CN106409818B - A non-destructive method for obtaining flexible ferroelectric thin film capacitors - Google Patents
A non-destructive method for obtaining flexible ferroelectric thin film capacitors Download PDFInfo
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- CN106409818B CN106409818B CN201610905648.2A CN201610905648A CN106409818B CN 106409818 B CN106409818 B CN 106409818B CN 201610905648 A CN201610905648 A CN 201610905648A CN 106409818 B CN106409818 B CN 106409818B
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- pzt
- sheet glass
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- H10D1/00—Resistors, capacitors or inductors
- H10D1/60—Capacitors
- H10D1/68—Capacitors having no potential barriers
- H10D1/682—Capacitors having no potential barriers having dielectrics comprising perovskite structures
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Abstract
A kind of method that non-destructive obtains flexible ferroelectric capacitor, belongs to ferro-electric device and field of semiconductor technology.The present invention is to obtain inorganic substrate by convenient, economic method and have ferroelectric film capacitor part flexible, the tool ground by using common materials such as diamond dust, industrial wax, sheet glass and glass plates as substrate, melt industrial wax using heating platform and bond sheet glass and PZT, 100 μ m-thicks then are thinned to become flexibility PZT with the rigid PZT device that substrate thickness can be about 500 μm by diamond dust, recycle a small amount of chemical reagent that can remove the residual industrial wax for being adhered to device surface.This method principle is simple, low in cost, safe and reliable, flexible ferroelectric thin film device faster can be more safely obtained compared to other methods, its excellent electrology characteristic will not be lost simultaneously, and the flexible device is still able to maintain good electric property under stress condition repeatedly, has excellent reliability.
Description
Technical field
The present invention relates to ferroelectric thin film device and field of semiconductor technology, are suitable for all kinds of ferroelectric capacitors, mainly answer
Ferroelectric capacitor for obtaining having flexible characteristic.
Background technique
With the development of semiconductor process technology, the development of the flexible substrate device based on ferroelectric material is received increasingly
More concerns, good physical and chemical properties, so that flexible substrate device has boundless application prospect.Traditional
Silica-base material has mechanical equivalent of light fragility, it is difficult to bear larger deformation, therefore Si based material device has its own in terms of flexible application
Limitation.
Flexible device under normal conditions is grown on RF magnetron sputtering, and electrology characteristic is far from being grown in inorganic lining
The device at bottom is ideal.Simultaneously, it is contemplated that the production of organic flexible substrate devices is more demanding to equipment and technique, needs a large amount of
Time and fund investment.Based on this it is proposed that a kind of side that is more convenient, economically obtaining flexible ferroelectric capacitor
Method can guarantee that its electric property is unaffected.Simultaneously can deformation occurs under larger stress condition, and keep original electricity
Performance has the characteristic of flexible device.
The present invention provides the methods that one kind convenient can obtain flexible ferroelectric capacitor, and this method is easy, quick,
It can also be applied to other small size silicon substrate devices.
Summary of the invention
The purpose of the invention to be reached is to provide a kind of safe and reliable method, with the zirconium being grown on silicon (Si) substrate
Lead titanates (PbZr0.44Ti0.56O3, PZT) and thin-film capacitor structure Pt/PZT/Pt/SiO2/ Si is main study subject, by rigid
The grinding of property silicon substrate, flexible pzt thin film capacitor is obtained in the case where not destroying device architecture and performance.
To reach above-mentioned purpose, the present invention provides following solution:
A kind of lead zirconate titanate (PbZr grown on a silicon substrate0.44Ti0.56O3, PZT) and thin-film capacitor structure feature includes:
Silicon substrate 1, epitaxial buffer silicon dioxide layer 2, lower electrode 3, PZT4, top electrode 5.Lower electrode 3 and the material of top electrode 5 are platinum.
Epitaxial buffer silicon dioxide layer 2 is grown on silicon substrate 1, and lower electrode 3 is grown in epitaxial buffer silicon dioxide layer 2, and PZT4 is raw
On the lower electrode 3, top electrode 5 is grown on PZT4 length.
First top electrode 5 and PZT4 industrial wax 6 are protected, and make top electrode 5 using the hot melt of industrial wax 6 and condensation
It is bonded together with small sheet glass 7, and then realizes the grinding of substrate with diamond dust.
The method for obtaining flexible ferroelectric capacitor using a kind of non-destructive that above structure is carried out as sample, the party
The step of method, implements as follows.
