CN101230450A - Method for preparing textured barium strontium titanate dielectric ceramic film by radio frequency sputtering - Google Patents
Method for preparing textured barium strontium titanate dielectric ceramic film by radio frequency sputtering Download PDFInfo
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- CN101230450A CN101230450A CNA2007101208721A CN200710120872A CN101230450A CN 101230450 A CN101230450 A CN 101230450A CN A2007101208721 A CNA2007101208721 A CN A2007101208721A CN 200710120872 A CN200710120872 A CN 200710120872A CN 101230450 A CN101230450 A CN 101230450A
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Abstract
The invention relates to a method of preparing a textured BST dielectric ceramic film through radio frequency sputtering. Firstly, Pt with a thickness of 100 nm is deposited on the Si sheet after a standard RCA cleaning process through sputtering and then the platinum-plated Si sheet is annealed at a temperature of 200 to 500 DEG C in a tubular furnace for one hour to be used as a substrate. Later on, the BST ceramic target, which satisfies the chemical dosage ratio of Ba plus Sr is equal to 1, is pre-sputtered for 24 hours and then a dielectric ceramic film with a thickness of 220 nm is deposited through radio frequency sputtering under the conditions that Ar:O2 is equal to 1.5 to 1, the total pressure is 10 to 100m Torrs, the temperature of the underlay is 550 to 700 DEG C and the distance between the target and the substrate is 40 to 80 mm. After the sputtering is finished, the BST dielectric ceramic film is slowly cooled to reach the room temperature under an oxygen atmosphere with a total pressure of 2*103 to 5*104 Pa. The dielectric ceramic film prepared in the invention has an adjustability of approximately 50 percent under a DC electric field, a dielectric constant as large as 680, a dielectric loss of 1.5 percent and merely an order of magnitude of 10-8A/cm2 for the drain current at the room temperature under a field intensity of 450 kVs per centimeter.
Description
Technical field
The present invention relates to a kind of radio-frequency sputtering preparation (111) texture (Ba
xSr
1-x) TiO
3The method of dielectric ceramic film promptly by ceramic target, is optimized processing parameter, prepares (the Ba of (111) texture of single uhligite phase
xSr
1-x) TiO
3Dielectric ceramic film, the bst thin film of preparing have big high adjustability, specific inductivity, lower loss and low leakage current.
Background technology
Since 20th century the fifties, the perovskite typed ferroelectric sosoloid is the interested research objects of people always.BaTiO
3Be a kind of perovskite typed ferroelectrics of finding the earliest, be characterized in that specific inductivity is big, non-linear by force, tangible temperature, frequency dependence are arranged.SrTiO
3Stable performance, good insulating, temperature factor is little, dielectric loss is little, SrTiO
3Be a kind of tendency type ferroelectrics, calculate its Curie point T by thermodynamic argument
CFor about 3.0K.People replace BaTiO with the Sr atom usually
3In the Ba atom, form (Ba
xSr
1-xTiO
3) (BST).From the materialogy viewpoint analysis, BST is BaTiO
3And SrTiO
3Sosoloid, BT is different fully with the ST electrical properties, but BST sosoloid but has extraordinary electrical property, has the BT high-k concurrently, the constitutionally stable characteristics of low-dielectric loss and ST.Particularly when the ratio of Ba/Sr is bordering on 1, this material has under high specific inductivity, low dielectric loss and the room temperature good adjustability (adding under certain direct-current biasing, specific inductivity can change a lot) is arranged.Therefore, its thin-film material is selected to the responsive microwave device of high frequency, for example: vibrator, phase shifter, retarding line, antenna and adjustability wave filter etc.In addition, ferroelectric barium strontium titanate is as a kind of novel dielectric materials, on dynamic RAM (DRAM), have extraordinary application prospect, reason is the ratio by choose reasonable Ba/Sr, can make material satisfy working conditions in room temperature range, and can possess desired different character simultaneously; And possessing relatively low leakage current and high specific inductivity simultaneously, this has just in time satisfied the advantage of DRAM to the electric capacity dielectric materials.BST has been considered to develop the important materials of super large-scale integration dynamic RAM of future generation (ULSIDRAM).Just because of its superior dielectric/ferroelectric properties, the research of strontium-barium titanate material and application and development become one of hot issue that everybody competitively contends.Referring to [1] H.N.Lee, D.Hesse, N.Zakharov, and U.G sele, Science (science) 296,2006 (2002) .[2] C.H.Ahn, K.M.Rabe, and J.-M.Triscone, Science (science) 303,488 (2004) .[3] J.Im, O.Auciello, P.K.Baumann, S.K.Streiffer, D.Y.Kaufman, and A.R.Krauss, Applied Physics Letters (Applied Physics wall bulletin) 76,625 (2000) .[4] A.I.Kingon, J.-P.Maria, S.K.Streiffer, Nature (nature) 406,1032 (2000).
