CN114836836B - Local rapid blackening method for lithium niobate wafer/lithium tantalate wafer - Google Patents
Local rapid blackening method for lithium niobate wafer/lithium tantalate wafer Download PDFInfo
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- CN114836836B CN114836836B CN202210716285.3A CN202210716285A CN114836836B CN 114836836 B CN114836836 B CN 114836836B CN 202210716285 A CN202210716285 A CN 202210716285A CN 114836836 B CN114836836 B CN 114836836B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/30—Niobates; Vanadates; Tantalates
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Abstract
The invention discloses a local rapid blackening method of a lithium niobate wafer/lithium tantalate wafer, which comprises the following steps: (1) Placing the polished lithium niobate wafer or lithium tantalate wafer in a sealing device, and filling reducing gas; (2) And (3) according to the set pattern, laser is used for undershooting Jiao Zhaoshe the lithium niobate wafer or the lithium tantalate wafer, inert gas is introduced, and reducing gas is discharged, so that the locally blackened wafer is obtained. The parameters of the laser under-focus are as follows: the laser wavelength is 1064nm, the laser power is 4-10W, the under-focus distance is 0.50-2.50 cm, and the scanning speed is 100-600 mm/s. According to the invention, the lithium niobate wafer or the lithium tantalate wafer is irradiated by laser in a reducing gas atmosphere, so that the blackening of the wafer can be realized rapidly, and the blackening area can be selected, so that the purpose of localized blackening is achieved.
Description
Technical Field
The invention relates to the technical field of wafer blackening, in particular to a local rapid blackening method for a lithium niobate wafer/lithium tantalate wafer.
Background
Lithium niobate and lithium tantalate crystals are widely used as piezoelectric substrates in devices such as high-frequency broadband filters and the like due to their excellent piezoelectric effect and photorefractive effect. Among the two kinds of crystals, lithium tantalate has absolute advantages in manufacturing Surface Acoustic Wave (SAW) devices below 3Ghz, and lithium niobate has considerable potential in developing high-power and large-bandwidth filters. However, the lithium niobate and lithium tantalate crystals have the properties of high pyroelectric property, high light transmission and the like, the high pyroelectric property can lead to the formation of a large amount of static charges, and the static charges accumulated to a certain degree can generate a discharge phenomenon, thereby damaging a wafer or burning out an electrode; the high light transmittance characteristic can cause problems such as linewidth distortion in the photoetching process. In view of these problems, some chemical reduction processes are proposed internationally, and by utilizing the property that oxygen atoms in lithium niobate and lithium tantalate crystals are easier to escape from crystal lattice to form oxygen vacancies under the reduction action, the oxygen vacancies can obtain an electron to form an F color center (F+), and the F color center has strong absorption to visible light, so that the wafer is changed from colorless transparent to brown or black after being subjected to reduction treatment, and we call the wafer subjected to reduction treatment a black sheet. The black sheet has lower pyroelectric effect and higher conductivity, so that the yield is higher in the processing process, and meanwhile, the black sheet relieves the problems of line width distortion and the like caused by high light transmittance.
At present, the main technical route for preparing the lithium niobate and lithium tantalate black sheets is to embed the lithium niobate and lithium tantalate wafers in reducing powder (such as carbon powder and iron powder), introduce inert or reducing gas for protection, and heat up to prepare the black sheets. The conventional reduction powder is used for blackening the wafer, so that the problems of uneven degree of wafer blackening, complex operation, long blackening time, low efficiency and the like exist. In recent years, methods such as plasma etching, ion implantation, molten salt and the like are increasingly developed. The plasma etching technique dissociates the reducing gas introduced into the chamber into a very reducing plasma for wafer reduction. Ion implantation can implant a chemically reactive species into the target, thereby achieving the purpose of reducing the wafer. Although both of these approaches can achieve blackening of the lithium niobate wafer. However, both of these methods are to realize the blackening of the whole wafer, if the local blackening is required, the pattern needs to be defined by combining the photolithography process, the equipment required by these methods is expensive, and the local blackening cannot be realized in one step. There is a need for a simple method that can rapidly locally blacken lithium niobate, lithium tantalate wafers.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a local rapid blackening method for a lithium niobate wafer/lithium tantalate wafer. According to the invention, the lithium niobate wafer or the lithium tantalate wafer is irradiated by laser in a reducing gas atmosphere, so that the blackening of the lithium niobate wafer or the lithium tantalate wafer can be realized rapidly, and the blackening area can be selected, so that the purpose of localized blackening is achieved.
