CN103469156A - Method for carrying out stressing engineering on thicker ferroelectric film for material modification - Google Patents
Method for carrying out stressing engineering on thicker ferroelectric film for material modification Download PDFInfo
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Abstract
The invention provides a method for carrying out stressing engineering on a thicker ferroelectric film for material modification. The method comprises the following steps of: sequentially depositing an LNO3 bottom electrode, a PZT film and a CFO film on an STO substrate by means of magnetron sputtering, and forming a PZT film layer with co-existent a electric domain and c electric domain. The method provided by the invention conquers the shortcomings in the prior art, is simple in operation method, stable in performance, and good in repeatability. By adopting the method provided by the invention, the performance of a photoelectric functional film material with the thickness more than 100nm can be greatly improved, and simultaneously, the production cost is greatly reduced.
Description
Technical field
The present invention relates to a kind of the thicker ferroelectric membranc that is greater than 100nm be implemented to " stress engineering ", for the method for material modification, belong to the film material with function technical field.
Background technology
In thin-film material, stress is almost ubiquitous.Especially in epitaxial film, stress plays a part very important on the impact of thin-film material performance.In ferroelectric thin-flim materials, common investigators utilize stress to strengthen ferroelectric properties.And, developing into ripe stress engineering now.Be published in masterpiece on Science and Nature and ideally represented stress engineering ferroelectric properties is improved greatly, this is to made relevant photoelectricity, information, and the improvement of functional device performance, have very dark direct significance.Yet the stress in film is along with thickness increase relaxation soon, until, after thickness reaches critical thickness, stress effect disappears.Thereby the angle of practical engineering application, the having little significance of stress engineering.
On the other hand, the research of multi-ferroic material starts to rise in recent ten years.Owing to having very strong ferroelectric and magnetic simultaneously, and the monophase materials that simultaneously has very strong magnetic, an iron percentage coupling almost can not find (preparation is not out), so the investigator starts, with ferroelectric and two single-phase mixing of magnetic, to make synthetic film.The structure formation that synthetic film is prepared into has the multilayer film (multilayer, 2-2 type) of level and vertical nano structure membrane (nanostructure, the 1-3 type, in order to improve percentage coupling).2-2 type and 1-3 type synthetic film form are shown as Fig. 1 and Fig. 2.In the structure of 1-3 type, the researchist finds to break through the restriction of thick film counter stress effect, stress application in vertical direction.Subsequently, in a series of relevant synthetic films of nanostructure, the result of study that stress improves film performance is seen in like the mushrooms after rain and is reported on various authoritative magazines.
Although the film of this 1-3 type nanostructure is favourable to improving two out of phase percentage coupling, also unfavorable to the performance that improves monophase materials.Such as, original 100% pzt thin film, mixed now the CFO of x%, there is ferroelectric PZT content and just reduce to (1-x) %.Thereby, along with the raising of mixed CFO content x, the ferroelectricity of whole film will decrease.
The applicant is at research CFO/PZT (CoFe
2o
4/ Pb (Zr
0.2) Ti
0.8o
3, the 2-2 type) and in composite double layer film [23,24] process, found unusual stress phenomena.Traditional stress is in film is subject to face during (in-plane) tension stress, and outer (out-of-plane) lattice parameter of the face of film will be shunk, as shown in Figure 3.And, when being subject to the face internal pressure stress, the outer lattice parameter of face will be extended, as shown in Figure 4.Yet we find, in the CFO/PZT composite double layer film of preparation, in film is subject to face, during tension stress, the outer lattice parameter of the face of film can be extended in appropriate circumstances.This singular stress effect has engineering technology application widely to be worth on the photoelectric functional device.
Develop into from block materials the use that thin-film material can be saved material widely, can greatly reduce operating voltage, make the device can be integrated with existing standard semiconductor circuit.And, can improve the performance of material from the block to the film.And " stress engineering " of film can improve the performance of film itself widely.But " stress engineering " of film is along with relaxation phenomena occurs soon in the increase of thickness (being generally less than 100nm).This energy is implemented effectively " stress engineering ", and film had both been required to very thin uniform thin film, requires again very high-quality epitaxy.This has just increased the difficulty of preparation greatly, thereby, improved widely cost.In actual production, this expensive production is that businessman is almost unacceptable.
Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of working method is simple, stable performance, reproducible, and can significantly improve the performance of the thick photoelectric function thin films material that is greater than 100nm, the method reduced production costs.
In order to solve the problems of the technologies described above, technical scheme of the present invention be to provide a kind of to thicker ferroelectric membranc implement stress engineering for material modification method, it is characterized in that: by adopting magnetron sputtering, in succession deposit LNO on the STO substrate
3bottom electrode, pzt thin film and CFO film, and form the pzt thin film layer that a, c electricdomain coexist; Specifically by following 2 steps, formed:
Step 1: the preparation of sputtering target
Step 1.1:LNO ceramic target
By purity, be 99.9%La
2o
3and Ni
2o
3powder is pressed into block after by the La of 1: 1, Ni atomic ratio mixed grinding, and high temperature sintering, make LaNiO
3ceramic target;
Step 1.2:PZT ceramic target
By PbO, ZrO
2and TiO
2powder evenly mixes, press forming, and last sintering forms;
Step 1.3:CFO ceramic target
By CoO and Fe
2o
3press forming after the even mixed grinding of powder, the final high temperature sintering, make CoFe
2o
4ceramic target;
Step 2: the preparation of thin-film material
Step 2.1: the too sour strontium SrTiO of the monocrystalline that substrate is 100 orientations
3/ STO; Substrate first, with the ultrasonic cleaning that hockets of ethanol, acetone, is then carried out matting with trieline, finally in vacuum chamber, peels off cleaning with Ar Ion Beam Etching again;
Step 2.2: pass into argon gas and oxygen, carry out sputtering sedimentation LaNiO
3film, obtain the LNO film;
Step 2.3: by LaNiO
3target changes the PZT ceramic target into, and sputter cavity background is vacuumized, and will be coated with bottom electrode LaNiO simultaneously
3monocrystalline STO substrate heating, then pass into argon gas, carry out the sputtering sedimentation pzt thin film; Carry out respectively the sputtering operation of different time on different LNO/STO substrates, obtain the pzt thin film layer of different thickness;
Step 2.4: the pzt thin film sample of gained different thickness is put on the vacuum chamber substrate frame simultaneously, by sputter cavity background suction, by all samples heating, then passed into argon gas simultaneously, carry out sputtering sedimentation CFO film; Control sputtering time, make the CFO thin film layer that all covers one deck same thickness on all different thickness pzt thin film samples.
Preferably, in described step 1.1, block diameter * thickness is 60mm * 3mm, and the temperature of high temperature sintering is 1100 ℃, and the time of high temperature sintering is 3 hours.
Preferably, in described step 1.2, at PbO, ZrO
2and TiO
2the excessive Pb that adds 10%wt in powder.
Preferably, in described step 1.2, sintering temperature is 900 ℃, and sintering time is 3 hours; PZT ceramic target size diameter * thickness of making is 60mm * 5mm, and the per-cent Zr of constituent content: Ti is 20: 80.
Preferably, in described step 1.3, the temperature of high temperature sintering is 1200 ℃, and the time of high temperature sintering is 3 hours.
Preferably, in described step 2.2, the processing condition of sputter-deposited thin films are as follows: base vacuum degree 5 * 10
-4pa, 400 ℃ of base reservoir temperatures, target-cardinal distance is from 7cm, radio frequency power 80～100W.
Preferably, in described step 2.2, pass into argon gas and oxygen and keep air pressure at 1.6Pa, the LNO film thickness is 50nm, the in-situ sputtering deposition LaNiO obtained
3the resistivity of film is 7 * 10
-4Ω cm.
Preferably, in described step 2.3, sputter cavity background suction is extracted into to 5 * 10
-4pa, will be coated with bottom electrode LaNiO
3monocrystalline STO substrate be heated to 650 ℃, pass into argon gas and keep air pressure at 1.6Pa, carry out the sputtering operation of different time, can obtain the sample P ZT/LNO/STO that thickness is 30～150nm PZT layer.