(Ba
xSr
1-x) TiO
3Be to be studied more typical case's representative in this type of material.Present many study group are all in research, in different single crystalline substrate (such as LaAlO
3, MgO, Al
2O
3Deng) carry out the epitaxy bst thin film.In recent years, along with the breakthrough of ferroelectric membranc technology of preparing, the research of thin-film material and film preparing technology has had significant progress, makes to prepare various ferroelectric membrancs easily and become possibility.And the performance of polycrystalline bst thin film can reach the advantage identical with epitaxial film to the greatest extent.Because the progress of semi-conductor integrated technology, integrated uhligite ferroelectric membranc has more and more attracted people's research sight line on single crystalline Si.For example: on single crystalline Si by technology such as buffer layer reach Si (100) go up the extension of growth (100) orientation or high orientation texture ferroelectric/dielectric film.Yet recently extension goes out the bst thin film of different orientation on the monocrystalline MgO of different orientation, and test-results shows that the bst thin film of (111) orientation has bigger advantage at the film than (100) orientation aspect the adjustable microwave device application.[5] S.E.Moon, E.-K.Kim, M.-H.Kwak, H.-C.Ryu, Y.-T.Kim, K.-Y.Kang, S.-J.Lee, and W.-J.Kim, Applied Physics Letters (Applied Physics wall bulletin) 83,2166 (2003).
But because the semi-conductor development of integration technology, the ferroelectric membranc of integrated perovskite structure has attracted people's research sight line more and more on single crystalline Si.Yet, be on single crystalline Si, seldom to make the bst thin film of growth (111) orientation up till now.The method that relates among the present invention not only can be prepared the bst thin film of (111) orientation on single crystalline Si, and this ferroelectric membranc has nearly 50% adjustability under DC electric field, and specific inductivity reaches more than 680, and dielectric loss only is 1.5%.Simultaneously, at room temperature, leakage current only is 10 under the field intensity of 450kV/cm
-8A/cm
2The order of magnitude.
Summary of the invention
The present invention is on the basis of traditional magnetron sputtering, by to target spacing, sputtering power, parameter such as sputtering atmosphere, air pressure is carried out refined control and adjustment, integrating on the Si monocrystalline and satisfy chemical dosage ratio, is (111) orientation fully, and (the Ba with excellent electrical
xSr
1-x) TiO
3Ferroelectric membranc.Advantage of the present invention can integratedly go out to have the bst thin film of advantage (111) orientation aspect microwave device on silicon single crystal, method is reliable, good reproducibility.
The objective of the invention is: utilize traditional magnetron sputtering technique,, on the Si monocrystalline, prepare and have excellent electrical, and be more suitable for the bst thin film of (111) orientation that microwave device uses by accurate control splash-proofing sputtering process parameter.
