CN102304767A - Method for preparing lithium niobate surface pattern - Google Patents

Method for preparing lithium niobate surface pattern Download PDF

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Publication number
CN102304767A
CN102304767A CN201110245639A CN201110245639A CN102304767A CN 102304767 A CN102304767 A CN 102304767A CN 201110245639 A CN201110245639 A CN 201110245639A CN 201110245639 A CN201110245639 A CN 201110245639A CN 102304767 A CN102304767 A CN 102304767A
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lithium
niobium trioxide
plasma
preparing
lithium niobate
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郑婉华
齐爱谊
王海玲
渠红伟
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Institute of Semiconductors of CAS
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Abstract

The invention discloses a method for preparing a lithium niobate surface figure. The method comprises the following steps of: manufacturing a mask pattern on the surface of a lithium niobate substrate; performing dry etching on the lithium niobate substrate by using fluorine plasma to etch lithium niobate; etching the lithium niobate substrate by using oxygen plasma to etch lithium fluoride formed on the surface of the lithium niobate; repeating the etching steps in which the fluorine plasma and the oxygen plasma are used, until the preparation of the lithium niobate surface pattern is finished. By the method, the problem that the lithium fluoride is redeposited on the surface when the lithium niobate is etched by the fluorine plasma is solved; and the lithium niobate surface pattern with large depth and a smooth bottom surface is prepared. The method is simple and easy to implement and can be used for etching the lithium niobate, so that the lithium niobate surface figure with the large depth and the smooth bottom surface is obtained.