Preferably, in described step 2.4, sputter cavity base vacuum degree is extracted into to 5 * 10
-4pa, be heated to 650 ℃ by all samples, passes into argon gas and keep air pressure at 1.6Pa, on the sample P ZT/LNO/STO that is 30～150nm PZT layer at thickness, carries out sputter CFO operation, and the CFO thin film layer thickness obtained is 50nm.
The method that thicker ferroelectric membranc enforcement stress engineering is used for to material modification provided by the invention has been avoided the high request of tradition " stress engineering " dexterously, and only need prepare the pzt thin film layer that a, c ferroelectric domain coexist, can put " oppositely " stress engineering to good use to thick pzt thin film.Under the prerequisite that significantly improves film performance, less demanding due to the present invention to film, therefore, increased the operability of production department greatly, greatly reduces production cost.
Method provided by the invention has overcome the deficiencies in the prior art, and working method is simple, and stable performance is reproducible, and can significantly improve the performance of the thick photoelectric function thin films material that is greater than 100nm, greatly reduces production cost simultaneously.
The accompanying drawing explanation
Fig. 1 is horizontal direction multilayer film (multilayer, 2-2 type) schematic diagram;
Fig. 2 is vertical direction nanostructure multilayer film (nanostructure, 1-3 type) schematic diagram;
Fig. 3 is that film is subject to tension stress schematic diagram in face;
Fig. 4 is that film is subject to face internal pressure stress schematic diagram;
The XRD diffraction spectrogram that Fig. 5 is CFO/PZT (30～150nm) sample;
The XRD figure that Fig. 6 is sample CFO/PZT (300nm)/LNO/STO and PZT (300nm)/LNO/STO;
Fig. 7 is the having of the thick PZT of 100nm, without the ferroelectric hysteresis loop P-V of CFO layer;
Fig. 8 is the having of the thick PZT of 300nm, without the ferroelectric hysteresis loop P-V of CFO layer.
Embodiment
For the present invention is become apparent, hereby with a preferred embodiment, and coordinate accompanying drawing to be described in detail below.
Provided by the invention to thicker ferroelectric membranc implement stress engineering for the method for material modification by adopting conventional magnetron sputtering in succession to deposit LNO on the STO substrate
3bottom electrode, pzt thin film and CFO film, and form the pzt thin film layer that a, c electricdomain coexist.Its concrete preparation process is as follows:
Step 1: the preparation of sputtering target (routine)
Step 1.1:LNO ceramic target
By purity, be 99.9%La
2o
3and Ni
2o
3powder is pressed into after by the La of 1: 1, Ni atomic ratio mixed grinding
block, then, 1100 ℃ of high temperature sinterings 3 hours, make LaNiO
3ceramic target;
Step 1.2:PZT ceramic target
By PbO, ZrO
2and TiO
2powder, by required stoichiometric ratio, is the volatilization loss of compensation Pb, adds the excessive Pb of 10%wt (weight percent), and evenly mixing, press forming, finally form at 900 ℃ of sintering in 3 hours, and it is of a size of
the per-cent Zr of constituent content: Ti is 20: 80.
Step 1.3:CFO ceramic target
By CoO and Fe
2o
3powder is by press forming after the required even mixed grinding of stoichiometric ratio, finally, 1200 ℃ of high temperature sinterings 3 hours, makes CoFe
2o
4ceramic target.
Step 2: the preparation of thin-film material (routine)
Step 2.1: the too sour strontium SrTiO of monocrystalline that substrate is (100) orientation
3(STO).Substrate first, with the ultrasonic cleaning that hockets of ethanol, acetone, is then carried out matting with trieline, finally in vacuum chamber, peels off cleaning with Ar Ion Beam Etching again.