The object of the present invention is achieved like this: a kind of radio-frequency sputtering preparation (111) texture (Ba
xSr
1-x) TiO
3The method of dielectric ceramic film is characterized in that comprising the following steps:
(1), will adopt the single crystalline Si sheet of RCA standard cleaning technology wash clean, put into sputtering equipment, the thick Pt of deposition 90-110nm, 200-500 ℃ of annealing 0.5-1.5 hour is with as substrate or directly plate Pt on the single crystalline Si substrate in tube furnace with platinized Si sheet subsequently, and the basic substrate of Si that applies of the Pt that obtains (111) orientation of anneal in 200-500 ℃ of air at room temperature the most finally deposits the substrate of bst thin film;
(2), in sputtering equipment, adopt the pre-sputter of radio frequency power to satisfy BST ceramic target 20-30 hour of chemical dosage ratio Ba+Sr=1;
(3), at Ar: O
2In the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature are 550-700 ℃, and the distance of target and substrate is under the condition of 40-80mm, adopt the thick (Ba of radio frequency sputtering method deposition 200-240nm
xSr
1-x) TiO
3Dielectric ceramic film after sputter finishes, is 2 * 10 at stagnation pressure
3-5 * 10
4Slow cool to room temperature under the oxygen atmosphere of Pa.
Radio-frequency sputtering preparation (111) texture (Ba
xSr
1-x) TiO
3The method of dielectric ceramic film, preferred steps is:
(1), will adopt the single crystalline Si sheet of RCA standard cleaning technology wash clean, put into sputtering equipment, Pt behind the deposition 95-105nm, 200-500 ℃ of annealing 0.75-1.2 hour is with as substrate or directly plate Pt on the single crystalline Si substrate in tube furnace with platinized Si sheet subsequently, and the basic substrate of Si that applies of the Pt that obtains (111) orientation of anneal in 200-500 ℃ of air at room temperature the most finally deposits the substrate of bst thin film;
(2), in sputtering equipment, adopt the pre-sputter of radio frequency power to satisfy BST ceramic target 22-26 hour of chemical dosage ratio Ba+Sr=1;
(3), at Ar: O
2In the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature are 550-700 ℃, and the distance of target and substrate is under the condition of 40-80mm, adopt the thick (Ba of radio frequency sputtering method deposition 210-230nm
xSr
1-x) TiO
3Dielectric ceramic film after sputter finishes, is 2 * 10 at stagnation pressure
3-5 * 10
4Slow cool to room temperature under the oxygen atmosphere of Pa.
Radio-frequency sputtering preparation (111) texture (Ba
xSr
1-x) TiO
3The method of dielectric ceramic film, preferred steps is:
(1), will adopt the single crystalline Si sheet of RCA standard cleaning technology wash clean, put into sputtering equipment, Pt behind the deposition 100nm, 200-500 ℃ of annealing 1 hour is with as substrate or directly plate Pt on the single crystalline Si substrate in tube furnace with platinized Si sheet subsequently, and the basic substrate of Si that applies of the Pt that obtains (111) orientation of anneal in 200-500 ℃ of air at room temperature the most finally deposits the substrate of bst thin film;
(2), in sputtering equipment, adopt the pre-sputter of radio frequency power to satisfy the BST ceramic target 24 hours of chemical dosage ratio Ba+Sr=1;
(3), at Ar: O
2In the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature are 550-700 ℃, and the distance of target and substrate is under the condition of 40-80mm, adopt the thick (Ba of radio frequency sputtering method deposition 220nm
xSr
1-x) TiO
3Dielectric ceramic film after sputter finishes, is 2 * 10 at stagnation pressure
3-5 * 10
4Slow cool to room temperature under the oxygen atmosphere of Pa.
