CN100381394C - Preparation method of highly magnesium-doped strontium plumbum titanate high dielectric adjustable film material - Google Patents
Preparation method of highly magnesium-doped strontium plumbum titanate high dielectric adjustable film material Download PDFInfo
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Abstract
The invention discloses a preparing method of high-dielectric adjustable film material of strontium lead titanate doped magnesium, which comprises the following steps: adopting butyl phthalate, lead acetate, strontium carbonate and magnesium carbonate as raw material; making ethandiol dimethyl ether and acetate as solvent; allocating sol former; adopting allocated relative sol former as coating solution; using immersing sash method to prepare film layer; drying the coating; disposing under high-temperature; sintering to obtain PSMT ferric electric film.
Description
Technical field
The present invention relates to a kind of preparation method of highly magnesium-doped strontium plumbum titanate high dielectric adjustable film material.
Background technology
In recent years, ferroelectric membranc relies on it superior ferroelectric, piezoelectricity, pyroelectricity, electric light, light is sold off and performances such as non-linear optical, is used to make ferroelectric storage memory, pyroelectric detector array, piezo-electric motor, ferroelectric film capacitor, thin film sensor array, iron spot thin film microwave device, ferroelectric optical and integrated optics or the like device.Can be widely used in numerous areas such as microtronics, integrated optics, micromechanics.Along with the progress of film preparing technology and the developing of Application Areas, particularly the technology of preparing of ferroelectric membranc can be compatible mutually with the semiconductor integrated circuit technology, make development research integrate all multi-functional multifunctional circuits, device and systems such as ferroelectric, the piezoelectricity of semi-conductor large-scale integrated circuit and ferroelectric membranc, pyroelectricity, electric light, non-linear optical, have more tempting prospect, ferroelectric thin-flim materials has been described as microelectronic material of new generation.
The adjustable dielectric materials of microwave has wide application background on the adjustable components and parts of microwave, as the phase shifter on the phased array antenna, resonator, wave filter etc.With regard to research system, mainly concentrate on uhligite phase ferroelectric material at present, as strontium-barium titanate (BST) and doped series thereof.Because various film preparing technologies all have the deficiency of himself, the technological factor that in addition influences film quality is more, so far for it, does not obtain to possess simultaneously very ideal high tuning and low-loss material as yet.Discovery strontium lead titanate (PST) potteries such as nearest Cross have higher adjustability and quite low dielectric loss, are a kind of materials that is highly suitable for the electric field adjusting element.Compare with BST, especially as thin-film material, the ferroelectric critical size of PST is less, crystallization temperature is lower, preparation technology and Si microelectronic technique compatibility, more can satisfy the needs that high performance Si basis set becomes circuit, to the miniaturization that promotes the modern device development with integratedly have a crucial meaning.As microwave dielectric material, in order to obtain better application in the adjustable microwave device, material should have (ratio of tunable performance and dielectric loss) of the higher figure of merit.Thereby dielectric materials should have following performance: under microwave frequency, on the one hand, specific inductivity is low, and defective will be lacked, and dielectric loss and leakage current are low; On the other hand, under the direct-current biasing electric field, it is big that the variation of specific inductivity is wanted, and higher tunable performance is arranged.Recently, one of foremost expert of world's dielectric materials research field, people such as the L.Eric Cross of U.S. University of Pennsylvania study strontium lead titanate (PST) material, find that PST is when having higher adjustability (70%), quite low dielectric loss is arranged, can be lower than 0.1%, also promptly reach dielectric loss 10
-4Magnitude, thereby its figure of merit can reach more than 700.With this, Cross etc. point out that PST is a kind of material that is highly suitable for the electric field adjusting element.
Along with the miniaturization of modern device development and integrated, thin-film material has shown its distinctive superiority, thereby the research of thin-film material has obtained suitable attention.Equally, the research work of PST film is also begun, existing existing report obtains the dielectric-constant adjustable of PST film with sol-gel process, and (50%～20%), dielectric loss are (2～5%) approximately.Compare with the data of people such as Cross report, the performance of film also reaches expected value far away, and therefore many problems are anxious to be treated in depth to study and solve.
