CN104134542B - A kind of microwave ferro-electricity compound film capacitor and preparation method thereof - Google Patents
A kind of microwave ferro-electricity compound film capacitor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of microwave ferro-electricity compound film capacitor, which is with monocrystal chip as substrate, with 13 type microwave ferro-electricity compound films as dielectric layer, with Pt, Au, Ag, Al, Cu, SrRuO or La0.5Sr0.5CoO3For the capacitor of the interdigital structure of electrode.The dielectric layer of microwave ferro-electricity compound film capacitor of the present invention（The BST laminated films of doping advanced low-k materials）With typical 13 type composite construction, compared with capacitor commonly with epitaxial BST thin films as dielectric layer, with considerably higher tuning rate and lower dielectric loss.The present invention discloses the preparation method of the capacitor, which is the method being co-deposited using magnetic control and pulse laser, 13 type laminated films are prepared in specific condition and specific deposition on substrate, then by the capacitor of interdigital structure is obtained using photoetching process and magnetic control device build, there is higher tuning rate and lower dielectric loss using the capacitor prepared by the method for the present invention.
Description
Technical field
The present invention relates to the preparation of ferroelectric thin film device, specifically a kind of microwave ferro-electricity compound film capacitor and its
Preparation method.
Background technology
Phase shifter is the device that can be adjusted to the phase place of ripple, is a kind of microwave device.For phased-array radar
Microwave phase shifter, is more crucial components and parts in phased array radar system, and which should possess, and switching speed is high, insertion loss
Low, power capacity is high, temperature stability is good, reciprocity is good, capability of resistance to radiation is strong, driving power is low, the little spy such as lightweight of size
Point.But, mainly have two classes currently used for the material for preparing the phase shifter：One class is the PIN diode type phase shifter, its ultimate principle
Be using PIN diode when just reverse-biased two states, connect or disconnect span line to realize electromagnetic wave signal phase shift work(
Energy.The PIN diode type phase shifter has very big advantage on overall dimensions and switch speed is prepared, but but there is microwave power
It is little, the shortcomings of insertion loss is big.Another kind of is ferrite phase shifter, and its ultimate principle is changed in waveguide by externally-applied magnetic field
Ferritic pcrmeability, so as to change the phase velocity of electromagnetic wave, finally obtains different phase-shift phases to realize phase shift function.Ferrite
Phase shifter has the advantages that insertion loss is low, microwave power big, phase shift degree is big, but while have exist complex structure, volume it is big and
It is heavy, the shortcomings of power consumption is big, response speed is slow, the on the one hand development trend of the inapplicable whole machine of hyundai electronicses " little, light, thin, smart ",
On the other hand, this kind of material relies primarily on external import, and the production and research and development of microwave device are subject to the serious system of material supply side
About.
Therefore, the electronic material that modern requirements, performance are good, make whole machine miniaturization is met in the urgent need to a kind of.Ask at this
In topic, ferroelectric thin-flim materials is because with good ferroelectricity, high dielectric property, piezoelectricity, pyroelectric and nonlinear optical properties
Etc., become the emphasis and focus of the research of microwave current device material.Application with regard to ferroelectric thin film on microwave device, mesh
Front research is concentrated mainly on BaTiO3(BT), (Ba, Sr) TiO3（BST）, Pb (Zr, Ti) O3（PZT）, (Pb, La) TiO3
（PLT）, (Pb, La) (Zr, Ti) O3（PLZT）, Ba (Zr, Ti) O3（BZT）Deng on.
More than in the ferroelectric thin-flim materials of all multiple types, barium strontium titanate（BaxSr1-xTiO3, abbreviation BST）In adjustable microwave
Device（Such as microwave ferroelectric phase shifter）Development in have huge application potential.BST is the solid solution of Barium metatitanate. and strontium titanates,
And Barium metatitanate. and strontium titanates can phase mixed phase completely it is molten.BST materials have excellent property, such as possess high dielectric constant,
Leakage current of the big thermoelectricity Changshu of low dielectric loss, high dielectric percentage modulation and very little etc., its outstanding feature the most is exactly
Its Curie temperature can be by adjusting the Ba/Sr compositions in material than realizing the effective control in the range of 100 ~ 400K, with full
The needs of the various application of foot.It is adjustable micro- with voltage can be prepared the characteristics of change in voltage using bst thin film dielectric constant
Wave device, such as phase shifter, variodenser, agitator, phased-array radar and adjustability wave filter etc., are especially suitable for preparing wide ripple
Section, adjustable microwave device, which has become key object of the people in microwave device research field.But, research is sent out simultaneously
Existing, bst thin film has larger dielectric loss and relatively low tuning rate at microwave frequencies, which limits bst thin film and exists
Application in terms of microwave device.