Description

A kind of method for preparing the Lithium niobium trioxide surfacial pattern
Technical field
The present invention relates to field of IC technique, disclose a kind of method for preparing the Lithium niobium trioxide surfacial pattern.
Background technology
Lithium niobium trioxide (Lithium Niobate, LiNbO 3) material is the ferroelectric material (ferrolectric) of synthetic.Utilize (Czochralski) method that lifts successfully to grow since the lithium niobate crystals from nineteen sixty-five Batlman, this " universal " (versatile), " clever " crystal (clever) receives people's attention always.Why the Lithium niobium trioxide material receives and paying close attention to widely is because material itself has special optical characteristics; Electrooptic effect (electro-optic effect) for example, acoustooptic effect (acousto-optic effect) and piezoelectric effect (piezoelectric effect) etc.
The Lithium niobium trioxide waveguide can be used for making high-speed modulation device and nonlinear device, for example parametric oscillator (parametric oscillator) and amplifier (amplifiers).Because material has higher electro-optic coefficient and lower optical loss, Lithium niobium trioxide also is often used in the telecommunication system again.The size that the photonic crystal that adopts Lithium niobium trioxide to make can also dwindle Primary Component in some optical system greatly.The Lithium niobium trioxide of the high vertical wide ratio of submicron order can also be processed mini-prober (microsensors), directional coupler (directional couplers), ultra-compact electrooptic modulator (electro-optic modulators) and wavelength filter.
Forming perfect figure on the Lithium niobium trioxide surface is the basis of each element manufacturing, and people also recognize the importance of making method gradually.But micro-nano complete processing gained result aspect the making of Lithium niobium trioxide surfacial pattern commonly used at present is unsatisfactory.
Plasma etching is swift and violent in development in recent years, brings very big improvement for the Lithium niobium trioxide manufacture craft.Adopt plasma method on the Lithium niobium trioxide surface, not only to obtain the large size figure at present, like waveguide; Also obtained meticulousr figure, like photonic crystal.Fluoridize niobate, in the time of 200 ℃, have volatility preferably,, comprise SF so the plasma body that adopts fluorine-containing (F) gas to form usually carries out the plasma dry etching to Lithium niobium trioxide 6, CF 4, CHF 3Deng.In order to strengthen the physical bombardment of plasma to material surface, balance physics and chemical action can add O usually 2, assist gas such as He, Ar.
But; The Lithium niobium trioxide plasma etch rate is lower; According to document 1: " N.Mitsugi; H.Nagata; K.Shima; and M.Tamai; J.Vac.Sci.Technol.A 16; 2245 (1998) " and document 2: " G.Y.Si andA.J.Danner; Int.J.Nanoscienc 9,311 (2010) " report, think mainly to be; lithium fluoride will stop the further etching to Lithium niobium trioxide, make etching depth smaller because Lithium niobium trioxide surface can depositing fluorinated again lithium (848 ℃ of fusing points) in plasma etching.In addition, lithium fluoride is deposited on the surface and also causes surface irregularity easily, forms microspike (whisker) on the surface, is the key process technology of the Lithium niobium trioxide material being lost and obtains smooth bottom surface deeply so how to remove the sedimentary lithium fluoride of substrate surface.
Summary of the invention
(1) technical problem that will solve
In view of this, main purpose of the present invention is to provide a kind of method for preparing the Lithium niobium trioxide surfacial pattern, and the surface problem of depositing fluorinated lithium again when solving fluorine-based plasma etching Lithium niobium trioxide reaches the purpose of the big degree of depth of preparation, the smooth Lithium niobium trioxide surfacial pattern in bottom surface.
(2) technical scheme
For achieving the above object, the invention provides a kind of method for preparing the Lithium niobium trioxide surfacial pattern, this method comprises: make mask pattern on the lithium niobate substrate surface; Adopt fluorine-based plasma that lithium niobate substrate is carried out dry etching, with the etching Lithium niobium trioxide; Adopt oxygen plasma that lithium niobate substrate is carried out etching, to be etched in the lithium fluoride that the Lithium niobium trioxide surface forms; Repeat the etch step of fluorine-based plasma of above-mentioned employing and oxygen plasma, until the preparation of accomplishing the Lithium niobium trioxide surfacial pattern.
(3) beneficial effect
Can find out that from technique scheme the present invention has following beneficial effect:
1, this method for preparing the Lithium niobium trioxide surfacial pattern provided by the invention; Adopt fluorine-based plasma that lithium niobate substrate is carried out dry etching with the etching Lithium niobium trioxide; Adopt oxygen plasma that lithium niobate substrate is carried out etching to be etched in the lithium fluoride that the Lithium niobium trioxide surface forms then; The surface problem of depositing fluorinated lithium again when having solved fluorine-based plasma etching Lithium niobium trioxide reaches the purpose of the big degree of depth of preparation, the smooth Lithium niobium trioxide surfacial pattern in bottom surface.
2, this method for preparing the Lithium niobium trioxide surfacial pattern provided by the invention; Low, the depositing fluorinated again lithium in surface of etch rate when having solved fluorine-based plasma etching Lithium niobium trioxide, can't obtain the problem of big degree of depth surfacial pattern; Reach the purpose of the big degree of depth of preparation, the smooth Lithium niobium trioxide surfacial pattern in bottom surface, realized the preparation of Lithium niobium trioxide surfacial pattern.
3, this method for preparing the Lithium niobium trioxide surfacial pattern provided by the invention realizes two kinds of isoionic etchings simultaneously in plasma etching equipment, and the plasma etching equipment distribution extensively, is simple and easy to use.
4, this method for preparing the Lithium niobium trioxide surfacial pattern provided by the invention, oxygen plasma can etch away the sedimentary again lithium fluoride in surface, helps etching end back substrate surface mask and peels off.
5, this method for preparing the Lithium niobium trioxide surfacial pattern provided by the invention can improve the etch rate of Lithium niobium trioxide, obtains the surfacial pattern of the big degree of depth.
6, this method for preparing the Lithium niobium trioxide surfacial pattern provided by the invention is compared with the method for wet etching Lithium niobium trioxide, and the pattern side wall that obtains is more steep.
7, this method for preparing the Lithium niobium trioxide surfacial pattern provided by the invention can reduce the influence of lithium fluoride to etching, alleviates lithium fluoride to the sheltering of bottom surface, and avoids the formation of surperficial microspike, obtains bottom surface surfacial pattern Paint Gloss.
Description of drawings
Fig. 1 is the lithium niobate substrate with surfacial pattern mask provided by the invention.
Fig. 2 is the lithium niobate substrate behind the fluorine-based plasma etching of substrate process among Fig. 1 provided by the invention.
Fig. 3 is the lithium niobate substrate after the substrate process oxygen plasma etching among Fig. 2 provided by the invention.
Fig. 4 is provided by the invention through the lithium niobate substrate after the cycle repeats etching.
Figure: 1 lithium niobate substrate; 2 mask material; 3
Figure BDA0000085836540000033
lithium fluoride
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, to further explain of the present invention.
A kind of method for preparing the Lithium niobium trioxide surfacial pattern provided by the invention; This method at first adopts fluorine-based plasma that lithium niobate substrate is carried out dry etching with the etching Lithium niobium trioxide; Adopt oxygen plasma that lithium niobate substrate is carried out etching to be etched in the lithium fluoride that the Lithium niobium trioxide surface forms then; The surface problem of depositing fluorinated lithium again when having solved fluorine-based plasma etching Lithium niobium trioxide; Two etch step can repeated multiple times be carried out, and can obtain the big degree of depth, the slick Lithium niobium trioxide surfacial pattern in bottom surface.
Wherein, make mask pattern, adopt micro-nano processing method to carry out on the lithium niobate substrate surface.Micro-nano processing method possibly comprise: photoetching, electron beam exposure, evaporation, sputter, focused-ion-beam lithography, plasma etching etc. can be used for making the method for mask.
Lithium niobate substrate adopts lithium niobate crystals to be made, and mask pattern is shifted by the surperficial mask patterns of making on the lithium niobate substrate surface, and surperficial mask adopts metal or non-metallic material to be made.
Fluorine-based plasma is the high density plasma that is produced by fluoro-gas glow discharge, and oxygen plasma is the high density plasma that is produced by oxygen glow discharge.
The said etch step that repeats fluorine-based plasma of above-mentioned employing and oxygen plasma is two kinds of plasma bodys of fluorine-based plasma of repeated using and oxygen plasma to lithium niobate substrate carry out repeatedly, multiple etching.The Lithium niobium trioxide surfacial pattern of said preparation, its degree of depth are repeatedly fluorine-based plasma etching gained degree of depth sums.
As shown in Figure 1, Fig. 1 is the lithium niobate substrate with surfacial pattern mask provided by the invention, and the substrate mask can adopt metal or non-metallic material, and mask pattern obtains through micro-nano processing methods such as photoetching, electron beam exposure, focused ion beams.
As shown in Figure 2, Fig. 2 be among Fig. 1 substrate through gained substrate behind the fluorine-based plasma etching, surface deposition one deck lithium fluoride, lithium fluoride can stop fluorine-based isoionic etching, makes etch rate slack-off; Lithium fluoride is non-uniformly distributed in substrate surface, also can make the surface form microspike, causes the figure bottom surface coarse.
As shown in Figure 3, Fig. 3 is that substrate is through gained substrate after the oxygen plasma etching among Fig. 2, and etching is removed with the sedimentary again lithium fluoride in rear surface, and mask window comes out again.
As shown in Figure 4, Fig. 4 is through the bigger Lithium niobium trioxide surfacial pattern of the degree of depth that obtains after fluorine-based plasma and the oxygen plasma repeated multiple times etching, and the figure degree of depth is fluorine-based plasma etching gained degree of depth sum repeatedly, and surperficial mask is equally by the plasma etching attenuation.
Embodiment
In this instance, obtaining the degree of depth through this method for preparing the Lithium niobium trioxide surfacial pattern is 1.2 μ m Lithium niobium trioxide waveguides, and this method may further comprise the steps:
1, at first makes thick chromium (Cr) the metal mask figure of one deck 200nm on the lithium niobate substrate surface through methods such as electron beam evaporation, optical exposures.Shown in accompanying drawing 1.
2, with substrate shown in Figure 1 in ICP equipment, adopt CF 4/ Ar plasma etching 4min obtains the dark Lithium niobium trioxide surfacial pattern of 600nm.The plasma condition that adopts is following: CF 4Be respectively 40sccm and 20sccm with the flow of Ar, ICP source power and substrate bias power are respectively 500W and 200W, and chamber pressure is 25mTorr, and underlayer temperature is set at 5 ℃.Obtain structure as shown in Figure 2, the surface has deposited one deck LiF again.
3, continue substrate shown in Figure 2 etching 20s in oxygen plasma is obtained substrate as shown in Figure 3, Surface L iF is removed.The plasma condition that adopts is following: 30sccm O 2, the ICP source power is 600W, substrate bias power is 0.Chamber pressure is 20mTorr.
4, repeat 2,3 liang of steps, surfacial pattern is further deepened, finally obtain the about 1.2 μ m Lithium niobium trioxide ridge waveguides of the degree of depth, as shown in Figure 4.
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain; Institute is understood that; The above only is a specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (10)