The making method of described ceramic target comprises the following steps:
(1), according to stoichiometric ratio weighing purity is 99.9% BaTiO
3And SrTiO
3(mol ratio is Ba+Sr=1) powder adds an amount of ethanol or acetone in the mixture of two kinds of powder, carry out ball milling then, and rotating speed is 100-250 rev/min, time 18-24 hour, makes two kinds of powder mixes even;
(2), the mixed powder of gained in the step (1) is carried out drying treatment, 1100 ℃ presintering 4-6 hour, make BaTiO
3And SrTiO
3Form (Ba
xSr
1-x) TiO
3Sosoloid, the powder that pre-burning is obtained grinds with mortar, and adds adhesive polyethylene alcohol, drying, and cross 80 or 100 eye mesh screens;
(3), adopt the powder compression flakiness of the pressure of 10-35Mpa with above-mentioned steps (2), diameter is 72 millimeters, thickness is the thin slice of 3-5 millimeter, and the powder that pre-burning obtains is put into Al
2O
3Crucible is put into the thin slice that suppresses, and with (Ba
xSr
1-x) TiO
3The solid solution powder cover sheet covers the ceramic crucible lid, subsequently crucible is put into retort furnace, slowly rise to 1400 ℃ with 2-5 ℃/minute temperature rise rate from room temperature, sintering 4-6 hour, reduce to room temperature with 2-5 ℃/minute rate of temperature fall again, obtain the BST ceramic target.
Characteristics of the present invention are: from crystalline structure, prepared BST ceramic membrane has single (111) preferred orientation, and electrical property is good, has nearly 50% adjustability under DC electric field, specific inductivity reaches more than 680, and dielectric loss only is about 1.5%.Simultaneously, this dielectric film at room temperature, leakage current only is 10 under the field intensity of 450kV/cm
-8A/cm
2The order of magnitude.Simultaneously, this inventive method method is reliable, and good reproducibility can be used to prepare the big area ceramic membrane.
Description of drawings
The present invention is further illustrated below in conjunction with accompanying drawing:
Fig. 1 is the XRD spectra of the bst thin film for preparing under the above-mentioned condition;
The relation curve of specific inductivity, dielectric loss and strength of electric field that Fig. 2 Agilent 4294A test obtains;
The curve of the leakage current performance that the table test of Fig. 3 Keithley 2400 sources obtains.
Embodiment
Embodiment 1: radio-frequency sputtering preparation (111) texture (Ba
xSr
1-x) TiO
3The method of dielectric ceramic film comprises the following steps:
The first step: at first according to stoichiometric ratio weighing high-purity (99.9%) BaTiO
3And SrTiO
3(mol ratio is Ba+Sr=1) powder adds ethanol in the mixture of two kinds of powder, carry out ball milling 100-250 rev/min, 18-24 hour, makes two kinds of powder mixes even.
Second step: with 1100 ℃ of presintering 4-6 of powder of the first step gained hours, add suitable binding agent, dry back 100 orders sieve.
The 3rd step: the pressure with 10-35Mpa becomes 72 millimeters of diameters with above-mentioned powder compression, the thin slice of thickness 3-5 millimeter.
The 4th step: put into airtight Al
2O
3Crucible, and bury with identical powder.
The 5th step: crucible is put into retort furnace, slowly rise to 1400 ℃ from room temperature with 2-5 ℃/minute temperature rise rate, sintering 4-6 hour, reduce to room temperature with 2-5 ℃/minute rate of temperature fall again, obtain the BST ceramic target.
The 6th step: will adopt the single crystalline Si sheet of RCA standard cleaning technology wash clean, and put into sputtering equipment, the thick Pt of deposition 105nm.
The 7th step: with platinized Si sheet in tube furnace 200-500 ℃ of annealing 1.1 hours with as substrate material.
The 8th step: in sputtering equipment, adopt the pre-sputter of radio frequency power to satisfy the BST ceramic target 25 hours of chemical dosage ratio Ba+Sr=1;
The 9th step: in Ar: O2 was the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature were 550-700 ℃, and the distance of target and substrate is under the condition of 40-80mm, adopted the thick (Ba of radio frequency sputtering method deposition 210nm
xSr
1-x) TiO
3Dielectric ceramic film is 2 * 10 at stagnation pressure
3-5 * 10
4The slow cool to room temperature of bst thin film that sputter is good under the oxygen atmosphere of Pa.