To solve this problem, the structure and performance that doping can be effectively improved bst thin film is attempted and demonstrated to researcher,
And it is known in bst thin film, during incorporation low-k oxide, effectively to suppress thin film internal flaw, reduce BST
The dielectric loss and leakage current density of thin film.And, by the doping for changing impurity in bst thin film, corresponding laminated film
Can be applied in the microwave device of different resonant frequencies.Additionally, it is known that the laminated film of low-k oxide and BST
There are three kinds of structure types：0-3,2-2,1-3 type.In the laminated film of these three structure types, although in theory at present
Foretell that 1-3 type low-k oxides and the laminated film of BST have more preferable microwave property, but with regard to prior art
Speech, the preparation of 1-3 type BST laminated films can especially change the preparation of the 1-3 type laminated films of rod diameter, remain pendulum
A difficult problem in face of researcher, and then also limit application of the 1-3 type laminated films in microwave device.
The content of the invention
An object of the present invention is to provide a kind of microwave ferro-electricity compound film capacitor, thin to solve existing use BST
The problem that capacitor tuning rate is low made by film, dielectric loss is high.
The second object of the present invention is to provide a kind of preparation method of microwave ferro-electricity compound film capacitor, to solve to adopt
Existing method cannot prepare the problem of the low microwave ferro-electricity compound film capacitor of tuning rate height, dielectric loss.
First purpose of the present invention is realized by following technical scheme：
A kind of microwave ferro-electricity compound film capacitor, the capacitor are answered with monocrystal chip as substrate, with microwave ferroelectricity
Conjunction thin film be dielectric layer, with Pt, Au, Ag, Al, Cu, SrRuO or La0.5Sr0.5CoO3For the capacitor of the interdigital structure of electrode；
The monocrystal chip is MgO monocrystal chips, LaAlO3Monocrystal chip, Al2O3Monocrystal chip, Si monocrystal chips or
SrTiO3Monocrystal chip；
The microwave ferro-electricity compound film is the 1-3 type laminated films in barium strontium titanate doped with MgO, and its thickness is
100~2000nm；Doping volume ratios of the MgO in the barium strontium titanate is 1 ﹕, 1 ~ 1 ﹕ 160；
The Ba/Sr ratios of the barium strontium titanate are 0.1 ﹕, 0.9 ~ 0.9 ﹕ 0.1.
Microwave ferro-electricity compound film capacitor of the present invention, the Ba/Sr ratios of the barium strontium titanate are 0.6 ﹕ 0.4.
Microwave ferro-electricity compound film capacitor of the present invention, doping volumes of the MgO in the barium strontium titanate
Than for 1 ﹕, 40 ~ 1 ﹕ 110.
Preferably, doping volume ratios of the MgO in the barium strontium titanate is 1 ﹕ 60.
Preferably, microwave ferro-electricity compound film capacitor of the present invention, the thickness of the microwave ferro-electricity compound film
For 200 ~ 1200nm；More preferably 800nm.
Preferably, the monocrystal chip is MgO (100) monocrystal chips or LaAlO3(100) monocrystal chip.
Second object of the present invention is realized by following technical scheme：
A kind of preparation method of microwave ferro-electricity compound film capacitor, which comprises the following steps：
A, the magnetic control target that A targets and B targets difference random installation are co-deposited vacuum installation in magnetic control and pulse laser
Position and laser target position；Substrate is carried out into cleaning treatment, is then bonded on sample carrier, be placed to magnetic control and pulse laser is co-deposited dress
Put on the sample stage of vacuum chamber；
Wherein, the B targets are high-purity barium strontium titanate targets of the Ba/Sr than 0.1 ﹕, 0.9 ~ 0.9 ﹕ 0.1；The A targets are
High-purity MgO target；The substrate is MgO monocrystal chips, LaAlO3Monocrystal chip, Al2O3Monocrystal chip, Si monocrystal chips or
SrTiO3Monocrystal chip；
B, the back end vacuum of vacuum chamber is adjusted to（0.01~100）×10-4Pa, then adjust magnetic control target spacing be 1 ~
10cm, laser target spacing are 1 ~ 10cm, then pass to argon/oxygen mixed gas that flow is 5 ~ 100sccm, and then setting is splashed
Condition is penetrated, growth over the substrate obtains the laminated film of 1-3 type structures；The growth thickness control of the laminated film exists
100~2000nm；
Argon in the argon/oxygen mixed gas: the volume ratio of oxygen is 1: 3 ~ 3: 1；
The sputtering condition is：Magnetron sputtering power be 0.1 ~ 100W, pulsed laser deposition power be 0.1 ~ 5W, pulse swash
Light frequency is 0.1 ~ 10Hz, and sputtering pressure is 1 ~ 100Pa, and growth temperature is 500 ~ 1000 DEG C；
Under the sputtering condition during growing mixed thin film, doping bodies of the MgO in the barium strontium titanate
Product is than control in 1 ﹕, 1 ~ 1 ﹕ 160；
C, on the laminated film of gained 1-3 type structures, make interdigital pattern first with photoetching process, then described
Pt, Au, Ag, Al, Cu, SrRuO or La are grown on interdigital pattern0.5Sr0.5CoO3Electrode, is finally peeled away pattern, and structure is pitched
Refer to the capacitor of structure.
Preferably, the preparation method of microwave ferro-electricity compound film capacitor of the present invention, in step b, splashes described
Under the conditions of penetrating during growing mixed thin film, doping volume ratios of the MgO in the barium strontium titanate is controlled in 1 ﹕, 40 ~ 1 ﹕
110, more preferably 1 ﹕ 60.
