the B position and substitute.BZT and BTS film have lower leakage conductance electric current, and BZT and BTS film have excellent dielectric properties equally under high frequency, therefore can be applied to the storage capacitor on the DRAM of future generation, ferroelectric material and the dielectric, nonlinear material of MLCC.
Sol-gel process with its stoichiometric ratio precise control, film forming area big and evenly, advantage such as the technological process temperature is low, equipment is simple and being adopted by people, especially have its remarkable advantages aspect the ferroelectric membranc for preparing the composition Gradient distribution.Utilize the low characteristics of sol-gel method thermal treatment temp, rotation each time applies the back and handles under lower temperature, and its organism is decomposed fully, handles under higher temperature more at last, makes it form composition gradient.In recent years, because to going deep into of lead ferro-electric film research, its preparation method is also more and more paid close attention to by people, but concentrate on mostly on the ferroelectric membranc of single composition, and its ferroelectric membranc with composition gradient structure all is to concentrate in the material system of strontium-barium titanate (BST), lead titanate billows (PLT), its pyroelectric property, temperature profile are improved to a certain extent, and have observed unusual ferroelectric hysteresis loop in PLT composition gradient film.The Ba (Zr, Ti) O that at present also do not have the composition gradient structure
3(BZT) and Ba (Ti, Sn) O
3(BTS) ferroelectric membranc.
Summary of the invention
One of purpose of the present invention provides a kind of Ba (Ti, Zr or Sn) O that composition gradient distributes that has
3Ferroelectric membranc.
Another object of the present invention provides a kind of Ba (Ti, Zr or Sn) O that composition gradient distributes that has
3The preparation method of ferroelectric membranc.
Ba (Ti, Zr or Sn) O with composition gradient distribution of the present invention
3Ferroelectric membranc contains Ba (Ti
1-x, Zr or Sn
x) O
3, wherein X is 0-0.70.The substrate that adopts is LaNiO
3/ Pt/Ti/SiO
2/ Si or Pt/Ti/SiO
2/ Si.
Ba (Ti, Zr or Sn) O with composition gradient distribution of the present invention
3The preparation method of ferroelectric membranc is as follows:
Adopt sol-gel method, the component of precursor solution is barium acetate, titanium isopropylate, tin acetate or zirconium iso-propoxide and solvent Glacial acetic acid, ethylene glycol ethyl ether and methyl ethyl diketone, the mol ratio of Zr/Ti or Sn/Ti is x: 1-x in the solution, wherein x is 0-0.70, the ultimate density of its precursor solution is controlled between the 0.2-0.4M, and the substrate of employing is LaNiO
3/ Pt/Ti/SiO
2/ Si or Pt/Ti/SiO
2/ Si.
Last gradient film involved in the present invention and following gradient film are defined as follows: along the film thickness direction, promptly to the substrate direction, the content of tin or zirconium reduces gradually and is defined as gradient film from film surface on the edge; Along the film thickness direction, promptly along from film surface to the substrate direction, the content of tin or zirconium increases gradually and then is defined as down gradient film.
Ba (Ti, Zr or Sn) O with composition gradient distribution of the present invention
3The preparation method of ferroelectric membranc adopts identical precursor solution concentration, different Zr/Ti or Sn/Ti ratio.For example, adopt barium acetate, tin acetate and titanium isopropylate and corresponding solvent, can make Sn/Ti is that 0.1/0.9, volumetric molar concentration are the precursor solution of the titanium barium stannate of 0.3M; Can obtain Sn/Ti equally respectively and be 0/1,0.05/0.95,0.10/0.90,0.15/0.85, volumetric molar concentration is the precursor solution of the titanium barium stannate of 0.3M.Adopt the method that applies with the compatible mutually rotation of semiconductor technology, and can obtain to have the ferroelectric membranc of composition gradient distribution through suitable thermal treatment process.
Ba (Ti, Zr or Sn) O with composition gradient distribution of the present invention
3Ferroelectric membranc, employed substrate are LaNiO
3/ Pt/Ti/SiO
2/ Si (100) or Pt/Ti/SiO
2/ Si, LaNiO
3, Pt, Ti, SiO
2With the thickness of Si sheet be respectively 150nm, 150nm, 50nm, 150nm and 3500nm.
Ba (Ti, Zr or Sn) O with composition gradient distribution of the present invention
3The preparation method of ferroelectric membranc, when rotation applied, speed of rotation was 3500 rev/mins, 20 seconds time.Gel-film is directly put into 500 ℃ tube furnace, was placed 5 minutes, takes out postcooling to room temperature, applies one deck gel-film down, move in circles up to the film that obtains desired thickness, at last with this film 650 ℃ of-700 ℃ of following thermal treatments 0.5～1 hour.The method sputter gold of the d.c. sputtering of surface employing thereon is as top electrode then, and its diameter is that 0.5mm, thickness are about 100nm.