Embodiment 2: radio-frequency sputtering preparation (111) texture (Ba
xSr
1-x) TiO
3The method of dielectric ceramic film comprises the following steps:
The first step: at first according to stoichiometric ratio weighing high-purity (99.9%) BaTiO
3And SrTiO
3(mol ratio is Ba+Sr=1) powder adds certain acetone in the mixture of two kinds of powder, carry out ball milling, rotational speed of ball-mill 100-250 rev/min, time 18-24 hour, makes two kinds of powder mixes even.
Second step: with 1100 ℃ of presintering 4-6 of powder of the first step gained hours, add suitable binding agent, dry back 80 or 100 orders sieve.
The 3rd step: the pressure with 10-35Mpa becomes 72 millimeters of diameters with above-mentioned powder compression, the thin slice of thickness 3-5 millimeter.
The 4th step: put into airtight Al
2O
3Crucible, and bury with identical powder.
The 5th step: crucible is put into retort furnace, slowly rise to 1400 ℃ from room temperature with 2-5 ℃/minute temperature rise rate, sintering 4-6 hour, reduce to room temperature with 2-5 ℃/minute rate of temperature fall again, obtain the BST ceramic target.
The 6th step: will adopt the single crystalline Si sheet of RCA standard cleaning technology wash clean, and put into sputtering equipment, the thick Pt of deposition 100nm.
The 7th step: with platinized Si sheet in tube furnace 200-500 ℃ of annealing 1 hour with as substrate material.
The 8th step: in sputtering equipment, adopt the pre-sputter of radio frequency power to satisfy the BST ceramic target 24 hours of chemical dosage ratio Ba+Sr=1;
The 9th step: in Ar: O2 was the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature were 550-700 ℃, and the distance of target and substrate is under the condition of 40-80mm, adopted the thick (Ba of radio frequency sputtering method deposition 220nm
xSr
1-x) TiO
3Dielectric ceramic film is 2 * 10 at stagnation pressure
3-5 * 10
4The slow cool to room temperature of bst thin film that sputter is good under the oxygen atmosphere of Pa.
Embodiment 3: radio-frequency sputtering preparation (111) texture (Ba
xSr
1-x) TiO
3The method of dielectric ceramic film comprises the following steps:
The first step: at first according to stoichiometric ratio weighing high-purity (99.9%) BaTiO
3And SrTiO
3(mol ratio is Ba+Sr=1) powder adds ethanol in the mixture of two kinds of powder, carry out ball milling, and rotational speed of ball-mill is 100-250 rev/min, time 18-24 hour, makes two kinds of powder mixes even.
Second step: with 1100 ℃ of presintering 4-6 of powder of the first step gained hours, add suitable binding agent, dry back 100 orders sieve.
The 3rd step: the pressure with 10-35Mpa becomes 72 millimeters of diameters with above-mentioned powder compression, the thin slice of thickness 3-5 millimeter.
The 4th step: put into airtight Al
2O
3Crucible, and bury with identical powder.
The 5th step: crucible is put into retort furnace, slowly rise to 1400 ℃ from room temperature with 2-5 ℃/minute temperature rise rate, sintering 4-6 hour, reduce to room temperature with 2-5 ℃/minute rate of temperature fall again, obtain the BST ceramic target.
The 6th step: will adopt the single crystalline Si sheet of RCA standard cleaning technology wash clean, and put into sputtering equipment, the thick Pt of deposition 90nm.
The 7th step: with platinized Si sheet in tube furnace 200-500 ℃ of annealing 0.9 hour with as substrate material.
The 8th step: the 8th step: in sputtering equipment, adopt the pre-sputter of radio frequency power to satisfy the BST ceramic target 26 hours of chemical dosage ratio Ba+Sr=1.
The 9th step: in Ar: O2 was the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature were 550-700 ℃, and the distance of target and substrate is under the condition of 40-80mm, adopted the thick (Ba of radio frequency sputtering method deposition 225nm
xSr
1-x) TiO
3Dielectric ceramic film is 2 * 10 at stagnation pressure
3-5 * 10
4The slow cool to room temperature of bst thin film that sputter is good under the oxygen atmosphere of Pa.