1. a method for preparing the Lithium niobium trioxide surfacial pattern is characterized in that, this method comprises:
Make mask pattern on the lithium niobate substrate surface;
Adopt fluorine-based plasma that lithium niobate substrate is carried out dry etching, with the etching Lithium niobium trioxide;
Adopt oxygen plasma that lithium niobate substrate is carried out etching, to be etched in the lithium fluoride that the Lithium niobium trioxide surface forms;
Repeat the etch step of fluorine-based plasma of above-mentioned employing and oxygen plasma, until the preparation of accomplishing the Lithium niobium trioxide surfacial pattern.
2. the method for preparing the Lithium niobium trioxide surfacial pattern according to claim 1 is characterized in that, and is said at lithium niobate substrate surface making mask pattern, adopts micro-nano processing method to carry out.
3. the method for preparing the Lithium niobium trioxide surfacial pattern according to claim 2 is characterized in that, said micro-nano processing method comprises: photoetching, electron beam exposure, evaporation, sputter, focused-ion-beam lithography or plasma etching.
4. the method for preparing the Lithium niobium trioxide surfacial pattern according to claim 1 is characterized in that, said lithium niobate substrate adopts lithium niobate crystals to be made.
5. the method for preparing the Lithium niobium trioxide surfacial pattern according to claim 1 is characterized in that, said mask pattern is shifted by the surperficial mask patterns of making on the lithium niobate substrate surface.
6. the method for preparing the Lithium niobium trioxide surfacial pattern according to claim 5 is characterized in that, said surperficial mask adopts metal or non-metallic material to be made.
7. the method for preparing the Lithium niobium trioxide surfacial pattern according to claim 1 is characterized in that, said fluorine-based plasma is the high density plasma that is produced by fluoro-gas glow discharge.
8. the method for preparing the Lithium niobium trioxide surfacial pattern according to claim 1 is characterized in that, said oxygen plasma is the high density plasma that is produced by oxygen glow discharge.
9. the method for preparing the Lithium niobium trioxide surfacial pattern according to claim 1; It is characterized in that; The said etch step that repeats fluorine-based plasma of above-mentioned employing and oxygen plasma is two kinds of plasma bodys of fluorine-based plasma of repeated using and oxygen plasma to lithium niobate substrate carry out repeatedly, multiple etching.
10. the method for preparing the Lithium niobium trioxide surfacial pattern according to claim 1 is characterized in that, the Lithium niobium trioxide surfacial pattern of said preparation, and its degree of depth is repeatedly fluorine-based plasma etching gained degree of depth sum.
CN201110245639A 2011-08-25 2011-08-25 Method for preparing lithium niobate surface pattern Pending CN102304767A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732965A (en) * 2012-07-04 2012-10-17 杭州士兰明芯科技有限公司 Lithium niobate substrate and manufacturing method thereof
CN102738339A (en) * 2012-07-04 2012-10-17 杭州士兰明芯科技有限公司 Lithium niobate substrate provided with pattern structure and manufacturing method thereof
CN111627811A (en) * 2020-06-10 2020-09-04 电子科技大学 Lithium tantalate micro-patterning method based on reactive ion etching
CN112596160A (en) * 2020-12-16 2021-04-02 南京中电芯谷高频器件产业技术研究院有限公司 Preparation method of high-quality thin-film lithium niobate micro-nano grating
CN112768348A (en) * 2021-01-18 2021-05-07 复旦大学 Optimization method for etching lithium niobate material and improving side wall angle