Ba (Ti, Zr or Sn) O with composition gradient distribution of the present invention
3Ferroelectric membranc, the concentration of used precursor solution, the number of plies of coating and last to obtain the total thickness of film relevant, promptly volumetric molar concentration is big more, and its thickness is also just big more; The number of plies is many more, and its thickness is also big more.For ferroelectric membranc, its thickness is 600-800nm generally speaking.
Beneficial effect of the present invention: (PLT) compares with the lead titanate billows, gradient film Ba (Zr, Ti) O involved in the present invention
3(BZT) and Ba (Ti, Sn) O
3(BTS) belong to nonlead system, in preparation process especially with the integrating process of Si technology in do not have plumbous pollution, and the scope of adjusting temperature is also than broad.(BST) compares with strontium-barium titanate, structurally: Ba (Zr, Ti) O
3(BZT) and Ba (Ti, Sn) O
3(BTS) material belongs to ABO
3B position in the perovskite structure substitutes, and its grain-size can be adjusted in bigger scope; On the performance: reduced leakage conductance for thin-film material, improved voltage endurance, widened the range of application of gradient film.Compare Ba (Ti, Zr or the Sn) O with composition gradient distribution of the present invention with the BTS ferroelectric membranc with the BZT that is evenly distributed along the thickness composition
3Ferroelectric membranc has the bigger specific inductivity and the temperature profile of improvement.
Description of drawings
Fig. 1 is that preparation is at LaNiO
3/ Pt/Ti/SiO
2Go up the depth profile figure of the x-ray photoelectron spectroscopy (XPS) of composition gradient BTS film on the/Si substrate.
Fig. 2 is that preparation is at LaNiO
3/ Pt/Ti/SiO
2Go up the specific inductivity of composition gradient BTS film and the relation of dielectric loss and temperature on/the Si substrate.
Fig. 3 is that preparation is at LaNiO
3/ Pt/Ti/SiO
2Go up the depth profile figure of the x-ray photoelectron spectroscopy (XPS) of composition gradient BZT film on the/Si substrate.
Fig. 4 is that preparation is at LaNiO
3/ Pt/Ti/SiO
2Go up the specific inductivity of composition gradient BZT film and the relation of dielectric loss and temperature on/the Si substrate.
Embodiment
Preparation Ba (Ti
1-xSn
x) O
3, composition gradient ferroelectric membranc on the x=0,0.05,0.10 and 0.15:
The chemical feedstocks that is adopted is barium acetate [Ba (CH
3COO
2], tin acetate [Sn (CH
3COO)
4] and titanium isopropylate [Ti (OC
3H
7)
4], solvent is Glacial acetic acid and ethylene glycol ethyl ether.Earlier barium acetate and tin acetate (according to certain stoichiometric ratio x=0.10) are heated to boiling in glacial acetic acid solution, stop heating after 10 minutes, and be cooled to room temperature, the mol ratio of Ba+Sn and Glacial acetic acid is 1: 10.Mixing solutions with titanium isopropylate, ethylene glycol ethyl ether and methyl ethyl diketone (AcAc) joins in the glacial acetic acid solution of baric and tin, wherein again: the mol ratio of Ti and AcAc is 1: 2, and the mol ratio of titanium isopropylate and ethylene glycol ethyl ether is 1: 10.Add ethylene glycol ethyl ether at last the concentration of final solution is adjusted to 0.3M.The precursor solution of same other component is according to said method synthetic, places and is used for preparing film after 24 hours.
Employed substrate is LaNiO
3/ Pt/Ti/SiO
2/ Si (100), LaNiO
3, Pt, Ti, SiO
2With the thickness of Si sheet be respectively 150nm, 150nm, 50nm, 150nm and 3500nm.Use the precursor solution of x=0 at substrate LaNiO earlier
3/ Pt/Ti/SiO
23 layers of the last coatings of/Si, precursor solution with x=0.05 applies 3 layers then, precursor solution with x==0.10 applies 3 layers again, precursor solution with x=0.15 applies 3 layers at last, like this along the film thickness direction, promptly along from film surface to the substrate direction, the content of tin reduces gradually form to go up gradient film.More than each layer all will be through 500 ℃, 5 minutes thermal treatment.At last with this film 700 ℃ of following thermal treatments 0.5 hour.Gold electrode is as top electrode in the method sputter of the d.c. sputtering of surface employing thereon then, and its diameter is that 0.5mm, thickness are about 100nm.