Doping is that present material modification is studied one of very effective means, can realize charge balance in the material, defective control, grain-size adjustment and crystal property improvement etc. by mixing, and reaches the purpose of optimizing material property.Existing report is to the different element that mixes in the solid bulk PST stupalith, as La
3+, Bi
3+, Y
3+, Mg
2+Or the like carried out preparation research, obtain result highly significant.Yet, the doping vario-property of PST thin-film material is still belonged to the starting stage.Shut out big first-class at Acta Physica Sinica, and 2005 Vol.54 No.11P.5411-5416 write articles and point out, Mg is one of very effective doping agent, can be used for the modification of PST film.Is 40% at experiment condition for Pb content, Sr content is under 60% the situation, Mg replaces the content of Ti can from 0 to 15%, and determined when the doping content of Mg is 10%, the crystal content of film is the highest, and too much Mg mixes then can increase defective greatly, reduces the crystal content of film, at this moment can't form the PST film of crystalline content height and structural integrity, also promptly in the adulterated scope of this lower aq Mg, also fail to obtain very good result.From can know the correlative study result to material in the past, the different Mg doping can produce bigger influence to the performance of associated materials, thereby in order to obtain best dielectric properties and microwave tunable performance, should consider to develop a kind of method that height is mixed Mg in PST, realize practicability in the hope of making PST mix the Mg thin-film material.The present invention selects for use high density Mg ion as doping agent the PST thin film system to be carried out modification, has successfully determined new compositing formula, has improved the incorporation of Mg, makes the Mg doping content can reach 30%.And every dielectric properties of this highly magnesium-doped PST material are all very excellent, and especially the adjustable row of the dielectric of material can reach 63%, has goodish using value.
Summary of the invention
The object of the present invention is to provide the preparation method who prepares a kind of highly magnesium-doped strontium plumbum titanate high dielectric adjustable film material with the sol-gel method.
The step of the technical solution used in the present invention is as follows:
1) plumbic acetate, Strontium carbonate powder, magnesiumcarbonate adding deionized water dissolve in acetic acid, and reacting by heating under 40 ℃～60 ℃ temperature obtains the solution first;
2) butyl (tetra) titanate dissolves in ethylene glycol monomethyl ether, is stirred to mix, and obtains solution second;
3) two kinds of solution of first, second mix, the concentration of controlling wherein Pb, Sr, Mg, four kinds of elementary compositions of Ti is respectively: Pb:0.22mol/L～0.26mol/L, Sr:0.08mol/L～0.12mol/L, Mg:0.035mol/L～0.105mol/L, Ti:0.245mol/L～0.35mol/L, stir, obtain precursor colloidal sol;
4) adopt the precursor colloidal sol of having prepared, at the uniform velocity all immerse substrate 3～5cm/min in the sol system that has prepared, placed for 10～15 seconds, promote with identical speed then, all propose liquid level until substrate, seasoning in air is then put into High Temperature Furnaces Heating Apparatus subsequently and is heat-treated at 550 ℃～600 ℃, after the cooling, repeat aforesaid operations and prepare the 6-8 layer film;
5), obtain mixing the strontium lead titanate film of magnesium 15%～30% with multilayer film thermal treatment 0.5h～1h under 550 ℃～600 ℃ temperature of preparation.
Described substrate is ito substrate, glass substrate, quartz base plate or Si substrate.
The crystalline phase of described strontium lead titanate film is the uhligite phase, and its crystal content is 80%～90%.
The present invention compares the useful effect that has with background technology:
1, the strontium lead titanate ferroelectric membranc that adopts highly magnesium-doped method to form, the film quality of preparation is better, and the thin film crystallization performance can increase under the effect of Mg;
2, since Mg mix the defective that can reduce in the film, thereby the specific inductivity of material increases, and connects electrical loss and obviously reduces;
3, the strontium lead titanate ferroelectric membranc that adopts highly magnesium-doped method to form has the higher dielectric adjustable and the figure of merit preferably.Experiment shows that when the content of magnesium was x=0.2, the dielectric adjustable of mixing the magnesium strontium lead titanate film was 63%, and the figure of merit is 3 times of low-mix magnesium sample;
4, the high adjustability strontium lead titanate ferroelectric membranc that adopts highly magnesium-doped method to form, preparing technique process is simple, and is with low cost, has good market outlook.
Description of drawings
Fig. 1 is the XRD curve of highly magnesium-doped strontium lead titanate ferroelectric membranc of the present invention;
The curve that changes with Mg content when Fig. 2 is the specific inductivity of highly magnesium-doped strontium lead titanate ferroelectric membranc of the present invention and loss 10kHz;
The curve that changes with Mg content when Fig. 3 is the performance the coordinated 10kHz of highly magnesium-doped strontium lead titanate ferroelectric membranc of the present invention.