In order to achieve the above purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, there is provided a method for localized rapid blackening of a lithium niobate wafer/lithium tantalate wafer, comprising the steps of:
(1) Placing the polished lithium niobate wafer or lithium tantalate wafer in a sealing device, and filling reducing gas;
(2) And (3) according to the set pattern, laser is used for undershooting Jiao Zhaoshe the lithium niobate wafer or the lithium tantalate wafer, inert gas is introduced, and reducing gas is discharged, so that the locally blackened lithium niobate wafer or the lithium tantalate wafer is obtained.
The parameters of the laser are adjusted to enable the laser to irradiate the lithium niobate wafer or the lithium tantalate wafer in an under-focus mode, the temperature of the lithium niobate wafer or the lithium tantalate wafer is increased through the thermal effect generated by the under-focus of the laser, oxygen atoms in crystal lattice on the surface layer of the wafer escape from the crystal lattice under the action of reducing gas introduced into a sealing device under the high-temperature condition to form oxygen vacancies, the oxygen vacancies can obtain an electron to form an F color center (F+), the F color center absorbs visible light more strongly, the wafer is changed from colorless transparent to brown or black after reduction treatment, and the blackened lithium niobate wafer or the blackened lithium tantalate wafer is obtained, and the local blackened wafer is realized according to the design of laser irradiation patterns.
Because of the localized nature of the laser action, the thermal effects do not affect the immediately adjacent non-blackened portions. There are two approaches by which the immediate non-blackened portion may be affected by the blackened area: heating in the laser irradiation process, and blackening to a certain extent; oxygen atoms in the non-blackened sites migrate into the holes of the blackened sites. Both processes, however, also require higher temperatures to be reached. The laser action is localized, and the temperature satisfying the condition is not generated in the immediate vicinity of the design pattern, so that the laser action is not affected.
Preferably, in the step (1), the sealing device is a photo-thermal reaction kettle; the photo-thermal reaction kettle is provided with a light-transmitting window, and the light-transmitting window is made of quartz glass or zinc selenide glass.
The photo-thermal reaction kettle has the characteristics of high temperature resistance, high pressure resistance and good sealing performance, and avoids the danger caused by the reaction of air entering the reaction kettle and reducing gas. And a mechanical vacuum pump is used for pumping gas, so that the accuracy of gas tightness detection is ensured.
The material of the reaction kettle can be one of stainless steel, glass and polytetrafluoroethylene or a sealing material with the same function.
The light transmission window can ensure laser incidence, and the material of the reaction kettle ensures that the reaction kettle is resistant to high temperature and high pressure.
Preferably, in step (1), the reducing gas is hydrogen, methane or argon-hydrogen mixture.
When the reducing gas is filled, the reducing gas is repeatedly filled into the reaction kettle for two times according to the steps of filling and extracting, and then the reducing gas is filled again, so that the purity of the reducing gas in the reaction kettle is ensured.
Preferably, in step (2), the parameters of the laser under-focus are: the wavelength of the laser is 1064nm, the laser power is 4-10W, the under-focus distance is 0.50-2.50 cm, and the scanning speed is 100-600 mm/s, so that the lithium niobate wafer/lithium tantalate wafer can be heated up rapidly under the irradiation of the laser.
In a second aspect of the present invention, there is provided a localized blackened wafer prepared by a lithium niobate wafer/lithium tantalate wafer localized rapid blacking method.
Preferably, the locally blackened pattern is a square, line, circle, dot matrix or text.
The invention has the beneficial effects that:
(1) The invention adopts laser to irradiate the lithium niobate wafer/lithium tantalate wafer, the area irradiated by the laser is quickly heated, and the area is directly reacted with reducing gas in the reaction kettle, thereby realizing the blackening of the lithium niobate wafer/lithium tantalate wafer. The laser irradiation can realize instant heating, compared with the heating of a plurality of hours in the traditional method, the blackening time is greatly shortened, the process period is short, and the method is simple and efficient.
(2) The diameter of the laser spot depends on the under-focus distance, and when the under-focus distance is 0.5cm, the diameter of the laser spot is 100 mu m, so that the smallest area acting on the wafer is a circular area with the diameter of 100 mu m, the blackening of the controllable area can be realized by editing a laser scanning path through software, and the local blackening of the wafer can be further realized.