Ba (the Ti of above-mentioned preparation
1-xSn
x) O
3, depth profile figure, specific inductivity and the dielectric loss of the x-ray photoelectron spectroscopy (XPS) of composition gradient ferroelectric membranc and the relation of temperature are seen Fig. 1 and Fig. 2 on the x=0,0.05,0.10 and 0.15.By Fig. 1 and Fig. 2 as seen, formed Ba (Ti with this method
1-xSn
x) O
3The ferroelectric membranc of last composition gradient, and have good specific inductivity and temperature profile.
Preparation Ba (Ti
1-xZr
x) O
3, composition gradient ferroelectric membranc on the x=0,0.09,0.18 and 0.35:
The chemical feedstocks that is adopted is barium acetate [Ba (CH
3COO)
2], zirconium iso-propoxide [Zr (OC
3H
7)
4] and titanium isopropylate [Ti (OC
3H
7)
4], solvent is Glacial acetic acid and ethylene glycol ethyl ether.Earlier barium acetate (according to certain stoichiometric ratio x=0.35) is heated to boiling in glacial acetic acid solution, stops heating after 5 minutes, and be cooled to room temperature, the mol ratio of Ba and Glacial acetic acid is 1: 10.Mixing solutions with zirconium iso-propoxide and titanium isopropylate, ethylene glycol ethyl ether and methyl ethyl diketone (AcAc) joins in the glacial acetic acid solution of baric again, wherein: the mol ratio of Ti and AcAc is 1: 2, (titanium isopropylate+zirconium iso-propoxide): the mol ratio of ethylene glycol ethyl ether is 1: 10.Add ethylene glycol ethyl ether at last the concentration of final solution is adjusted to 0.3M.The precursor solution of same other component is according to said method synthetic, places and is used for preparing film after 24 hours.
Employed substrate is LaNiO
3/ Pt/Ti/SiO
2/ Si (100), LaNiO
3, Pt, Ti, SiO
2With the thickness of Si sheet be respectively 150nm, 150nm, 50nm, 150nm and 3500nm.Use the precursor solution of x=0 at substrate LaNiO earlier
3/ Pt/Ti/SiO
23 layers of the last coatings of/Si, precursor solution with x=0.09 applies 3 layers then, precursor solution with x=0.18 applies 3 layers again, precursor solution with x=0.35 applies 3 layers at last, like this along the film thickness direction, promptly along from film surface to the substrate direction, the content of zirconium reduces gradually form to go up gradient film.More than each layer all will be through 500 ℃, 5 minutes thermal treatment.At last with this film 700 ℃ of following thermal treatments 0.5 hour.Gold electrode is as top electrode in the method sputter of the d.c. sputtering of surface employing thereon then, and its diameter is that 0.5mm, thickness are about 100nm.
Ba (the Ti of above-mentioned preparation
1-xZr
x) O
3, depth profile figure, specific inductivity and the dielectric loss of the x-ray photoelectron spectroscopy (XPS) of composition gradient ferroelectric membranc and the relation of temperature are seen Fig. 3 and Fig. 4 on the x=0,0.09,0.18 and 0.35.By Fig. 3 and Fig. 4 as seen, formed Ba (Ti with this method
1-xZr
x) O
3The ferroelectric membranc of last composition gradient, and have good specific inductivity and temperature profile.
Embodiment 3
Preparation Ba (Ti
1-xZr
x) O
3, x=0.15,0.30,0.50 and 0.70 time composition gradient ferroelectric membranc:
The chemical feedstocks that is adopted and the collocation method of precursor solution are with embodiment 2.The substrate that adopts is Pt/Ti/SiO
2/ Si.Use the precursor solution of x=0.70 at substrate LaNiO earlier
3/ Pt/Ti/SiO
23 layers of the last coatings of/Si, precursor solution with x=0.50 applies 3 layers then, precursor solution with x=0.30 applies 3 layers again, precursor solution with x=0.15 applies 3 layers at last, like this along the film thickness direction, promptly along from film surface to the substrate direction, the content of zirconium increases gradually and forms gradient film down.More than each layer all will be through 500 ℃, 5 minutes thermal treatment.At last with this film 650 ℃ of following thermal treatments 1 hour.Gold electrode is as top electrode in the method sputter of the d.c. sputtering of surface employing thereon then, and its diameter is that 0.5mm, thickness are about 100nm.By the graph of a relation of depth profile figure, specific inductivity and the dielectric loss of its x-ray photoelectron spectroscopy (XPS) and temperature as seen, formed the BZT film of time component gradient, and this Ba (Ti
1-xZr
x) O
3Film has good specific inductivity and temperature profile.