The experiment equipment for implementing this method includes: a kind of lead zirconate titanate (PbZr grown on a silicon substrate0.44Ti0.56O3,
PZT) thin-film capacitor structure, diamond dust, industrial wax 6, small sheet glass 7, big glass plate, screw-thread micrometer, blade, tweezers, heating
Platform, chemical reagent, lens paper, small beaker, spring steel plate.Chemical reagent includes carbon tetrachloride, trichloro ethylene, acetone, ethyl alcohol
And deionized water；Heating platform can be such that wax melts.
Step 1: the top electrode 5 at the top of PZT4 is protected using the hot melt and condensation of industrial wax 6, while will be powered on
Pole 5 and the side of small sheet glass 7 are bonded.
A kind of step 2: the silicon substrate 1 of the PZT thin film capacitance structure using diamond dust to growth on a silicon substrate
It is ground, hold small sheet glass 7 and " draws 8 words " on silicon substrate 1, until 1 thickness of silicon substrate reduces to 100 μm or so.
Step 3: melt industrial wax 6 heating of small sheet glass 7 again, remove PZT4 and be put into and be lined with the small of lens paper
In beaker, last cleaning is done to it using chemical reagent.
In view of sample grinding front and back needs to carry out electrical measurement, and need to keep with small sheet glass 7 during the grinding process
More close tacky state, therefore use this relatively stable material of industrial wax 6.
Using the silicon substrate 1 of diamond dust ground PZT quickly, while the main component of diamond dust is Al2O3, will not be right
Properties of sample has an impact.
Last chemical reagent cleaning can effectively remove the industrial wax 6 for being attached at the top of PZT4, shielding, with
Prevent residual industrial wax 6 from having an impact to the electric property of sample.Rigid sample: substrate thickness is thicker, does not have flexible characteristic
The sample of (electric property is degenerated after bending repeatedly).Flexible sample: obtaining by this method, after substrate thinning and has
The sample of standby flexible device characteristic (electric property is not degenerated after bending repeatedly).
This method is before grinding the pzt thin film capacitor of growth on a silicon substrate first with industrial wax to top electrodes
It is protected, so that will not cause to damage to the electrode structure at the top of sample during substrate thinning, while being made using diamond dust
It can be realized for grinding-material in the case where not influencing sample electric property, safely, quickly finish the thinning operation of substrate,
To obtain PZT flexible.
PZT after being thinned can preferably realize bending repeatedly, have the property of flexible device, and electric property is not sent out
It is raw to degenerate.And the easy easily implementation of the method, it is easy to operate, widely used, cheap, it can be used for any need and obtain flexible iron
The field of conductive film capacitor.
Detailed description of the invention
The present invention is described further with reference to the accompanying drawings and examples.
Fig. 1 is that one kind is grown in the lead zirconate titanate PZT thin-film capacitor structure on silicon (Si) substrate.
Fig. 2 is the PZT structure with the rigid silicon substrate after sheet glass bonding.
Fig. 3 is flexibility (after substrate grinding) the PZT structure bonded with sheet glass.
Fig. 4 is the ferroelectric hysteresis loop comparison of rigidity and flexibility PZT sample.
Fig. 5 is ferroelectric hysteresis loop of the flexibility PZT under different stress circle said conditions.
Fig. 6 is that the PZT (substrate thickness is about 500 μm) of rigid silicon substrate is bending 5 times (strain 0.186%) and 55 repeatedly
The ferroelectric hysteresis loop comparison measured after secondary (strain 0.186%).
In figure: 1, silicon substrate, 2, epitaxial buffer layer silica (SiO2) layer, 3, lower electrode, 4, PZT, 5, top electrode, 6,
Industrial wax, 7, sheet glass.
Specific embodiment
It is a kind of rigidity silicon substrate PZT structure feature include: silicon substrate 1, epitaxial buffer silica (SiO2) layer 2, under
Electrode 3, PZT4, top electrode 5, such as Fig. 1.
The ferroelectric hysteresis loop of sample is measured in advance before grinding, is compared for subsequent measurement, the instrument used is
Ferroelectric properties tester, test condition are as follows: voltage 40V, frequency 1kHz, test waveform are triangular wave.
Warming temperature first is carried out to heating platform, by a fritter industry while small sheet glass 7 is put on heating platform
Wax 6 is placed in the center position of small sheet glass 7, and (about 80 DEG C or so) clamp sample with tweezers after industrial wax 6 melts completely, this
When sample be rigidity, while silicon substrate 1 up, be placed on the center of small sheet glass 7, come into full contact with it with industrial wax 6, such as
Fig. 2.
It then removes small sheet glass 7 to be cooled to room temperature, wipes work extra around PZT4 off with blade after it is completely cooling
Industry wax 6 remembers that small sheet glass is stained with the one side of PZT4 as front.