Preferably, the preparation method of microwave ferro-electricity compound film capacitor of the present invention, it is in step b, described compound
The growth thickness of thin film is controlled in 200 ~ 1200nm, more preferably 800nm.
The preparation method of microwave ferro-electricity compound film capacitor of the present invention, growth temperature described in step b are preferably
900℃。
The preparation method of microwave ferro-electricity compound film capacitor of the present invention, vacuum described in step b are 2 × 10- 4Pa, the magnetic control target spacing are 6.5cm, and the laser target spacing is 5cm, and the flow of the argon/oxygen mixed gas is
100sccm；
Argon in the argon/oxygen mixed gas: the volume ratio of oxygen is 3: 1；
The sputtering condition is specially：40 ~ 80W of magnetron sputtering power, pulsed laser deposition power 0.7W, pulse laser frequency
Rate 3Hz, sputtering pressure are maintained at 5Pa, and growth temperature is 900 DEG C.
The preparation method of microwave ferro-electricity compound film capacitor of the present invention, barium strontium titanate target described in step a
Ba/Sr ratios are 0.6 ﹕ 0.4.
A targets, in step a, are preferably installed by the preparation method of microwave ferro-electricity compound film capacitor of the present invention
In magnetic control target position, B targets are arranged on into laser target position.
The preparation method of microwave ferro-electricity compound film capacitor of the present invention, substrate described in step a are preferably MgO
(100) monocrystal chip or LaAlO3(100) monocrystal chip.
The preparation method of microwave ferro-electricity compound film capacitor of the present invention, the thickness of substrate described in step a are 0.1
~ 2mm, preferably 0.5mm.
Heretofore described A targets（I.e. described high-purity MgO target）, the B targets（I.e. described high-purity barium strontium titanate target
Material）For the target of purity ＞ 99.95%.
The dielectric layer of microwave ferro-electricity compound film capacitor of the present invention（The BST of doping advanced low-k materials is multiple
Close thin film）With typical 1-3 types composite construction, compared with capacitor commonly with epitaxial BST thin films as dielectric layer, with bright
Show higher tuning rate and lower dielectric loss.Microwave ferro-electricity compound film capacitor prepared by the inventive method, first
The method that is co-deposited using magnetic control and pulse laser is simultaneously grown in specific condition, specific substrate up and down and obtains 1-3 type structures
Low-k compound and BST composite film materials, then construct by photoetching process and magnetron sputtering technique interdigital
The capacitor of structure, has higher tuning rate and lower dielectric loss using the capacitor prepared by the method for the present invention.
Description of the drawings
Fig. 1 is the XRD figure of the 60 laminated film interdigitated capacitors of 1-3 type MgO ﹕ BST=1 ﹕ prepared by embodiment 1.
Fig. 2 is the XRD figure of the epitaxial BST thin films interdigitated capacitors prepared by comparative example 1.
Fig. 3 is the dielectric layer of the 60 laminated film interdigitated capacitors of 1-3 type MgO ﹕ BST=1 ﹕ prepared by embodiment 1（MgO ﹕
BST laminated films）TEM figure.
Fig. 4 is C-V the and D-V characteristic curve comparison diagrams of embodiment 1 and the interdigitated capacitors prepared by comparative example 1.
In Fig. 4,（a）C-V the and D-V characteristic curves of the interdigitated capacitors prepared by comparative example 1 are represented,（b）Represent and implement
C-V the and D-V characteristic curves of the interdigitated capacitors prepared by example 1.
Fig. 5 is C-V performance diagram of the 3 prepared two kinds of different doping of embodiment 2 and embodiment than interdigitated capacitors.
Fig. 6 is the LaAlO prepared by embodiment 43(100) the C-V performance diagrams of base interdigitated capacitors.
Fig. 7 is the C-V characteristics of the 60 laminated film interdigitated capacitors of reducing 1-3 type MgO ﹕ BST=1 ﹕ prepared by embodiment 5
Curve chart.
Fig. 8 is the dielectric layer of the plane-parallel capacitor prepared by embodiment 6（0-3 type MgO ﹕ BST laminated films）XRD
Figure.
Fig. 9 is the C-V performance diagrams of the plane-parallel capacitor prepared by embodiment 6.
Specific embodiment
For a better understanding of the present invention, below by several specific embodiments, the present invention will be further described, but not
Mean any restriction of the content of the invention to the present invention.
The preparation of 1 1-3 type MgO ﹕ BST=1 ﹕ of embodiment, 60 laminated film interdigitated capacitors
A, target prepare and substrate cleaning：A targets and B targets are separately mounted to into magnetic control and pulse laser is co-deposited device
Magnetic control target position and laser target position；Substrate is carried out into cleaning treatment：Routinely cleaning operation method, first by substrate successively in acetone
Cleaned with ultrasound wave 5 minutes with dehydrated alcohol respectively, then dried up with high pure nitrogen, to ensure the cleaning of substrate, so
Afterwards cleaned substrate is bonded on sample carrier, magnetic control is placed to and pulse laser is co-deposited on the sample stage of vacuum installation；
In this step, from high-purity MgO（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target as A targets,
From high-purity Ba0.6Sr0.4TiO3（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target is used as B targets；From
0.5mm thick MgO (100) monocrystal chip is used as substrate.