Step 2.2: the processing condition of sputter-deposited thin films are as follows: base vacuum degree 5 * 10
-4pa, 400 ℃ of base reservoir temperatures, target-cardinal distance is from 7cm, and radio frequency power 80～100W, then pass in proportion argon gas and oxygen and keep air pressure in the 1.6Pa left and right, at this moment carries out sputtering sedimentation LaNiO
3film obtains the LNO film that about 50am is thick.At this moment the in-situ sputtering deposition LaNiO obtained
3the resistivity of film is～7 * 10
-4Ω cm.
Step 2.3: then, by LaNiO
3target changes the PZT ceramic target into.Equally, sputter cavity base vacuum degree is extracted into to 5 * 10
-4pa.Simultaneously, will be coated with bottom electrode LaNiO
3monocrystalline STO substrate be heated to 650 ℃, then pass into argon gas and keep air pressure in about 1.6Pa, carry out the sputtering sedimentation pzt thin film.Carry out respectively the sputtering operation of different time on different LNO/STO substrates, can obtain the pzt thin film layer of required different thickness.
Step 2.4: last, the pzt thin film sample (PZT/LNO/STO) of gained different thickness is put on the vacuum chamber substrate frame simultaneously.Equally, sputter cavity base vacuum degree is extracted into to 5 * 10
-4pa.Simultaneously, all samples is heated to 650 ℃, then passes into argon gas and keep air pressure in the 1.6Pa left and right, carry out sputtering sedimentation CFO film.Control sputtering time, make on all different thickness pzt thin film samples and all cover the CFO thin film layer that the about 50nm of one deck is thick.
For the convenience of discussing, at first we list in the lattice parameter of associated materials as following table 1.
The structure of table 1 associated materials and lattice parameter
At STO (SrTiO
3) on substrate, at first deposit the LaNiO of one deck thickness 50nm
3as bottom electrode.Then in succession deposit the pzt thin film of a series of thickness 30nm～150nm.Finally deposit again the CFO layer that one deck 50nm is thick.The XRD diffraction spectra of series samples as shown in Figure 5.
Wherein, (200) and (002) two peak appear in PZT, and (200) peak is corresponding to a farmland in PZT, and (002) peak is corresponding to the c farmland.Illustrate in pzt thin film that a farmland and c farmland coexist.As can be seen from Figure 5, after having added the CFO layer, (002) peak, to the skew of wide-angle direction, illustrate that outer (out-of-plane) lattice parameter of face on c farmland reduces, and the outer lattice parameter of the face on a farmland in contrast, for increasing.And, along with the reduction of pzt thin film thickness, the side-play amount of peak position increases.Because as can be seen from Table 1, the lattice parameter a of PZT and b or be greater than the lattice parameter of LNO or STO simultaneously, or be less than the lattice parameter of CFO simultaneously.Thereby the in-plane stress (in-plane) that a farmland of PZT and c farmland are subject to should be all tension stress or be all stress.
So (002) of PZT and (200) peak should be offset to same direction, and the phenomenon that we observe is to different direction skews.And as can be seen from Figure 5, two sample P ZT (30nm)/LNO/STO is identical with (002) peak position in PZT (150nm)/LNO/STO, illustrate that LNO/STO is basic identical to the stress of top PZT, (002) and the thickness of (200) peak position skew and PZT self have nothing to do, but be subject to the impact of top CFO layer.Because 1/2nd of CFO lattice parameter is greater than lattice parameter a and the b (table one) of PZT, thereby the CFO layer has applied tension stress in face (in-plane) to pzt thin film, make PZT the outer lattice parameter of face (out-of-plane, a on a farmland, corresponding to (200) peak; The c on c farmland, corresponding to (002) peak), along with the reduction of PZT thickness, reduce, (002) and (200) peak all should be to the skew of large angular direction.And the phenomenon of observing be (002) to large angular variation, (200) are to little angular variation.Similarly phenomenon also is found in the researchists' such as M.Murakami experiment.Yet the people such as M.Murakami move phenomenon by the peak of observing and are diffused into PbTiO owing to iron and cobalt ion
3in film, cause.Yet during to 300nm and 500nm, the phenomenon of observing is very interesting when the thickness that increases PZT.The CFO layer is arranged and compare without the CFO layer, the skew of (002) Xiang little angular direction, peak, the skew of Xiang great angular direction, (200) peak.The XRD diffraction spectrogram of measuring as shown in Figure 6.If explain with the diffusion of iron, cobalt ion, the offset direction at (002) and (200) peak should be contrary with the situation of Fig. 6.