In the inventive method, through different underlayer temperatures, the film that different sputtering pressures obtains has different orientations and different compositions, and represents different character.The result shows, only under certain underlayer temperature (550-700 ℃), sputtering pressure under 40-60Pa, the electrical property excellence of the film that obtains, and all there are other orientations in the performance of the film that obtains under other conditions, and performance is undesirable.
Fig. 1 is the X ray diffracting spectrum of the bst thin film for preparing under the above-mentioned condition, and it illustrates that the bst thin film for preparing under this condition only has (111) orientation, and crystal property is good, and the impurity such as the silicide of Pt does not produce mutually.
Fig. 2 is the relation curve of the bst thin film specific inductivity, dielectric loss and the strength of electric field that prepare under the above-mentioned condition.As can be seen, this sample has good adjustability.Under the field intensity of 450kV/cm, has nearly 50% adjustability.Have specific inductivity under the null field and reach more than 680, and dielectric loss only is 1.5%.In our work, the bst thin film of other condition preparation does not have single orientation, and corresponding adjustability, specific inductivity are all little than the revise product, and dielectric loss data is bigger than this sample.
To be log (J) transform the relation of 1og (E) for the curve of the bst thin film leakage current performance for preparing under the above-mentioned condition during Fig. 3, illustration wherein, as can be seen sample satisfy the space charge limited current theory, and under the field intensity of 450kV/cm, leakage current only is 10
-8A/cm
2The order of magnitude.
More than the explanation of several aspects, on traditional sputtering technology basis, through strict control process parameters (underlayer temperature, target spacing, sputtering power, sputtering atmosphere, sputtering pressure etc.), the uhligite BST dielectric film that can be had (111) orientation, and prepared film has good electrical property.Corresponding best sputter deposition craft condition is Ar: O
2In the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature are 550-700 ℃, and the distance of target and substrate is 40-80mm.
Claims (4)
1. a radio-frequency sputtering prepares (111) texture (Ba
xSr
1-x) TiO
3The method of dielectric ceramic film is characterized in that comprising the following steps:
(1), will adopt the single crystalline Si sheet of RCA standard cleaning technology wash clean, put into sputtering equipment, the thick Pt of deposition 90-110nm, 200-500 ℃ of annealing 0.5-1.5 hour is with as substrate or directly plate Pt on the single crystalline Si substrate in tube furnace with platinized Si sheet subsequently, and the basic substrate of Si that applies of the Pt that obtains (111) orientation of anneal in 200-500 ℃ of air at room temperature the most finally deposits the substrate of bst thin film;
(2), in sputtering equipment, adopt the pre-sputter of radio frequency power to satisfy BST ceramic target 20-30 hour of chemical dosage ratio Ba+Sr=1;
(3), at Ar: O
2In the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature are 550-700 ℃, and the distance of target and substrate is under the condition of 40-80mm, adopt the thick (Ba of radio frequency sputtering method deposition 200-240nm
xSr
1-x) TiO
3Dielectric ceramic film after sputter finishes, is 2 * 10 at stagnation pressure
3-5 * 10
4Slow cool to room temperature under the oxygen atmosphere of Pa.
2. radio-frequency sputtering preparation (111) texture (Ba according to claim 1
xSr
1-x) TiO
3The method of dielectric ceramic film is characterized in that:
(1), will adopt the single crystalline Si sheet of RCA standard cleaning technology wash clean, put into sputtering equipment, the thick Pt of deposition 95-105nm, 200-500 ℃ of annealing 0.75-1.2 hour is with as substrate or directly plate Pt on the single crystalline Si substrate in tube furnace with platinized Si sheet subsequently, and the basic substrate of Si that applies of the Pt that obtains (111) orientation of anneal in 200-500 ℃ of air at room temperature the most finally deposits the substrate of bst thin film;
(2), in sputtering equipment, adopt the pre-sputter of radio frequency power to satisfy BST ceramic target 22-26 hour of chemical dosage ratio Ba+Sr=1;
(3), at Ar: O
2In the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature are 550-700 ℃, and the distance of target and substrate is under the condition of 40-80mm, adopt the thick (Ba of radio frequency sputtering method deposition 210-230nm
xSr
1-x) TiO
3Dielectric ceramic film after sputter finishes, is 2 * 10 at stagnation pressure
3-5 * 10
4Slow cool to room temperature under the oxygen atmosphere of Pa.
