CN111740009B - Piezoelectric wafer surface treatment method based on ion beam enhanced corrosion - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000010884 ion-beam technique Methods 0.000 title claims abstract description 12
- 230000007797 corrosion Effects 0.000 title claims abstract description 11
- 238000005260 corrosion Methods 0.000 title claims abstract description 11
- 238000004381 surface treatment Methods 0.000 title claims abstract description 8
- 150000002500 ions Chemical class 0.000 claims abstract description 56
- 230000007547 defect Effects 0.000 claims abstract description 35
- 230000003746 surface roughness Effects 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 230000002378 acidificating effect Effects 0.000 claims abstract description 10
- 238000005468 ion implantation Methods 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 12
- 238000010849 ion bombardment Methods 0.000 claims description 12
- 238000002513 implantation Methods 0.000 claims description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 claims description 3
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 2
- OBTSLRFPKIKXSZ-UHFFFAOYSA-N lithium potassium Chemical compound [Li].[K] OBTSLRFPKIKXSZ-UHFFFAOYSA-N 0.000 claims description 2
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 26
- 238000005530 etching Methods 0.000 description 15
- 239000010409 thin film Substances 0.000 description 12
- 239000000758 substrate Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 3
- 238000005280 amorphization Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010897 surface acoustic wave method Methods 0.000 description 2
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 1
- 229910003327 LiNbO3 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/08—Shaping or machining of piezoelectric or electrostrictive bodies
- H10N30/082—Shaping or machining of piezoelectric or electrostrictive bodies by etching, e.g. lithography
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/04—Treatments to modify a piezoelectric or electrostrictive property, e.g. polarisation characteristics, vibration characteristics or mode tuning
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Abstract
The invention relates to a piezoelectric wafer surface treatment method based on ion beam enhanced corrosion, which comprises the following steps: firstly, injecting He ions into the piezoelectric film to form a defect layer on the near surface of the piezoelectric film; then bombarding the surface of the wafer by using Ar ions to form a smooth surface; bombarding the surface of the wafer by using Kr ions to convert the defect layer into an amorphous layer; and finally, removing the formed amorphous layer by using acidic corrosive liquid for corrosion to obtain the film surface with low surface roughness. The method effectively reduces the surface roughness of the piezoelectric film, reduces the acoustic loss and the optical loss caused by the surface roughness, and has the advantages of simplicity, low cost and good application prospect.
Description
Technical Field
The invention belongs to the field of electronic components, and particularly relates to a piezoelectric wafer surface treatment method based on ion beam enhanced corrosion.
Background
With the development of 5G technology, the market of radio frequency front end modules of mobile communication terminals has rapidly increased. Acoustic wave filters based on surface acoustic wave and bulk acoustic wave technologies have become the fastest growing electronic components in radio frequency front end modules. However, with the release of new frequency bands and the application of Carrier Aggregation (CA) and Multiple Input Multiple Output (MIMO) technologies, the market places more demands on the size, power consumption, power, operating frequency, bandwidth, stability, and the like of the acoustic wave filter. Therefore, on the basis of the traditional acoustic wave filter based on the piezoelectric single crystal substrate, researchers adopt a heterogeneous composite substrate to improve the performance of the device and develop a novel working mode. However, at present, heterogeneous composite substrates for high-performance surface acoustic wave filters are prepared by an ion beam stripping technology, and the prepared thin film has a large number of implantation defects on the surface and large surface roughness, and cannot be directly used for device preparation. And because the supporting substrate and the piezoelectric film in the heterogeneous composite substrate have great thermal expansion coefficient mismatch, the prepared substrate The curvature of the bottom is large, and the surface treatment cannot be directly carried out by adopting the traditional chemical mechanical polishing process. Thus, university of electronic technology published a paper "Surface modifications of crystal-ion-sliced LiNbO3thin films by low energy irradiation ion radiations "proposed the use of bottom energy ion irradiation to reduce wafer surface roughness. However, this technique still has problems in that the surface roughness is still large, and in that irradiation with low-energy ions generates a large number of defect layers on the surface of the thin film.
Disclosure of Invention
The invention aims to solve the technical problem of providing a piezoelectric wafer surface treatment method based on ion beam enhanced corrosion, which overcomes the defect of poor surface roughness improvement effect in the prior art.
The invention provides a piezoelectric wafer surface treatment method based on ion beam enhanced corrosion, which comprises the following steps:
firstly, injecting He ions into the piezoelectric film to form a defect layer in the single crystal layer; then bombarding the surface of the wafer by using Ar ions to form a smooth surface; bombarding the surface of the wafer by using Kr ions to convert the defect layer into an amorphous layer; and finally, removing the formed amorphous layer by using acidic corrosive liquid for corrosion to obtain the film surface with low surface roughness.