(3) According to the invention, the temperature is raised by laser irradiation, and the lithium niobate wafer/lithium tantalate wafer is reduced by the reducing gas, so that the phenomenon of blackening non-uniformity caused by non-uniform contact between the reducing powder and the wafer in the traditional mode is avoided; the uniformity of local blackening of the wafer can be ensured. Meanwhile, the invention adopts the reducing gas to reduce the lithium niobate wafer/lithium tantalate wafer, and the reduced wafer avoids the problem that the reduced powder blackened wafer is difficult to clean.
Drawings
FIG. 1 is a schematic diagram of a laser reduced blackened lithium niobate device. The figure shows: 1. the laser device comprises a laser device 2, laser beams 3, a quartz window 4, an upper bolt hole 5, a pressure gauge 6, a lower bolt hole 7, an air inlet 8, an air outlet 9 and a reaction cavity.
Fig. 2 is a laser blackened lithium niobate wafer of example 1.
FIG. 3 is an SEM image of a sample before (a) and after (b) and after (c) laser focusing treatment of example 1 laser-blackened lithium niobate wafer
Fig. 4 is a laser patterned lithium niobate wafer of example 2.
Fig. 5 is a laser interdigital electrode blackened lithium tantalate wafer of example 3.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
In order to enable those skilled in the art to more clearly understand the technical solutions of the present application, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and are commercially available.
Example 1
The embodiment discloses a method for local rapid blackening of a lithium niobate wafer, which adopts a reaction kettle structure as shown in figure 1 and comprises the following implementation steps:
(1) Preparation of lithium niobate wafer for polishing treatment under pressure of 8psi with SiO 2 Grinding materials, polishing leather by using chamois leather, and carrying out chemical mechanical polishing treatment on the lithium niobate wafer at the rotating speed of 60 r/min; when there is a case where polishing of the lithium niobate wafer is uneven, a difference in laser absorption is caused, resulting in a slight difference in blackening degree. Therefore, before blackening, it is necessary to examine the polishing degree of the wafer by a microscope, and if polishing is uneven, the polishing may be performed again and then the blackening may be performed again.
(2) Sealing the wafer: and placing the lithium niobate wafer to be treated into a reaction cavity, and sealing the high-pressure reaction kettle by screwing the upper bolt hole and the lower bolt hole.
(3) And (3) testing air tightness: and adopting a vacuum pump to pump gas in the reaction cavity, spraying a leak detection agent at the gas valve and the opening of the metal high-pressure reaction kettle for leak detection, and observing for 5 minutes to show that the reading of the barometer of the gas pressure in the metal high-pressure reaction kettle does not rise so as to determine that the gas tightness of the metal high-pressure reaction kettle is good.
(4) The reaction chamber is filled with reducing gas: opening an air inlet and an air outlet of the reaction kettle, continuously introducing argon/hydrogen (volume ratio: 85%: 15%) at a flow rate of 15sccm, closing the air inlet, connecting a vacuum pump and a tail gas treatment device to the air outlet, pumping out reducing gas, and repeating the inflation and the pumping for two times to ensure that the air in the reaction cavity is completely discharged, and re-filling the argon/hydrogen (volume ratio: 85%: 15%).
(5) Setting laser parameters: nd with an output wavelength of 1064 nm: YAG laser, which is equipped with a polarizer to adjust the laser emitting direction, setting the laser power to 4W, under-focusing to 1.50cm, and scanning speed to 150mm/s, and drawing 1cm×1cm blackened area in marking software.
(6) Laser reduction blackening: the laser beam emitted by the laser irradiates the lithium niobate wafer in the reaction cavity through the quartz window of the reaction kettle in an under-focus way, and the laser beam scans point by point according to a set area of 1cm multiplied by 1 cm.
(7) Taking a piece: the gas outlet is connected with a vacuum pump and a tail gas processor, argon is introduced into the gas inlet at a flow rate of 50sccm for five minutes, and then the high-pressure reaction kettle is opened to obtain a lithium niobate black sheet, and the lithium niobate wafer is uniformly blackened in a 1cm multiplied by 1cm area. As shown in fig. 2.