B, growth MgO ﹕ BST laminated films：The back end vacuum of vacuum chamber is set to into 2 × 10-4Pa, then adjusts magnetic control target
Spacing is 6.5cm, and laser target spacing is 5cm, then passes to the mixed gas of argon and oxygen that flow is 100sccm, then
Setting sputtering condition, grows MgO ﹕ BST laminated films on MgO (100) monocrystal chip；
In this step, argon flow amount is 75sccm, and the flow of oxygen is 25sccm；
In this step, specific sputtering condition is：Magnetron sputtering power is 60W, and pulsed laser deposition power is 0.7W, pulse
Laser frequency is 3Hz；During cosputtering, in vacuum room, sputtering pressure is 5Pa, and growth temperature is 900 DEG C；
By above-mentioned sputtering condition cosputtering 1h, you can the growth on MgO (100) monocrystal chip obtains thickness for 800nm
, MgO volume ratio is adulterated in BST for 1:60, the MgO ﹕ BST laminated films of 1-3 type structures.
C, 60 laminated film interdigitated capacitors of preparation 1-3 type MgO ﹕ BST=1 ﹕：It is on gained MgO ﹕ BST laminated films, first
Interdigital pattern is made first with photoetching process, then Pt electrodes is grown by magnetic control sputtering device, is finally peeled away pattern, so as to structure
Build the 1-3 types obtained with Pt as electrode, with MgO ﹕ BST laminated films as dielectric layer, with MgO (100) monocrystal chip as substrate
60 laminated film interdigitated capacitors of MgO ﹕ BST=1 ﹕.
The preparation of 1 epitaxial BST thin films interdigitated capacitors of comparative example
A, target prepare and substrate cleaning：By high-purity Ba0.6Sr0.4TiO3（Purity ＞ 99.95%, Beijing Tai Kenuo science and technology have
Limit company）Target is arranged on magnetic control and pulse laser is co-deposited the laser target position of device；Substrate is carried out into cleaning treatment：From
0.5mm thick MgO (100) monocrystal chips as substrate, routinely cleaning operation method, first by substrate successively in acetone and anhydrous
Cleaned with ultrasound wave 5 minutes in ethanol respectively, then dried up with high pure nitrogen, to ensure the cleaning of substrate, then will be clear
Washed substrate is bonded on sample carrier, is placed to magnetic control and pulse laser is co-deposited on the sample stage of vacuum installation.
B, growth epitaxial BST thin films：The back end vacuum of vacuum chamber is set to into 2 × 10-4Pa, then adjusts laser target spacing
For 5cm, the mixed gas of argon and oxygen that flow is 100sccm are then passed to, sputtering condition is then set, in MgO (100)
MgO ﹕ BST laminated films are grown on monocrystal chip；
In this step, argon flow amount is 75sccm, and the flow of oxygen is 25sccm；
In this step, specific sputtering condition is：Pulsed laser deposition power is 0.7W, and pulse laser frequency is 3Hz, sputtering
Air pressure is 5Pa, and growth temperature is 900 DEG C；
By above-mentioned sputtering condition sputtering 61min, you can the growth on MgO (100) monocrystal chip obtains thickness for 800nm
Epitaxial BST thin films.
C, prepare epitaxial BST thin films interdigitated capacitors：On gained epitaxial BST thin films, make first with photoetching process
Interdigital pattern, then grows Pt electrodes by magnetic control sputtering device, is finally peeled away pattern, so as to build obtain with Pt as electrode,
Epitaxial BST thin films interdigitated capacitors with epitaxial BST thin films as dielectric layer, with MgO (100) monocrystal chip as substrate.
X-ray diffraction is carried out to the 60 laminated film interdigitated capacitors of 1-3 type MgO ﹕ BST=1 ﹕ prepared by embodiment 1
（XRD）Analysis, as a result as shown in Figure 1；In addition, transmission electricity is carried out to 60 laminated films of MgO ﹕ BST=1 ﹕ prepared by embodiment 1
Mirror（TEM）Scanning, as a result as shown in Figure 3.
XRD analysis are carried out to the epitaxial BST thin films interdigitated capacitors prepared by comparative example 1, as a result as shown in Figure 2.
The MgO and BST that can be seen that by Fig. 1 and Fig. 3 in 1-3 type MgO ﹕ BST laminated films is epitaxial growth, and MgO
Nanometer rods even thickness, diameter are about 2nm.
As seen from Figure 2, the bst thin film prepared by comparative example 1 is epitaxial growth, is epitaxial BST thin films.
Fig. 4 gives embodiment 1 and the C-V characteristic curves and D-V characteristics of the interdigitated capacitors prepared by comparative example 1 are bent
Line, as can be seen from Figure, epitaxial BST thin films interdigitated capacitors tuning rate is only 30%, dielectric loss but up to 0.022, and
1-3 types MgO:BST laminated film interdigitated capacitors tuning rates are up to 40%, and dielectric loss is only 0.008.This result is fully demonstrate,proved
1-3 types MgO prepared by the clear method of the present invention:BST laminated films interdigitated capacitors have very strong microstructure feature and
Functional characteristic.