Embodiment
Embodiment 1:
Plumbic acetate, Strontium carbonate powder add small quantity of deionized water and dissolve in acetic acid, and reacting by heating obtains colourless transparent solution; Butyl (tetra) titanate dissolves in ethylene glycol monomethyl ether, is stirred to mix.Two kinds of solution are mixed, obtain Pb-Sr-Ti precursor colloidal sol, wherein Pb, Sr, three kinds of component concentrations of Ti are respectively: Pb:0.22mol/L, Sr:0.12mol/L, Ti:0.35mol/L.In the glass substrate sol system that at the uniform velocity (4cm/min) immersion has prepared, placed for 10 seconds, make glass substrate be in steady state, promote (4cm/min) with identical speed then, until sheet glass liquid level is proposed all, seasoning in air then.Put into High Temperature Furnaces Heating Apparatus subsequently, under 560 ℃ of temperature, carry out rapid thermal process 5min, after the cooling, repeat aforesaid operations and prepare multilayer film.Multilayer film thermal treatment 0.5h under 590 ℃ of temperature with preparation obtains uhligite phase PST film.Its XRD curve is seen accompanying drawing 1 (a), as seen from the figure, can generate pure strontium lead titanate film under this example condition.Specific inductivity is seen accompanying drawing 2 during its 10kHz.
Embodiment 2:
Plumbic acetate, Strontium carbonate powder, magnesiumcarbonate add small quantity of deionized water and dissolve in acetic acid, and reacting by heating obtains colourless transparent solution; Butyl (tetra) titanate dissolves in ethylene glycol monomethyl ether, is stirred to mix.Two kinds of solution are mixed, obtain Pb-Sr-Mg-Ti precursor colloidal sol, wherein Pb, Sr, four kinds of component concentrations of Mg, Ti are respectively: Pb:0.26mol/L, Sr:0.08mol/L, Mg:0.035mol/L, Ti:0.315mol/L.In the ITO slide sol system that at the uniform velocity (5cm/min) immersion has prepared, placed for 15 seconds, make the ITO slide be in steady state, promote (5cm/min) with identical speed then, until substrate liquid level is proposed all, seasoning in air then.Put into High Temperature Furnaces Heating Apparatus subsequently, under 550 ℃ of temperature, carry out rapid thermal process 5min, after the cooling, repeat aforesaid operations and prepare multilayer film.Multilayer film thermal treatment 1h under 600 ℃ of temperature with preparation obtains uhligite phase PSMT film.Its XRD curve is seen accompanying drawing 1 (b), as seen from the figure, can generate the adulterated strontium lead titanate film of magnesium under this example condition.Specific inductivity and dielectric loss are seen accompanying drawing 2 during its 10kHz, and its dielectric adjustable is seen accompanying drawing 3.Generate under this example condition mix magnesium strontium lead titanate film 10kHz the time dielectric adjustable be 35%.
Embodiment 3: one
Plumbic acetate, Strontium carbonate powder, magnesiumcarbonate add small quantity of deionized water and dissolve in acetic acid, and reacting by heating obtains colourless transparent solution; Butyl (tetra) titanate dissolves in ethylene glycol monomethyl ether, is stirred to mix.Two kinds of solution are mixed, obtain Pb-Sr-Mg-Ti precursor colloidal sol, wherein Pb, Sr, four kinds of component concentrations of Mg, Ti are respectively: Pb:0.24mol/L, Sr:0.10mol/L, Mg:0.035mol/L, Ti:0.315mol/L.In the Si substrate sol system that at the uniform velocity (5cm/min) immersion has prepared, placed for 12 seconds, make the Si substrate be in steady state, promote (5cm/min) with identical speed then, until substrate liquid level is proposed all, seasoning in air then.Put into High Temperature Furnaces Heating Apparatus subsequently, under 580 ℃ of temperature, carry out rapid thermal process 5min, after the cooling, repeat aforesaid operations and prepare multilayer film.Multilayer film thermal treatment 1h under 600 ℃ of temperature with preparation obtains uhligite phase PSMT film.Can generate the adulterated strontium lead titanate film of magnesium under this example condition.Dielectric adjustable is 40% during its 10kHz.