Traditional stress mechanism only considers that two alternate lattice mismatches (also will consider the stress effect that the mismatch of coefficient of thermal expansion causes certainly.But the stress effect that the coefficient of thermal expansion mismatch causes is all identical concerning our series samples.So can not consider its impact).And the experimental result that the present invention observes can not explain with traditional stress mechanism, can not explain with the diffusion of iron, cobalt ion.Yet, if consider lattice mismatch and the original residing lattice gesture state of structure cell simultaneously, the experimental result that just the energy well explain is observed.
As seen from Figure 7, when the thickness of PZT is 100nm, have the ratio of CFO layer little without the residual polarization of CFO layer sample.As seen from Figure 8, when the thickness of PZT is 300nm, have the ratio of CFO layer large without the residual polarization of CFO layer sample, and increased approximately 175% left and right.(have document to point out, a farmland in ferroelectric material and c farmland are different to the contribution of surveyed residual polarization.Find out have, without in CFO layer sample from the XRD of Fig. 6, the ratio on c farmland and a farmland is substantially constant.So the residual polarization of surveying has comparability).From then on the test result of finding out ferroelectric hysteresis loop conforms to the situation that tetragonality develops.
The present invention has avoided tradition " stress engineering " dexterously needs the high request that film thickness is very thin, and only need prepare the pzt thin film layer that a, c ferroelectric domain coexist, and can put " oppositely " stress engineering to good use to thick pzt thin film.Under the prerequisite that significantly improves film performance, less demanding due to the present invention to film, therefore, increased the operability of production department greatly, greatly reduces production cost.
Claims (9)
1. one kind thicker ferroelectric membranc is implemented to the method for stress engineering for material modification, it is characterized in that: by adopting magnetron sputtering, in succession deposit LNO on the STO substrate
3bottom electrode, pzt thin film and CFO film,
And form the pzt thin film layer that a, c electricdomain coexist; Specifically by following 2 steps, formed:
Step 1: the preparation of sputtering target
Step 1.1:LNO ceramic target
By purity, be 99.9%La
2o
3and Ni
2o
3powder is pressed into block after by the La of 1: 1, Ni atomic ratio mixed grinding, and high temperature sintering, make LaNiO
3ceramic target;
Step 1.2:PZT ceramic target
By PbO, ZrO
2and TiO
2powder evenly mixes, press forming, and last sintering forms;
Step 1.3:CFO ceramic target
By CoO and Fe
2o
3press forming after the even mixed grinding of powder, the final high temperature sintering, make CoFe
2o
4ceramic target;
Step 2: the preparation of thin-film material
Step 2.1: the too sour strontium SrTiO of the monocrystalline that substrate is 100 orientations
3/ STO; Substrate first, with the ultrasonic cleaning that hockets of ethanol, acetone, is then carried out matting with trieline, finally in vacuum chamber, peels off cleaning with Ar Ion Beam Etching again;
Step 2.2: pass into argon gas and oxygen, carry out sputtering sedimentation LaNiO
3film, obtain the LNO film;
Step 2.3: by LaNiO
3target changes the PZT ceramic target into, and sputter cavity background is vacuumized, and will be coated with bottom electrode LaNiO simultaneously
3monocrystalline STO substrate heating, then pass into argon gas, carry out the sputtering sedimentation pzt thin film; Carry out respectively the sputtering operation of different time on different LNO/STO substrates, obtain the pzt thin film layer of different thickness;
Step 2.4: the pzt thin film sample of gained different thickness is put on the vacuum chamber substrate frame simultaneously, by sputter cavity background suction, by all samples heating, then passed into argon gas simultaneously, carry out sputtering sedimentation CFO film; Control sputtering time, make the CFO thin film layer that all covers one deck same thickness on all different thickness pzt thin film samples.