The preparation of 2 1-3 type MgO ﹕ BST=1 ﹕ of embodiment, 110 laminated film interdigitated capacitors
A, target prepare and substrate cleaning：A targets and B targets are separately mounted to into magnetic control and pulse laser is co-deposited device
Magnetic control target position and laser target position；Substrate is carried out into cleaning treatment：Routinely cleaning operation method, first by substrate successively in acetone
Cleaned with ultrasound wave 5 minutes with dehydrated alcohol respectively, then dried up with high pure nitrogen, to ensure the cleaning of substrate, so
Afterwards cleaned substrate is bonded on sample carrier, magnetic control is placed to and pulse laser is co-deposited on the sample stage of vacuum installation；
In this step, from high-purity MgO（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target as A targets,
From high-purity Ba0.6Sr0.4TiO3（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target is used as B targets；From
0.5mm thick MgO (100) monocrystal chip is used as substrate.
B, growth doping volume ratio are MgO ﹕ BST=1:110 laminated films：The back end vacuum of vacuum chamber is set to into 2 ×
10-4Pa, it is 6.5cm then to adjust magnetic control target spacing, and laser target spacing is 5cm, then pass to argon that flow is 100sccm and
The mixed gas of oxygen, then set sputtering condition, and MgO ﹕ BST laminated films are grown on MgO (100) monocrystal chip；
In this step, argon flow amount is 75sccm, and the flow of oxygen is 25sccm；
In this step, specific sputtering condition is：Magnetron sputtering power is 40W, and pulsed laser deposition power is 0.7W, pulse
Laser frequency is 3Hz；During cosputtering, in vacuum room, sputtering pressure is 5Pa, and growth temperature is 900 DEG C；
By above-mentioned sputtering condition cosputtering 1h, you can the growth on MgO (100) monocrystal chip obtains thickness for 800nm
, the doping volume ratio that MgO is in BST be 1:110, the MgO ﹕ BST laminated films of 1-3 type structures.
C, 110 laminated film interdigitated capacitors of preparation 1-3 type MgO ﹕ BST=1 ﹕：It is on gained MgO ﹕ BST laminated films, first
Interdigital pattern is made first with photoetching process, then Pt electrodes is grown by magnetic control sputtering device, is finally peeled away pattern, so as to structure
Build the 1-3 types obtained with Pt as electrode, with MgO ﹕ BST laminated films as dielectric layer, with MgO (100) monocrystal chip as substrate
110 laminated film interdigitated capacitors of MgO ﹕ BST=1 ﹕.
The preparation of 3 1-3 type MgO ﹕ BST=1 ﹕ of embodiment, 40 laminated film interdigitated capacitors
A, target prepare and substrate cleaning：A targets and B targets are separately mounted to into magnetic control and pulse laser is co-deposited device
Magnetic control target position and laser target position；Substrate is carried out into cleaning treatment：Routinely cleaning operation method, first by substrate successively in acetone
Cleaned with ultrasound wave 5 minutes with dehydrated alcohol respectively, then dried up with high pure nitrogen, to ensure the cleaning of substrate, so
Afterwards cleaned substrate is bonded on sample carrier, magnetic control is placed to and pulse laser is co-deposited on the sample stage of vacuum installation；
In this step, from high-purity MgO（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target as A targets,
From high-purity Ba0.6Sr0.4TiO3（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target is used as B targets；From
0.5mm thick MgO (100) monocrystal chip is used as substrate.
B, growth doping volume ratio are MgO ﹕ BST=1:40 laminated films：The back end vacuum of vacuum chamber is set to into 2 × 10- 4Pa, it is 6.5cm then to adjust magnetic control target spacing, and laser target spacing is 5cm, then passes to argon and oxygen that flow is 100sccm
The mixed gas of gas, then set sputtering condition, and MgO ﹕ BST laminated films are grown on MgO (100) monocrystal chip；
In this step, argon flow amount is 75sccm, and the flow of oxygen is 25sccm；
In this step, specific sputtering condition is：Magnetron sputtering power is 80W, and pulsed laser deposition power is 0.7W, pulse
Laser frequency is 3Hz；During cosputtering, in vacuum room, sputtering pressure is 5Pa, and growth temperature is 900 DEG C；
By above-mentioned sputtering condition cosputtering 1h, you can the growth on MgO (100) monocrystal chip obtains thickness for 800nm
, the doping volume ratio that MgO is in BST be 1:40, the MgO ﹕ BST laminated films of 1-3 type structures.
C, the different doping of preparation are than MgO ﹕ BST laminated film interdigitated capacitors：It is on gained MgO ﹕ BST laminated films, first
Interdigital pattern is made first with photoetching process, then Pt electrodes is grown by magnetic control sputtering device, is finally peeled away pattern, so as to structure
Build the 1-3 types obtained with Pt as electrode, with MgO ﹕ BST laminated films as dielectric layer, with MgO (100) monocrystal chip as substrate
MgO ﹕ BST laminated film interdigitated capacitors.