Embodiment 4:
Plumbic acetate, Strontium carbonate powder, magnesiumcarbonate add small quantity of deionized water and dissolve in acetic acid, and reacting by heating obtains colourless transparent solution; Butyl (tetra) titanate dissolves in ethylene glycol monomethyl ether, is stirred to mix.Two kinds of solution are mixed, obtain Pb-Sr-Mg-Ti precursor colloidal sol, wherein Pb, Sr, four kinds of component concentrations of Mg, Ti are respectively: Pb:0.245mol/L, Sr:0.105mol/L, Mg:0.07mol/L, Ti:0.28mol/L.In the quartz base plate sol system that at the uniform velocity (3cm/min) immersion has prepared, placed for 10 seconds, make quartz base plate be in steady state, promote (3cm/min) with identical speed then, until substrate liquid level is proposed all, seasoning in air then.Put into High Temperature Furnaces Heating Apparatus subsequently, under 600 ℃ of temperature, carry out rapid thermal process 5min, after the cooling, repeat aforesaid operations and prepare multilayer film.Multilayer film thermal treatment 1h under 600 ℃ of temperature with preparation obtains uhligite phase PSMT film.Its XRD curve is seen accompanying drawing 1 (c), as seen from the figure, can generate the adulterated strontium lead titanate film of magnesium under this example condition, and its crystal content is close with pure PST film.Specific inductivity and dielectric loss are seen accompanying drawing 2 during its 10kHz, and its dielectric adjustable is seen accompanying drawing 3.Generate under this example condition mix magnesium strontium lead titanate film 10kHz the time dielectric adjustable be 63%.As calculated, its figure of merit is that Mg content is 0.1 o'clock 3 times of strontium lead titanate film.
Embodiment 5:
Plumbic acetate, Strontium carbonate powder, magnesiumcarbonate add small quantity of deionized water and dissolve in acetic acid, and reacting by heating obtains colourless transparent solution; Butyl (tetra) titanate dissolves in ethylene glycol monomethyl ether, is stirred to mix.Two kinds of solution are mixed, obtain Pb-Sr-Mg-Ti precursor colloidal sol, wherein Pb, Sr, four kinds of component concentrations of Mg, Ti are respectively: Pb:0.245mol/L, Sr:0.105mol/L, Mg:0.07mol/L, Ti:0.28mol/L.In the quartz base plate sol system that at the uniform velocity (4cm/min) immersion has prepared, placed for 10 seconds, make quartz base plate be in steady state, promote (4cm/min) with identical speed then, until substrate liquid level is proposed all, seasoning in air then.Put into High Temperature Furnaces Heating Apparatus subsequently, under 570 ℃ of temperature, carry out rapid thermal process 5min, after the cooling, repeat aforesaid operations and prepare multilayer film.Multilayer film thermal treatment 1h under 600 ℃ of temperature with preparation obtains uhligite phase PSMT film.Can generate the adulterated strontium lead titanate film of magnesium under this example condition, its crystal content is close with pure PST film.The dielectric adjustable of magnesium strontium lead titanate film when 10kHz of mixing that generates under this example condition is 60%.
Embodiment 6:
Plumbic acetate, Strontium carbonate powder, magnesiumcarbonate add small quantity of deionized water and dissolve in acetic acid, and reacting by heating obtains colourless transparent solution; Butyl (tetra) titanate dissolves in ethylene glycol monomethyl ether, is stirred to mix.Two kinds of solution are mixed, obtain Pb-Sr-Mg-Ti precursor colloidal sol, wherein Pb, Sr, four kinds of component concentrations of Mg, Ti are respectively: Pb:0.245mol/L, Sr:0.105mol/L, Mg:0.105mol/L, Ti:0.245mol/L.In the Si substrate sol system that at the uniform velocity (4cm/min) immersion has prepared, placed for 10 seconds, make the Si substrate be in steady state, promote (4cm/min) with identical speed then, until substrate liquid level is proposed all, seasoning in air then.Put into High Temperature Furnaces Heating Apparatus subsequently, under 600 ℃ of temperature, carry out rapid thermal process 5min, after the cooling, repeat aforesaid operations and prepare multilayer film.Multilayer film thermal treatment 1h under 600 ℃ of temperature with preparation obtains uhligite phase PSMT film.Its XRD curve is seen accompanying drawing 1 (d), as seen from the figure, can generate the adulterated strontium lead titanate film of magnesium under this example condition, and its crystal content is slightly higher than pure PST film.Specific inductivity and dielectric loss are seen accompanying drawing 2 during its 10kHz, and dielectric adjustable is seen accompanying drawing 3.Generate under this example condition mix magnesium strontium lead titanate film 10kHz the time dielectric adjustable be 58%.