2. as claimed in claim 1ly a kind of thicker ferroelectric membranc is implemented to the method for stress engineering for material modification, it is characterized in that: in described step 1.1, block diameter * thickness is 60mm * 3mm, and the temperature of high temperature sintering is 1100 ℃, and the time of high temperature sintering is 3 hours.
3. a kind of method that thicker ferroelectric membranc enforcement stress engineering is used for to material modification as claimed in claim 1, is characterized in that: in described step 1.2, at PbO, ZrO
2and TiO
2the excessive Pb that adds 10%wt in powder.
4. as describedly as claim 1 or 3 a kind of thicker ferroelectric membranc is implemented to the method for stress engineering for material modification, it is characterized in that: in described step 1.2, sintering temperature is 900 ℃, and sintering time is 3 hours; PZT ceramic target size diameter * thickness of making is 60mm * 5mm, and the per-cent Zr of constituent content: Ti is 20: 80.
5. as claimed in claim 1ly a kind of thicker ferroelectric membranc is implemented to the method for stress engineering for material modification, it is characterized in that: in described step 1.3, the temperature of high temperature sintering is 1200 ℃, and the time of high temperature sintering is 3 hours.
6. as claimed in claim 1ly a kind of thicker ferroelectric membranc is implemented to the method for stress engineering for material modification, it is characterized in that: in described step 2.2, the processing condition of sputter-deposited thin films are as follows: base vacuum degree 5 * 10
-4pa, 400 ℃ of base reservoir temperatures, target-cardinal distance is from 7em, radio frequency power 80～100W.
7. as claimed in claim 1ly a kind of thicker ferroelectric membranc is implemented to the method for stress engineering for material modification, it is characterized in that: in described step 2.2, pass into argon gas and oxygen and keep air pressure at 1.6Pa, the LNO film thickness is 50nm, the in-situ sputtering deposition LaNiO obtained
3the resistivity of film is 7 * 10
-4Ω cm.
8. a kind of method that thicker ferroelectric membranc enforcement stress engineering is used for to material modification as claimed in claim 1, is characterized in that: in described step 2.3, sputter cavity background suction is extracted into to 5 * 10-4Pa, will be coated with bottom electrode LaNiO
3monocrystalline STO substrate be heated to 650 ℃, pass into argon gas and keep air pressure at 1.6Pa, carry out the sputtering operation of different time, can obtain the sample P ZT/LNO/STO that thickness is 30～150nm PZT layer.
9. as claimed in claim 8ly a kind of thicker ferroelectric membranc is implemented to the method for stress engineering for material modification, it is characterized in that: in described step 2.4, sputter cavity base vacuum degree is extracted into to 5 * 10-4Pa, all samples is heated to 650 ℃, pass into argon gas and keep air pressure at 1.6Pa, on the sample P ZT/LNO/STO that is 30～150nm PZT layer at thickness, carry out sputter CFO operation, the CFO thin film layer thickness obtained is 50nm.
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| CN104868048A (en) * | 2015-05-13 | 2015-08-26 | 重庆科技学院 | Photoinduced telescopic composite membrane and light driver made of photoinduced telescopic composite membrane |
| CN108281544A (en) * | 2018-01-26 | 2018-07-13 | 哈尔滨工业大学 | More resistance state ferroelectricity quantum tunneling knots and preparation method on farmland coexist based on ferroelectricity |
| CN108559954A (en) * | 2018-03-30 | 2018-09-21 | 湖北大学 | A kind of preparation method of negative expansion PZT thin film |
| CN113235159A (en) * | 2021-04-07 | 2021-08-10 | 兰州大学 | Method for preparing single crystal nickel ferrite film |
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| CN104868048A (en) * | 2015-05-13 | 2015-08-26 | 重庆科技学院 | Photoinduced telescopic composite membrane and light driver made of photoinduced telescopic composite membrane |
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| CN113235159B (en) * | 2021-04-07 | 2022-07-01 | 兰州大学 | Method for preparing single crystal nickel ferrite film |
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