The piezoelectric film is one or more of lithium niobate, lithium tantalate, potassium niobate and potassium lithium niobate.
The He ion implantation depth is 5% -15% of the total thickness of the piezoelectric film.
The energy of the Ar ions is 0.5-2 keV; the removal amount of Ar ion bombardment is 50 to 80 percent of the implantation depth of He ions.
The energy of the Kr ions is 0.5-10 keV; the sum of the removal amount of Ar ion bombardment and the removal amount of Kr ion bombardment is 1.05-1.2 times of the implantation depth of He ions; the unit atomic displacement dpa of Kr ion introduction is 0.3-0.7.
The acidic corrosive liquid comprises fluorine-based corrosive liquid, and the volume concentration of the acidic corrosive liquid is 1-25%.
Nitric acid is further added into the acidic corrosive liquid, and the volume ratio of the nitric acid to fluoride in the fluorine-based corrosive liquid is 1: 10-10: 1.
For the piezoelectric film with the initial surface roughness less than 5nm, He ion implantation can be omitted, and the sum of the Ar ion bombardment removal amount and the Kr ion bombardment removal amount is 5-15% of the total thickness of the film.
When the initial surface roughness of the piezoelectric thin film is large, for example, greater than 5nm, the surface roughness still fails to meet the requirement after Ar ions bombard the surface of the piezoelectric thin film (e.g., begins to deteriorate after decreasing from 8.7nm to 3.4 nm). In this case, the dose of Kr ions may be increased to increase the degree of damage to the film surface, i.e., dpa, and 0.8dpa may be used, for example. According to the article "Ion beam enhanced etching of LiNbO 3"it is known that a lithium niobate material can be completely amorphized when dpa is 0.4 or more. Further increasing the degree of amorphization can have two effects, 1. increasing the etch rate of the amorphous layer; 2. the etching selectivity of the amorphous layer and the single crystal layer is increased. In this case, the etching of the amorphous layer can be completed by using an etching solution having a smaller concentration, for example, 0.1%, and the influence on the single crystal layer can be reduced.
The method firstly utilizes He ions to inject a defect layer with uniform thickness into the piezoelectric film with rough surface. And then etching the surface of the film by using Ar ions, and using the single crystal layer on the surface of the film as a self-stopping layer so as to form a smooth surface. This step makes use of: a. the etching speed of the defect layer is different from that of the single crystal layer; b. the defect layer has no crystal structure and no anisotropy is generated. A surface of high defect density, i.e. an amorphous layer, is then formed using Kr ion bombardment. The method utilizes the advantages of heavy mass, shallow depth and large damage of Kr ions. Finally, the defect layer is removed by IBEE corrosion specific to the piezoelectric monocrystal, but the monocrystal layer is remained, so that a high-quality surface is obtained.
According to previous researches, the defect layer of the thin film after ion beam stripping is 5-25% of the total thickness of the piezoelectric layer. For example, the article "Wafer-Scale contamination of 42 ° Rotated Y-Cut LiTaO 3Panel four in on-insulator (LTOI) Substrate for a SAW susceptor "shows the defect layer at the surface region of the thin film. According to the method, a thickness layer to be removed is determined by He ion implantation, and the thickness of the total film is 5-15%. That is, He ion further enhances the originalDefect density of the defect layer. Subsequently, since the Ar ion etching still has a broad defect distribution, the defect layer formed by directly etching the He ions forms an Ar defect layer in the inner single crystal region. The Ar defect layer has two disadvantages, 1. distribution uniformity is worse than Kr defect layer; 2. the amorphization efficiency is lower than that of Kr. Therefore, at the moment, by utilizing the advantages of mature Ar ion irradiation etching technology, low Ar gas source cost and low ionization cost, a large number of defect layers are removed, and the surface roughness is optimized to be in an intermediate state. Finally, Kr ion irradiation with high cost and good effect is adopted to achieve the required effect, and the Kr etching depth and the Ar etching depth reach more than 1.05 times of He ion implantation, so that the original defects of ion beam stripping and the defects introduced by He ion implantation can be completely removed.
Advantageous effects
The method effectively reduces the surface roughness of the piezoelectric film, reduces the acoustic loss and the optical loss caused by the surface roughness, and has the advantages of simplicity, low cost and good application prospect.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a graph showing the surface roughness of a piezoelectric thin film after irradiation with Ar ions in example 1;
fig. 3 is a surface roughness test chart of the piezoelectric film after He ion implantation, irradiation of Ar ions and Kr ions, and HF etching in example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
1. And performing He ion implantation on the piezoelectric film stripped by the ion beam with the thickness of 550nm, so as to increase the defect density in the defect layer of the near-surface area of the piezoelectric film. The defect layer causes the piezoelectric film to form two regions with large mass difference, namely a defect layer on the near surface and a single crystal layer in the inner part. The defect layer preformed in the film through He ion implantation destroys the atomic arrangement of the original single crystal structure, and has the following three advantages that (1) the etching is more uniform than that of the single crystal structure; the anisotropy caused by different sputtering rates of different atoms is reduced; and inhibiting the channel effect in the subsequent process. In this embodiment, He ion implantation depth is 5% of the total thickness of the piezoelectric film.