Embodiment 7:
Plumbic acetate, Strontium carbonate powder, magnesiumcarbonate add small quantity of deionized water and dissolve in acetic acid, and reacting by heating obtains colourless transparent solution; Butyl (tetra) titanate dissolves in ethylene glycol monomethyl ether, is stirred to mix.Two kinds of solution are mixed, obtain Pb-Sr-Mg-Ti precursor colloidal sol, wherein Pb, Sr, four kinds of component concentrations of Mg, Ti are respectively: Pb:0.245mol/L, Sr:0.105mol/L, Mg:0.105mol/L, Ti:0.245mol/L.In the ito substrate sol system that at the uniform velocity (3cm/min) immersion has prepared, placed for 10 seconds, make ito substrate be in steady state, promote (3cm/min) with identical speed then, until substrate liquid level is proposed all, seasoning in air then.Put into High Temperature Furnaces Heating Apparatus subsequently, under 560 ℃ of temperature, carry out rapid thermal process 5min, after the cooling, repeat aforesaid operations and prepare multilayer film.Multilayer film thermal treatment 0.5h under 600 ℃ of temperature with preparation.Can generate the adulterated strontium lead titanate film of magnesium under this example condition, its crystal content is slightly higher than pure PST film.Its dielectric adjustable when 10kHz is 45%.
Claims (4)
1. the preparation method of a highly magnesium-doped strontium plumbum titanate high dielectric adjustable film material is characterized in that the step of this method is as follows:
1) plumbic acetate, Strontium carbonate powder, magnesiumcarbonate adding deionized water dissolve in acetic acid, and reacting by heating under 40 ℃～60 ℃ temperature obtains the solution first;
2) butyl (tetra) titanate dissolves in ethylene glycol monomethyl ether, is stirred to mix, and obtains solution second;
3) two kinds of solution of first, second mix, the concentration of controlling wherein Pb, Sr, Mg, four kinds of elementary compositions of Ti is respectively: Pb:0.22mol/L～0.26mol/L, Sr:0.08mol/L～0.12mol/L, Mg:0.035mol/L～0.105mol/L, Ti:0.245mol/L～0.35mol/L, stir, obtain precursor colloidal sol;
4) adopt the precursor colloidal sol of having prepared, at the uniform velocity all immerse substrate 3～5cm/min in the sol system that has prepared, placed for 10～15 seconds, promote with identical speed then, all propose liquid level until substrate, seasoning in air is then put into High Temperature Furnaces Heating Apparatus subsequently and is heat-treated at 550 ℃～600 ℃, after the cooling, repeat aforesaid operations and prepare the 6-8 layer film;
5), obtain mixing the strontium lead titanate film of magnesium 15%～30% with multilayer film thermal treatment 0.5h～1h under 550 ℃～600 ℃ temperature of preparation.
2. the preparation method of highly magnesium-doped strontium plumbum titanate high dielectric adjustable film material according to claim 1, it is characterized in that: described substrate is a glass substrate.
3. the preparation method of highly magnesium-doped strontium plumbum titanate high dielectric adjustable film material according to claim 1, it is characterized in that: described substrate is ito substrate, quartz base plate or Si substrate.
4. the preparation method of highly magnesium-doped strontium plumbum titanate high dielectric adjustable film material according to claim 1, it is characterized in that: the crystalline phase of described strontium lead titanate film is the uhligite phase, its crystal content is 80%～90%.
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| CN102176355B (en) * | 2011-01-22 | 2013-05-22 | 浙江大学 | Nano Ag particle-(Pb0.4Sr0.6)TiO3 solid solution seepage-type composite ceramic film and preparation method thereof |
| CN102514260B (en) * | 2011-12-03 | 2014-09-03 | 三峡大学 | Sol-gel preparation method of strontium titanate lead thin film |
| CN109180179B (en) * | 2018-10-17 | 2021-08-17 | 吕梁学院 | Magnesium-doped strontium titanate ceramic powder and preparation method and application thereof |
Citations (2)
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| CN1776011A (en) * | 2005-12-05 | 2006-05-24 | 武汉大学 | PST[(pB, sR)tIo3] and its Ba solution, Mg/Mn/K doping material system preparing method |
| CN1789198A (en) * | 2004-12-15 | 2006-06-21 | 同济大学 | Ferroelectric membrane with constituents graded distribution and its preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1789198A (en) * | 2004-12-15 | 2006-06-21 | 同济大学 | Ferroelectric membrane with constituents graded distribution and its preparation method |
| CN1776011A (en) * | 2005-12-05 | 2006-05-24 | 武汉大学 | PST[(pB, sR)tIo3] and its Ba solution, Mg/Mn/K doping material system preparing method |
Non-Patent Citations (3)
| Title |
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| Mg掺杂PST薄膜的溶胶-凝胶法制备及晶相形成研究. 杜丕一.物理学报，第54卷第11期. 2005 * |
| 溶胶-凝胶法制备钛酸锶铅薄膜和多层膜及其介电性质. 王季魁.功能材料，第37卷第2期. 2006 * |
| 热处理对sol-gel法Pb0.4Sr0.6TiO3薄膜形成影响的研究. 刘远良.无机材料学报，第20卷第1期. 2005 * |
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