3. radio-frequency sputtering preparation (111) texture (Ba according to claim 1 and 2
xSr
1-x) TiO
3The method of dielectric ceramic film is characterized in that:
(1), will adopt the single crystalline Si sheet of RCA standard cleaning technology wash clean, put into sputtering equipment, Pt behind the deposition 100nm, 200-500 ℃ of annealing 1 hour is with as substrate or directly plate Pt on the single crystalline Si substrate in tube furnace with platinized Si sheet subsequently, and the basic substrate of Si that applies of the Pt that obtains (111) orientation of anneal in 200-500 ℃ of air at room temperature the most finally deposits the substrate of bst thin film;
(2), in sputtering equipment, adopt the pre-sputter of radio frequency power to satisfy the BST ceramic target 24 hours of chemical dosage ratio Ba+Sr=1;
(3), at Ar: O
2In the 1.5-1 scope, stagnation pressure 10-100mTorr, underlayer temperature are 550-700 ℃, and the distance of target and substrate is under the condition of 40-80mm, adopt the thick (Ba of radio frequency sputtering method deposition 220nm
xSr
1-x) TiO
3Dielectric ceramic film after sputter finishes, is 2 * 10 at stagnation pressure
3-5 * 10
4Slow cool to room temperature under the oxygen atmosphere of Pa.
4. radio-frequency sputtering preparation (111) texture (Ba according to claim 1 and 2
xSr
1-x) TiO
3The method of dielectric ceramic film is characterized in that the making method of described ceramic target comprises the following steps:
(1), according to stoichiometric ratio weighing purity is 99.9% BaTiO
3And SrTiO
3(mol ratio is Ba+Sr=1) powder adds an amount of ethanol or acetone in the mixture of two kinds of powder, carry out ball milling then, and rotating speed is 100-250 rev/min, time 18-24 hour, makes two kinds of powder mixes even;
(2), the mixed powder of gained in the step (1) is carried out drying treatment, 1100 ℃ presintering 4-6 hour, make BaTiO
3And SrTiO
3Form (Ba
xSr
1-x) TiO
3Sosoloid, the powder that pre-burning is obtained grinds with mortar, and adds adhesive polyethylene alcohol, drying, and cross 80 or 100 eye mesh screens;
(3), adopt the powder compression flakiness of the pressure of 10-35Mpa with above-mentioned steps (2), diameter is 72 millimeters, thickness is the thin slice of 3-5 millimeter, and the powder that pre-burning obtains is put into Al
2O
3Crucible is put into the thin slice that suppresses, and with (Ba
xSr
1-x) TiO
3The solid solution powder cover sheet covers the ceramic crucible lid, subsequently crucible is put into retort furnace, slowly rise to 1400 ℃ with 2-5 ℃/minute temperature rise rate from room temperature, sintering 4-6 hour, reduce to room temperature with 2-5 ℃/minute rate of temperature fall again, obtain the BST ceramic target.
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|---|---|---|---|---|
| CN102634836A (en) * | 2011-11-29 | 2012-08-15 | 沈阳理工大学 | Method for preparing metal-based composite ceramic coating on surface of titanium alloy |
| CN104134541A (en) * | 2014-05-30 | 2014-11-05 | 天津大学 | Full-transparent film voltage controlled varactor and preparation method thereof |
| CN111138187A (en) * | 2020-01-08 | 2020-05-12 | 西北工业大学 | Barium strontium titanate textured ceramic formed by water-based gel tape casting and preparation method thereof |
| WO2023005008A1 (en) * | 2021-07-26 | 2023-02-02 | 西安交通大学 | Low-dielectric constant high-entropy film and preparation method therefor |
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