It takes appropriate diamond dust to be placed on big glass plate, is stained with 7 thickness of small sheet glass of PZT simultaneously with screw-thread micrometer measurement
It writes down, small 7 face down of sheet glass is placed on the big glass plate for being covered with diamond dust, pin small sheet glass 7 and in big glass
" 8 words are drawn " on plate.
Moment keeps having diamond dust between silicon substrate 1 and big glass plate, and repeats aforesaid operations, uses spiral shell every 10 times or so
Rotation micrometer measures 7 thickness of small sheet glass for being stained with PZT4, and compared with measurement result before.
Since the thickness of sample is about 500 μm, the amount of grinding of silicon substrate is obtained by the difference of grinding front and back, and then learn
1 residual thickness of silicon substrate.
Stop grinding when the thickness of its silicon substrate 1 is thinned to about 100 μm, is wiped on small sheet glass 7 with clean test paper
Diamond dust, such as Fig. 3.
At this time obtained flexible PZT is placed on heating platform again together with sheet glass and is heated, until industrial wax 6 melts
Change, the PZT after removing grinding with tweezers.By camera lens paper washer to beaker bottom, it is put into carbon tetrachloride and PZT, is taken after boiling 2 minutes
PZT out then successively repeats aforesaid operations with trichloro ethylene, acetone, ethanol reagent, finally uses deionized water repeated flushing PZT
At least 20 times, to remove residual chemical agents.
The measurement of ferroelectric hysteresis loop is carried out to sample using probe station and ferroelectric properties tester, thus judges grinding front and back
Whether the electrology characteristic of sample changes.And measurement result is integrated, such as Fig. 4.
For the difference for determining rigidity and flexibility PZT sample electric property under different bending amplitudes, flexible PZT sample is glued
Close on the spring steel plate of 30mmx8mmx0.5mm, by apply external force make sample generate size be respectively 0.186%,
0.223%, 0.260% bending strain, every kind of strain applies 50 times repeatedly, and measures to the ferroelectric hysteresis loop of sample.Knot
Fruit is not as shown in figure 5, the polarization value of sample is degenerated.
The PZT sample for taking one piece of rigid silicon substrate makes it generate 5 0.186% bending strain and 50 times 0.186% bendings
Strain, and its ferroelectric hysteresis loop is measured.As a result as shown in fig. 6, after carrying out 50 bendings repeatedly to sample, polarization
Value deteriorates 22.8%.
It is thus regarded that the electric property of obtained flexible PZT sample is not degenerated, at the same can by hundred times repeatedly
Its electrology characteristic (ferroelectric hysteresis loop) is kept not change after bending, it is more standby flexible compared to the PZT sample of rigid silicon substrate
Characteristic.
Finally, it should be noted that above embodiments are only and not to limit this hair to illustrate preferred embodiment
Bright described technical solution；Therefore, those skilled in the art should understand that, what all design key according to this case were done
Equivalent variations is intended to be within the scope of the claims of the invention.
Claims (2)
1. a kind of method that non-destructive obtains flexible ferroelectric capacitor, it is characterised in that: the structure for realizing this method includes
Silicon substrate (1), epitaxial buffer silicon dioxide layer (2), lower electrode (3), PZT (4), top electrode (5)；Lower electrode (3) and top electrode
(5) material is platinum；Epitaxial buffer silicon dioxide layer (2) is grown on silicon substrate (1), and lower electrode (3) is grown in epitaxial buffer
In silicon dioxide layer (2), PZT (4) is grown on lower electrode (3), and top electrode (5) is grown on PZT (4)；
Top electrode (5) and PZT (4) are protected with industrial wax (6) first, and made using the hot melt and condensation of industrial wax (6)
Electrode (5) is bonded together with small sheet glass (7), and then the grinding of substrate is realized with diamond dust；
The method for obtaining flexible ferroelectric capacitor using a kind of non-destructive that above structure is carried out as sample, this method
Step is implemented as follows；
Implement this method experiment equipment include: a kind of growth PZT thin film capacitance structure on a silicon substrate, diamond dust,
Industrial wax (6), small sheet glass (7), big glass plate, screw-thread micrometer, blade, tweezers, heating platform, chemical reagent, lens paper,
Small beaker, spring steel plate；Chemical reagent includes carbon tetrachloride, trichloro ethylene, acetone, ethyl alcohol and deionized water；Heating platform energy
Enough melt wax；
Step 1: the top electrode (5) at the top of PZT (4) is protected using the hot melt and condensation of industrial wax (6), while will be upper
Electrode (5) and the side of small sheet glass (7) are bonded；
Step 2: using diamond dust to the silicon substrate (1) of growth PZT thin film capacitance structure on a silicon substrate a kind of into
Row grinding holds small sheet glass (7) and " draws 8 words " above in silicon substrate (1), until silicon substrate (1) thickness reduces to 100 μm of left sides
It is right；
Step 3: melt industrial wax (6) small sheet glass (7) heating again, remove PZT (4) and be put into and be lined with lens paper
In small beaker, last cleaning is done to it using chemical reagent；
In view of sample grinding front and back need to carry out electrical measurement, and need during the grinding process with small sheet glass (7) keep compared with
For close tacky state, therefore use industrial wax (6) this relatively stable material；
Using the silicon substrate (1) of diamond dust ground PZT quickly, while the main component of diamond dust is Al2O3, will not be to sample
Moral character can have an impact；
Last chemical reagent cleaning can effectively remove the industrial wax (6) for being attached at the top of PZT (4), shielding, with
Prevent residual industrial wax (6) from having an impact to the electric property of sample；
The ferroelectric hysteresis loop of sample is measured in advance before grinding, is compared for subsequent measurement, the instrument used is ferroelectricity
Ability meter, test condition are as follows: voltage 40V, frequency 1kHz, test waveform are triangular wave.