The C-V characteristic curves of the interdigitated capacitors by prepared by Fig. 5 gives embodiment 2 and embodiment 3, can be with by Fig. 5
Find out, the tuning rate of the 110 laminated film interdigitated capacitors of 1-3 type MgO ﹕ BST=1 ﹕ prepared by embodiment 2 is 34%, embodiment 3
The tuning rate of prepared 40 laminated film interdigitated capacitors of 1-3 type MgO ﹕ BST=1 ﹕ is 13%.
4 LaAlO of embodiment3The preparation of 60 laminated film interdigitated capacitors of base 1-3 type MgO ﹕ BST=1 ﹕
A, target prepare and substrate cleaning：A targets and B targets are separately mounted to into magnetic control and pulse laser is co-deposited device
Magnetic control target position and laser target position；Substrate is carried out into cleaning treatment：Routinely cleaning operation method, first by substrate successively in acetone
Cleaned with ultrasound wave 5 minutes with dehydrated alcohol respectively, then dried up with high pure nitrogen, to ensure the cleaning of substrate, so
Afterwards cleaned substrate is bonded on sample carrier, magnetic control is placed to and pulse laser is co-deposited on the sample stage of vacuum installation；
In this step, from high-purity MgO（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target as A targets,
From high-purity Ba0.6Sr0.4TiO3（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target is used as B targets；From
0.5mm thick LaAlO3(100) monocrystal chip is used as substrate.
B, growth MgO ﹕ BST laminated films：The back end vacuum of vacuum chamber is set to into 2 × 10-4Pa, then adjusts magnetic control target
Spacing is 6.5cm, and laser target spacing is 5cm, then passes to the mixed gas of argon and oxygen that flow is 100sccm, then
Setting sputtering condition, in LaAlO3(100) MgO ﹕ BST laminated films are grown on monocrystal chip；
In this step, argon flow amount is 75sccm, and the flow of oxygen is 25sccm；
In this step, specific sputtering condition is：Magnetron sputtering power is 60W, and pulsed laser deposition power is 0.7W, pulse
Laser frequency is 3Hz；During cosputtering, in vacuum room, sputtering pressure is 5Pa, and growth temperature is 900 DEG C；
By above-mentioned sputtering condition cosputtering 1h, you can in LaAlO3(100) on monocrystal chip, growth obtains thickness and is
800nm, MgO and BST volume ratio is 1:60, the MgO ﹕ BST laminated films of 1-3 type structures.
C, 60 laminated film interdigitated capacitors of preparation 1-3 type MgO ﹕ BST=1 ﹕：It is on gained MgO ﹕ BST laminated films, first
Interdigital pattern is made first with photoetching process, then Pt electrodes is grown by magnetic control sputtering device, is finally peeled away pattern, so as to structure
Build and obtain with Pt as electrode, with MgO ﹕ BST laminated films as dielectric layer, with LaAlO3(100) 1-3 type of the monocrystal chip for substrate
60 laminated film interdigitated capacitors of MgO ﹕ BST=1 ﹕.
Fig. 6 is the LaAlO prepared by embodiment 43(100) the C-V characteristic curves of base interdigitated capacitors, can be seen by Fig. 6
Go out, its tuning rate is 14%.
The preparation of 5 reducing 1-3 type MgO ﹕ BST=1 ﹕ of embodiment, 60 laminated film interdigitated capacitors
A, target prepare and substrate cleaning：A targets and B targets are separately mounted to into magnetic control and pulse laser is co-deposited device
Magnetic control target position and laser target position；Substrate is carried out into cleaning treatment：Routinely cleaning operation method, first by substrate successively in acetone
Cleaned with ultrasound wave 5 minutes with dehydrated alcohol respectively, then dried up with high pure nitrogen, to ensure the cleaning of substrate, so
Afterwards cleaned substrate is bonded on sample carrier, magnetic control is placed to and pulse laser is co-deposited on the sample stage of vacuum installation；
In this step, from high-purity MgO（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target as A targets,
From high-purity Ba0.6Sr0.4TiO3（Purity ＞ 99.95%, Beijing Technol Science Co., Ltd.）Target is used as B targets；From
0.5mm thick MgO (100) monocrystal chip is used as substrate.
B, growth MgO ﹕ BST laminated films：The back end vacuum of vacuum chamber is set to into 2 × 10-4Pa, then adjusts magnetic control target
Spacing is 6.5cm, and laser target spacing is 5cm, then passes to the mixed gas of argon and oxygen that flow is 100sccm, then
Setting sputtering condition, grows MgO ﹕ BST laminated films on MgO (100) monocrystal chip；
In this step, argon flow amount is 75sccm, and the flow of oxygen is 25sccm；
In this step, specific sputtering condition is：Magnetron sputtering is divided into three phases, is followed successively by respectively：Power 80W, sputtering
20min；Power 60W, sputters 20min；Power 40W, sputters 20min；Pulsed laser deposition power 0.7W, pulse laser frequency
3Hz, sputtering time 1h；During cosputtering, in vacuum room, sputtering pressure is 5Pa, and growth temperature is 900 DEG C；
Cosputtering is carried out by above-mentioned sputtering condition, you can the growth on MgO (100) monocrystal chip obtains thickness and is
800nm, MgO and BST volume ratio is 1:60, the MgO ﹕ BST laminated films of reducing 1-3 type structures.