In order to verify the principle of blackening the laser lithium niobate, a lithium niobate sample irradiated by laser focusing under the same condition is introduced as a comparison sample. It can be seen that there is no significant difference in the smoothness of the surface of the laser under-focus irradiated wafer compared to the untreated wafer surface, as shown in fig. 3 (a) (b). And the surface of the lithium niobate wafer irradiated by laser focusing is roughened as shown in fig. 3 (c). Therefore, when the lithium niobate wafer is subjected to laser under-focus treatment, a thermal effect is generated, the lithium niobate wafer is heated by the thermal effect, oxygen atoms in crystal lattices on the surface layer of the lithium niobate wafer escape from the crystal lattice under the action of reducing gas introduced into a closed device to form oxygen vacancies, the oxygen vacancies can obtain an electron to form an F color center (F+), the F color center has strong absorption to visible light, and the wafer is changed from colorless transparent to brown or black after reduction treatment. This is quite different from conventional laser focus irradiation of the substrate to coarsen and blacken the substrate.
Example 2
The present invention differs from example 1 in that the laser output pattern parameter in step (5) is changed to "LNO". The resulting patterned "blackened" lithium niobate wafer is shown in fig. 4, and it can be seen that the uniform blackened "LNO" pattern is formed on the lithium niobate wafer.
Example 3
The present invention is different from example 1 in that the lithium tantalate wafer is subjected to polishing treatment by the method of step (1); in the step (5), the laser output pattern parameter is changed into the shape of the interdigital electrode, and the obtained patterned blackened lithium tantalate wafer is shown in fig. 5, and it can be seen that uniform blackened interdigital electrodes are formed on the lithium tantalate wafer.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (4)
1. The local rapid blackening method for the lithium niobate wafer/lithium tantalate wafer is characterized by comprising the following steps of:
(1) Placing the polished lithium niobate wafer or lithium tantalate wafer in a sealing device, and filling reducing gas;
(2) And (3) according to the set pattern, laser is used for undershooting Jiao Zhaoshe the lithium niobate wafer or the lithium tantalate wafer, inert gas is introduced, and reducing gas is discharged, so that the locally blackened lithium niobate wafer or the locally blackened lithium tantalate wafer is obtained.
2. The method for localized rapid blackening of lithium niobate/lithium tantalate wafers according to claim 1, wherein in step (1), the sealing device is a photo-thermal reaction kettle; the photo-thermal reaction kettle is provided with a light-transmitting window, and the light-transmitting window is made of quartz glass or zinc selenide glass.
3. The method for localized rapid blackening of lithium niobate/lithium tantalate wafers of claim 1, wherein in step (1), the reducing gas is hydrogen, methane, or argon-hydrogen mixture.
4. The method for localized rapid blackening of lithium niobate/lithium tantalate wafers of claim 1 wherein in step (2), the parameters of the laser under-focus are: the laser wavelength is 1064nm, the laser power is 4-10W, the under-focus distance is 0.50-2.50 cm, and the scanning speed is 100-600 mm/s.
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| CN117444381B (en) * | 2023-11-02 | 2024-06-04 | 深圳技术大学 | Method for preparing conductive microstructure on surface of lithium niobate crystal based on femtosecond laser direct writing technology |
| CN117403326B (en) * | 2023-12-13 | 2024-02-20 | 天通控股股份有限公司 | Whitening method for lithium tantalate blackened wafer |
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| CN101824653B (en) * | 2009-03-04 | 2012-03-28 | 中国科学院半导体研究所 | Method for manufacturing black silicon material by scanning and irradiation of light source of broad-pulse laser |
| CN101908591A (en) * | 2010-06-23 | 2010-12-08 | 山东华光光电子有限公司 | Preparation method for ohmic contact electrode for LED with SiC substrate |
| CN103586578B (en) * | 2013-11-14 | 2016-08-31 | 苏州图森激光有限公司 | A kind of material surface laser melanism or color method |
| JP6256955B2 (en) * | 2016-01-07 | 2018-01-10 | 信越化学工業株式会社 | Method for producing lithium tantalate single crystal substrate |
| CN110835781B (en) * | 2018-08-16 | 2021-08-31 | 江南石墨烯研究院 | Blackening method of lithium niobate or lithium tantalate wafer |
| CN112310214B (en) * | 2019-07-31 | 2021-09-24 | 复旦大学 | Nonvolatile ferroelectric memory and preparation method thereof |
| CN111962156A (en) * | 2020-08-06 | 2020-11-20 | 武汉大学 | Method for repairing single crystal diamond crystal structure based on ultrashort pulse laser |
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