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
H. NAGATA等: "Growth of crystalline LiF on CF4 plasma etched LiNbO3 substrates", 《JOURNAL OF CRYSTAL GROWTH》 *
H.HU等: "Plasma etching of proton-exchanged lithium niobate", 《J.VAC.SCI.TECHNOL.A》 *
NAOKI MITSUGI等: "Challenges in electron cyclotron resonance plasma etching of LiNbO3 Surface for fabrication of ridge optical waveguides", 《J. VAC. SCI. TECHNOL. A》 *
SARAH BENCHABANE等: "Highly selective electroplated nickel mask for lithium niobate dry etching", 《JOURNAL OF APPLIED PHYSICS》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732965A (en) * 2012-07-04 2012-10-17 杭州士兰明芯科技有限公司 Lithium niobate substrate and manufacturing method thereof
CN102738339A (en) * 2012-07-04 2012-10-17 杭州士兰明芯科技有限公司 Lithium niobate substrate provided with pattern structure and manufacturing method thereof
CN102738339B (en) * 2012-07-04 2015-09-16 杭州士兰明芯科技有限公司 There is lithium niobate substrate and the manufacture method thereof of patterned structures
CN111627811A (en) * 2020-06-10 2020-09-04 电子科技大学 Lithium tantalate micro-patterning method based on reactive ion etching
CN112596160A (en) * 2020-12-16 2021-04-02 南京中电芯谷高频器件产业技术研究院有限公司 Preparation method of high-quality thin-film lithium niobate micro-nano grating
CN112596160B (en) * 2020-12-16 2022-07-05 南京中电芯谷高频器件产业技术研究院有限公司 Preparation method of high-quality thin-film lithium niobate micro-nano grating
CN112768348A (en) * 2021-01-18 2021-05-07 复旦大学 Optimization method for etching lithium niobate material and improving side wall angle
CN112768348B (en) * 2021-01-18 2022-05-20 复旦大学 Optimization method for etching lithium niobate material and improving side wall angle

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Application publication date: 20120104