2. the method that a kind of non-destructive according to claim 1 obtains flexible ferroelectric capacitor, it is characterised in that: first
Warming temperature is carried out to heating platform, is placed in a fritter industrial wax (6) while small sheet glass (7) is put on heating platform
The center position of small sheet glass (7) clamps sample with tweezers after industrial wax (6) melts completely, and sample is rigidity at this time, together
When silicon substrate (1) up, be placed on the center of small sheet glass (7), come into full contact with it with industrial wax (6)；
It then removes small sheet glass (7) to be cooled to room temperature, wipes work extra around PZT (4) off with blade after it is completely cooling
Industry wax (6) remembers that small sheet glass is stained with the one side of PZT (4) as front；
It takes appropriate diamond dust to be placed on big glass plate, be stained with small sheet glass (7) thickness of PZT with screw-thread micrometer measurement and remember
Under, small sheet glass (7) face down is placed on the big glass plate for being covered with diamond dust, pins small sheet glass (7) and in big glass
" 8 words are drawn " in glass plate；
Moment keeps having diamond dust between silicon substrate (1) and big glass plate, and repeats aforesaid operations, uses spiral every 10 times or so
Micrometer measures small sheet glass (7) thickness for being stained with PZT (4), and compared with measurement result before；
Since the thickness of sample is about 500 μm, the amount of grinding of silicon substrate is obtained by the difference of grinding front and back, and then learn that silicon serves as a contrast
Bottom (1) residual thickness；
Stop grinding when the thickness of its silicon substrate (1) is thinned to about 100 μm, is wiped on small sheet glass (7) with clean test paper
Diamond dust；
At this time obtained flexible PZT is placed on heating platform again together with sheet glass and is heated, until industrial wax (6) melt,
PZT after removing grinding with tweezers；By camera lens paper washer to beaker bottom, it is put into carbon tetrachloride and PZT, is taken out after boiling 2 minutes
PZT then successively repeats aforesaid operations with trichloro ethylene, acetone, ethanol reagent, finally extremely with deionized water repeated flushing PZT
It is 20 times few, to remove residual chemical agents.
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| CN111668372B (en) * | 2020-06-18 | 2023-05-30 | 中国科学院微电子研究所 | A kind of HfO2-based ferroelectric capacitor and its preparation method and HfO2-based ferroelectric memory |
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| CN1682371A (en) * | 2003-01-17 | 2005-10-12 | 富士通株式会社 | Ferroelectric capacitor and its manufacturing method |
| CN102185025A (en) * | 2011-04-01 | 2011-09-14 | 中国科学院上海技术物理研究所 | Manufacturing process of metal waveguide microcavity optical coupling structure used for photoelectric functional devices |
| CN105811914A (en) * | 2016-02-25 | 2016-07-27 | 锐迪科微电子（上海）有限公司 | Bulk acoustic wave device, integrated structure and manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1682371A (en) * | 2003-01-17 | 2005-10-12 | 富士通株式会社 | Ferroelectric capacitor and its manufacturing method |
| CN102185025A (en) * | 2011-04-01 | 2011-09-14 | 中国科学院上海技术物理研究所 | Manufacturing process of metal waveguide microcavity optical coupling structure used for photoelectric functional devices |
| CN105811914A (en) * | 2016-02-25 | 2016-07-27 | 锐迪科微电子（上海）有限公司 | Bulk acoustic wave device, integrated structure and manufacturing method |
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