C, prepare 60 laminated film interdigitated capacitors of reducing 1-3 type MgO ﹕ BST=1 ﹕：In gained MgO ﹕ BST laminated films
On, interdigital pattern is made first with photoetching process, then grow Pt electrodes by magnetic control sputtering device, be finally peeled away pattern,
So as to build the change obtained with Pt as electrode, with MgO ﹕ BST laminated films as dielectric layer, with MgO (100) monocrystal chip as substrate
60 laminated film interdigitated capacitors of footpath 1-3 type MgO ﹕ BST=1 ﹕.
Fig. 7 gives the C-V of the 60 laminated film interdigitated capacitors of reducing 1-3 type MgO ﹕ BST=1 ﹕ prepared by embodiment 5
Characteristic curve, as can be seen from Figure, reducing 1-3 types MgO:BST laminated film interdigitated capacitors tuning rate is 44%.This knot
Fruit is indicated by real-time control MgO incorporation, thus it is possible to vary the diameter of MgO nanometer rods, can further optimize laminated film
Performance.
The preparation of 6 0-3 type MgO ﹕ BST=1 ﹕ of embodiment, 60 laminated film plane-parallel capacitors
A, target prepare and substrate cleaning：A targets and B targets are separately mounted to into magnetic control and pulse laser is co-deposited device
Magnetic control target position and laser target position；Substrate is carried out into cleaning treatment：Routinely cleaning operation method, first by substrate successively in acetone
Cleaned with ultrasound wave 5 minutes with dehydrated alcohol respectively, then dried up with high pure nitrogen, to ensure the cleaning of substrate, so
Afterwards cleaned substrate is bonded on sample carrier, magnetic control is placed to and pulse laser is co-deposited on the sample stage of vacuum installation；
In this step, from high-purity MgO（Purity>99.95%, Beijing Technol Science Co., Ltd.）Target as A targets,
From high-purity Ba0.6Sr0.4TiO3（Purity>99.95%, Beijing Technol Science Co., Ltd.）Target is used as B targets；From
0.5mm thick Pt (111)/TiO2/SiO2/ Si (001) substrate is used as substrate.
B, growth MgO ﹕ BST laminated films：The back end vacuum of vacuum chamber is set to into 2 × 10-4Pa, then adjusts magnetic control target
Spacing is 6.5cm, and laser target spacing is 5cm, then passes to the mixed gas of argon and oxygen that flow is 100sccm, then
Setting sputtering condition, in Pt (111)/TiO2/SiO2MgO ﹕ BST laminated films are grown on/Si (001) substrate；
In this step, argon flow amount is 75sccm, and the flow of oxygen is 25sccm；
In this step, specific sputtering condition is：Magnetron sputtering power is 60W, and pulsed laser deposition power is 0.7W, pulse
Laser frequency is 3Hz；During cosputtering, in vacuum room, sputtering pressure is maintained at 5Pa, and growth temperature is 900 DEG C；
By above-mentioned sputtering condition cosputtering 1h, you can in Pt (111)/TiO2/SiO2Grow on/Si (001) substrate and obtain
It is 1 that thickness is 800nm, MgO and BST volume ratio:60, the MgO ﹕ BST laminated films of 0-3 type structures.
C, 60 laminated film plane-parallel capacitors of preparation 0-3 type MgO ﹕ BST=1 ﹕：On gained MgO ﹕ BST laminated films,
Pt electrodes are grown by magnetic control sputtering device, obtain with Pt as Top electrode, with MgO ﹕ BST laminated films as dielectric so as to build
Layer, with Pt (111)/TiO2/SiO2The Pt of/Si (001) substrate（111）0-3 type MgO ﹕ BST=1 ﹕ 60 THIN COMPOSITE of the layer for bottom electrode
Film plane-parallel capacitor.
Dielectric layer to the 60 laminated film plane-parallel capacitors of 0-3 type MgO ﹕ BST=1 ﹕ prepared by embodiment 6, i.e. MgO ﹕
BST laminated films carry out XRD analysis, as a result as shown in Figure 8.As seen from Figure 8, which is 0-3 type laminated films, and BST is many
Crystal structure, MgO are mono-crystalline structures.
Fig. 9 gives the C-V characteristic curves of the plane-parallel capacitor prepared by embodiment 6, as can be seen from Figure, the electricity
The tuning rate of container is 27%.
Claims (7)
1. a kind of microwave ferro-electricity compound film capacitor, is characterized in that, the capacitor is with monocrystal chip as substrate, with microwave
Ferro-electricity compound film be dielectric layer, with Pt, Au, Ag, Al, Cu, SrRuO or La0.5Sr0.5CoO3For the electricity of the interdigital structure of electrode
Container；
The monocrystal chip is MgO monocrystal chips, LaAlO3Monocrystal chip, Al2O3Monocrystal chip, Si monocrystal chips or SrTiO3It is single
Brilliant substrate；
The microwave ferro-electricity compound film is the 1-3 type laminated films in barium strontium titanate doped with MgO, its thickness is 100 ~
2000nm；Doping volume ratios of the MgO in the barium strontium titanate is 1 ﹕, 1 ~ 1 ﹕ 160；
The Ba/Sr ratios of the barium strontium titanate are 0.1 ﹕, 0.9 ~ 0.9 ﹕ 0.1.