The concentration of used precursor solution, the number of plies of coating and last to obtain the total thickness of film relevant, promptly volumetric molar concentration is big more, and its thickness is also just big more; The number of plies is many more, and its thickness is also big more.For ferroelectric membranc, its thickness is 600-800nm generally speaking.
Claims (6)
1. one kind has Ba (Ti, Zr or the Sn) O that composition gradient distributes
3Ferroelectric membranc is characterized in that, contains Ba (Ti
1-xZr
x) O
3Or Ba (Ti
1-xSn
x) O
3, wherein x is 0～0.70, to the substrate direction, forms the film of the concentration gradients variation of tin or zirconium from film surface.
2. Ba (Ti, Zr or the Sn) O with composition gradient distribution as claimed in claim 1
3Ferroelectric membranc is characterized in that from film surface to the substrate direction, forms the following gradient film that the content of tin or zirconium increases gradually.
3. Ba (Ti, Zr or the Sn) O with composition gradient distribution as claimed in claim 1
3Ferroelectric membranc is characterized in that from film surface to the substrate direction, forms the last gradient film that the content of tin or zirconium reduces gradually.
4. claim 1～3 is arbitrary has Ba (Ti, a Zr or Sn) O that composition gradient distributes
3The preparation method of ferroelectric membranc, sol-gel method is adopted in the preparation of gel in this method, the component of precursor solution is barium acetate, titanium isopropylate, tin acetate or zirconium iso-propoxide and solvent Glacial acetic acid, ethylene glycol ethyl ether and methyl ethyl diketone, the mol ratio of Zr/Ti or Sn/Ti is x: 1-x in the solution, wherein x is 0～0.70, and the final volumetric molar concentration of its precursor solution is controlled between the 0.2-0.4M; The substrate that adopts is LaNiO
3/ Pt/Ti/SiO
2/ Si or Pt/Ti/SiO
2/ Si; Apply to adopt with the method for the compatible mutually rotation coating of semiconductor technology and heat-treat.
5. Ba (Ti, Zr or the Sn) O with composition gradient distribution as claimed in claim 4
3The preparation method of ferroelectric membranc is characterized in that substrate LaNiO
3, Pt, Ti, SiO
2With the thickness of Si sheet be respectively 150nm, 150nm, 50nm, 150nm and 3500nm.
6. Ba (Ti, Zr or the Sn) O with composition gradient distribution as claimed in claim 4
3The preparation method of ferroelectric membranc is characterized in that said rotation coating and thermal treatment are meant: speed of rotation is 3500 rev/mins, 20 seconds time; Gel-film is directly put into 500 ℃ tube furnace, was placed 5 minutes, take out postcooling, apply one deck gel-film down, move in circles up to the film that obtains desired thickness to room temperature, at last with this film 650 ℃ of-700 ℃ of following thermal treatments 0.5～1 hour.
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| CN102136315B (en) * | 2011-03-21 | 2012-08-15 | 四川师范大学 | Multilayer-ceramic total-area LNO (lanthanum nickel oxide)/Ag/LNO composite electrode and preparation method thereof |
| CN103762078B (en) * | 2014-01-20 | 2017-02-01 | 中国科学院物理研究所 | Wide-temperature area tunable microwave device based on combined thin film |
| CN108531867B (en) * | 2018-03-28 | 2020-03-03 | 天津大学 | Preparation method of flexible BTS/BZT/BTS multilayer thin film varactor |
| CN112397643B (en) * | 2020-11-17 | 2023-04-18 | 武汉理工大学 | Thin film material with high electrocaloric effect near room temperature and preparation method thereof |
| CN114388266B (en) * | 2022-01-14 | 2024-01-30 | 西安交通大学 | High-energy-storage-density wide-working-temperature component gradient structural film and preparation method thereof |
| CN115304368B (en) * | 2022-08-26 | 2023-05-12 | 广东康荣高科新材料股份有限公司 | Microwave dielectric ceramic material for positioning antenna and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1342783A (en) * | 2001-09-14 | 2002-04-03 | 中国科学院上海硅酸盐研究所 | Process for preparing functional gradient film of lead zirconate titanate ceramics |
| CN1537826A (en) * | 2003-10-23 | 2004-10-20 | 同济大学 | Method of preparing leadless calcium titanium ore structure ferroelectric film possessing high orientation |
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2005
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1342783A (en) * | 2001-09-14 | 2002-04-03 | 中国科学院上海硅酸盐研究所 | Process for preparing functional gradient film of lead zirconate titanate ceramics |
| CN1537826A (en) * | 2003-10-23 | 2004-10-20 | 同济大学 | Method of preparing leadless calcium titanium ore structure ferroelectric film possessing high orientation |
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