2. Because the depth distribution of the injected He ions in the material is Gaussian distribution, the surface roughness of the film has certain influence on the depth distribution of the He ions. And bombarding the surface of the piezoelectric film implanted with the He ions by using Ar ions, wherein the energy of the Ar ions is 1keV, the implantation depth of the Ar ions is 2.4nm, and the ion implantation width is about 1.1 nm. Because Ar ions have a larger atomic mass, they have a stronger etch. The Ar ions have a faster etching speed for the area with more defects, so that the near-surface area can be removed quickly. With the etching selectivity of the Ar ions, the defect layer is gradually increased. As shown in fig. 2, the surface roughness of the piezoelectric thin film was reduced to 5nm after the irradiation of Ar ions.
3. Since Ar ions do not completely improve the surface roughness of the thin film, bombardment continues with Kr ions of greater atomic mass. The irradiation with Kr ions is mainly for improving the surface roughness, and thus the energy of Kr ions is selected to be 1 keV. Irradiation was performed using Kr ions, the ion implantation depth was 2.4nm, the ion implantation width was about 0.9nm, and the unit atomic displacement dpa introduced by Kr ions was 0.3. The lower implantation width can effectively improve the uniformity of the defect layer.
4. Finally, 1% acid corrosive liquid such as HF or HF: HNO is adopted3The solution corrodes the defect layer and removes the formed amorphous layer to obtain a thin film surface with low surface roughness, as shown in fig. 3, the surface roughness is 0.86 nm.
Example 2
1. When the initial surface roughness of the piezoelectric film is less than 5nm, Ar ions are directly used for bombarding the surface of the piezoelectric film, the energy of the Ar ions is 0.5keV, the implantation depth of the Ar ions is 1.7nm, and the ion implantation width is about 0.7 nm.
2. The energy of the Kr ion selected is 0.5 keV. Irradiation was performed using Kr ions, the ion implantation depth was 1.2nm, the ion implantation width was about 0.4nm, and the unit atomic displacement dpa introduced by Kr ions was 0.3.
When the initial surface roughness of the piezoelectric film is less than 5nm, the surface has a smaller roughness after Ar ion bombardment on the surface of the piezoelectric film, and then Kr ion bombardment with a lower dose can be adopted, for example dpa is 0.3. At the moment, the etching thickness can be reduced and the utilization rate of the piezoelectric film can be increased by adopting Kr ion bombardment with smaller dose, and the machine time can be saved.
3. Finally, 1% acidic corrosive liquid such as HF or HF: HNO is adopted3The solution etches the defect layer and removes the formed amorphous layer, and the thin film surface with low surface roughness can be obtained.
Claims (6)
1. A piezoelectric wafer surface treatment method based on ion beam enhanced corrosion comprises the following steps:
firstly, injecting He ions into the piezoelectric film to form a defect layer in the single crystal layer; then bombarding the surface of the wafer by using Ar ions to form a smooth surface; bombarding the surface of the wafer by using Kr ions to convert the defect layer into an amorphous layer; finally, removing the formed amorphous layer by using acidic corrosive liquid for corrosion to obtain a film surface with low surface roughness; the piezoelectric film is one or more of lithium niobate, lithium tantalate, potassium niobate and potassium lithium niobate.
2. The method of claim 1, wherein: the He ion implantation depth is 5% -15% of the total thickness of the piezoelectric film.
3. The method of claim 1, wherein: the energy of the Ar ions is 0.5-2 keV; the removal amount of Ar ion bombardment is 50 to 80 percent of the implantation depth of He ions.
4. The method of claim 1, wherein: the energy of the Kr ions is 1-10 keV; the sum of the removal amount of Ar ion bombardment and the removal amount of Kr ion bombardment is 1.05-1.2 times of the implantation depth of He ions; the unit atomic displacement dpa of Kr ion introduction is 0.3-0.7.
5. The method of claim 1, wherein: the acidic corrosive liquid comprises fluorine-based corrosive liquid, and the volume concentration of the acidic corrosive liquid is 0.1-25%.
6. The method of claim 5, wherein: nitric acid is further added into the acidic corrosive liquid, and the volume ratio of the nitric acid to fluoride in the fluorine-based corrosive liquid is 1: 10-10: 1.
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