2. microwave ferro-electricity compound film capacitor according to claim 1, is characterized in that, the Ba/Sr of the barium strontium titanate
Than for 0.6 ﹕ 0.4.
3. microwave ferro-electricity compound film capacitor according to claim 1, is characterized in that, the MgO is in the strontium titanates
Doping volume ratio in barium is 1 ﹕, 40 ~ 1 ﹕ 110.
4. a kind of preparation method of microwave ferro-electricity compound film capacitor, is characterized in that, comprise the following steps：
A, magnetic control target position and laser that A targets and B targets are separately mounted to magnetic control and pulse laser co-deposition vacuum installation
Target position；Substrate is carried out into cleaning treatment, is then bonded on sample carrier, be placed to magnetic control and pulse laser is co-deposited vacuum installation
Sample stage on；
Wherein, the B targets are high-purity barium strontium titanate targets of the Ba/Sr than 0.1 ﹕, 0.9 ~ 0.9 ﹕ 0.1；The A targets are high-purity
MgO target；The substrate is MgO monocrystal chips, LaAlO3Monocrystal chip, Al2O3Monocrystal chip, Si monocrystal chips or SrTiO3
Monocrystal chip；
B, the back end vacuum of vacuum chamber is adjusted to（0.01~100）×10-4Pa, then adjusts magnetic control target spacing and is 1 ~ 10cm, swashs
Light target spacing is 1 ~ 10cm, then passes to argon/oxygen mixed gas that flow is 5 ~ 100sccm, then sets sputtering condition,
Growth over the substrate obtains the laminated film of 1-3 type structures；The growth thickness control of the laminated film 100 ~
2000nm；
Argon in the argon/oxygen mixed gas: the volume ratio of oxygen is 1: 3 ~ 3: 1；
The sputtering condition is：Magnetron sputtering power is 0.1 ~ 100W, and pulsed laser deposition power is 0.1 ~ 5W, and pulse laser is frequently
Rate is 0.1 ~ 10Hz, and sputtering pressure is 1 ~ 100Pa, and growth temperature is 500 ~ 1000 DEG C；
Under the sputtering condition during growing mixed thin film, doping volume ratios of the MgO in the barium strontium titanate
Control is in 1 ﹕, 1 ~ 1 ﹕ 160；
C, on the laminated film of gained 1-3 type structures, make interdigital pattern first with photoetching process, then described interdigital
Pt, Au, Ag, Al, Cu, SrRuO or La are grown on pattern0.5Sr0.5CoO3Electrode, is finally peeled away pattern, and structure obtains interdigital knot
The capacitor of structure.
5. the preparation method of microwave ferro-electricity compound film capacitor according to claim 4, is characterized in that, described in step b
Growth temperature is 900 DEG C.
6. the preparation method of microwave ferro-electricity compound film capacitor according to claim 4, is characterized in that, described in step b
Vacuum is 2 × 10-4Pa, the magnetic control target spacing be 6.5cm, the laser target spacing be 5cm, the argon/oxygen mix
The flow of gas is 100sccm；
The sputtering condition is specially：40 ~ 80W of magnetron sputtering power, pulsed laser deposition power 0.7W, pulse laser frequency
3Hz, sputtering pressure are maintained at 5Pa, and growth temperature is 900 DEG C.
7. the preparation method of microwave ferro-electricity compound film capacitor according to claim 4, is characterized in that, described in step a
The Ba/Sr ratios of barium strontium titanate target are 0.6 ﹕ 0.4.
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|---|---|---|---|---|
| US5635434A (en) * | 1995-09-11 | 1997-06-03 | The United States Of America As Represented By The Secretary Of The Army | Ceramic ferroelectric composite material-BSTO-magnesium based compound |
| CN1738097A (en) * | 2005-09-12 | 2006-02-22 | 中国科学院物理研究所 | Ferroelectric phase shifter |
| CN101609689A (en) * | 2009-07-02 | 2009-12-23 | 中国科学院宁波材料技术与工程研究所 | A kind of magnetic recording media and wiring method thereof based on multiferroic film |
| CN102593588A (en) * | 2011-11-21 | 2012-07-18 | 中国科学院合肥物质科学研究院 | Scanning end-fire array antenna based on boundary scan test (BST) film phase shifter |
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| US5635434A (en) * | 1995-09-11 | 1997-06-03 | The United States Of America As Represented By The Secretary Of The Army | Ceramic ferroelectric composite material-BSTO-magnesium based compound |
| CN1738097A (en) * | 2005-09-12 | 2006-02-22 | 中国科学院物理研究所 | Ferroelectric phase shifter |
| CN101609689A (en) * | 2009-07-02 | 2009-12-23 | 中国科学院宁波材料技术与工程研究所 | A kind of magnetic recording media and wiring method thereof based on multiferroic film |
| CN102593588A (en) * | 2011-11-21 | 2012-07-18 | 中国科学院合肥物质科学研究院 | Scanning end-fire array antenna based on boundary scan test (BST) film phase shifter |
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