CN104992900B - α‑Al2O3Single-crystal surface SiO2The preparation method of mask - Google Patents

α‑Al2O3Single-crystal surface SiO2The preparation method of mask Download PDF

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Publication number
CN104992900B
CN104992900B CN201510354321.6A CN201510354321A CN104992900B CN 104992900 B CN104992900 B CN 104992900B CN 201510354321 A CN201510354321 A CN 201510354321A CN 104992900 B CN104992900 B CN 104992900B
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sio
mask
crystal surface
preparation
monocrystalline
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CN104992900A (en
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申健
张丹
庞春玲
张飞虎
甘阳
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Harbin Institute of Technology
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Harbin Institute of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/027—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34
    • H01L21/033—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising inorganic layers
    • H01L21/0334—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising inorganic layers characterised by their size, orientation, disposition, behaviour, shape, in horizontal or vertical plane
    • H01L21/0337—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising inorganic layers characterised by their size, orientation, disposition, behaviour, shape, in horizontal or vertical plane characterised by the process involved to create the mask, e.g. lift-off masks, sidewalls, or to modify the mask, e.g. pre-treatment, post-treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/20—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate

Abstract

α‑Al2O3Single-crystal surface SiO2The preparation method of mask, it is related to a kind of single-crystal surface SiO2The preparation method of mask.The present invention is to solve photoetching process to prepare SiO2Mask step is complicated, and cost is high, causes existing α Al2O3Single-crystal surface SiO2Mask is difficult in α Al2O3The problem of upper preparation.Method：First, pre-process；2nd, SiO will have been disperseed2The absolute ethyl alcohol of ball is added dropwise in α Al2O3Single-crystal surface；3rd, by the α Al after step 2 is handled2O3Monocrystalline is placed in 5min at room temperature, is then placed into handling in tube furnace, that is, completes α Al2O3Single-crystal surface SiO2The making of mask.The present invention's can be simply in α Al2O3Single-crystal surface prepares SiO2Mask, and can obtain micron order hexagon SiO2Mask and nanoscale hemispherical SiO2Mask, the preparation method are reproducible.The SiO of preparation2Mask equipment is simple, easy to operate, is easy to grasp, process safety, pollution-free.The invention belongs to the preparation field of mask.

Description

α-Al2O3Single-crystal surface SiO2The preparation method of mask
Technical field
The present invention relates to a kind of single-crystal surface SiO2The preparation method of mask.
Background technology
α-Al2O3 is the most common configuration crystal formation of aluminum oxide, α-Al2O3Monocrystalline is called corundum, sapphire, ruby.α- Al2O3Monocrystalline possesses many unique physical and chemical performances, is a kind of important electronics, ceramics, catalysis oxide material, In these applications, sapphire is grown in common Sapphire Substrate as the backing material prepared needed for GaN base thin film epitaxial growth On GaN, a large amount of dislocation defects propagate bottom-up.The GaN, GaN being grown in groove-shaped Sapphire Substrate (1 μm of depth) Layer carries out lateral growth at the top of Sapphire Substrate, and it is empty that some are formd in two growth front boundary mergences in pattern side wall Hole.The lateral growth region dislocation of heterojunction structures of the GaN on PSS has bent 90 °, and dislocation does not travel to the surface of GaN layer, So as to strengthen GaN base light emitting (LED) luminescent properties.
α-Al2O3The patterned substrate preparation method of monocrystalline is broadly divided into dry etching and wet etching, at present wet etching Cost is relatively low, but needs in α-Al2O3Single-crystal surface is earth silicon mask, SiO2α-the Al of mask covering part2O3Monocrystalline by To protection, it is not etched.SiO is not covered2Mask covering part is etched by high-temperature strong acid, so as in α-Al2O3Single-crystal surface generates Figure.
But photoetching process prepares SiO2Mask step is complicated, and cost is high, causes existing α-Al2O3Single-crystal surface SiO2Cover Film is difficult to, in α-Al2O3The problem of upper preparation.
The content of the invention
The invention aims to solve photoetching process to prepare SiO2Mask step is complicated, and cost is high, cause existing α- Al2O3Single-crystal surface SiO2Mask is difficult in α-Al2O3The problem of upper preparation, the invention provides a kind of α-Al2O3Single-crystal surface SiO2The preparation method of mask.
α-the Al of the present invention2O3Single-crystal surface SiO2The preparation method of mask is through the following steps that realize：
First, pre-process：
At room temperature, by α-Al2O3Monocrystalline, which is placed in ethanol, soaks 12h, then with deionized water rinsing α-Al2O3Monocrystalline, Nitrogen dries up again；
At room temperature, by SiO2Ball is added in absolute ethyl alcohol, ultrasonic disperse 10min；
2nd, by the α-Al by step 1 processing2O3Monocrystalline is placed in corundum crucible, and will disperse SiO2Ball it is anhydrous Ethanol is added dropwise in α-Al2O3Single-crystal surface, to having disperseed SiO2The absolute ethyl alcohol of ball is paved with α-Al2O3The surface of monocrystalline；
3rd, by the α-Al after step 2 is handled2O3Monocrystalline is placed in 5min at room temperature, is then placed into tube furnace, sets Tubular type furnace temperature is warming up to 1000 DEG C, and constant temperature 20min by 20 DEG C through 200min, then is warming up to 1300 through 80min by 1000 DEG C DEG C~1450 DEG C, constant temperature 1h~2h, 20 DEG C finally are cooled to through 800min by 1300 DEG C~1450 DEG C, completes α-Al2O3Monocrystalline table Face SiO2The making of mask.
SiO described in the step one of the present invention2Bulb diameter is 5 microns.
The absolute ethyl alcohol used in the step one of the present invention is commercially available prod.
α-the Al of the present invention2O3Single-crystal surface SiO2The preparation method of mask is a kind of simple micron order, nanoscale SiO2 Mask preparation method, can be simply in α-Al2O3Single-crystal surface prepares SiO2Mask, and can obtain micron order hexagon SiO2Cover Film and nanoscale hemispherical SiO2Mask, the preparation method are reproducible.The SiO of preparation2Mask equipment is simple, easy to operate, easily It is process safety, pollution-free in grasp.
Present invention has the advantages that：
(1) present invention applies 5 microns of commercially available SiO2Microballoon and common tube furnace, make SiO2Microballoon is at 1400 DEG C or so Lower softening and partial sublimation, in temperature-fall period, SiO2Condense in α-Al2O3Single-crystal surface, softening part generation micron order six side The SiO of shape2Mask, sublimed fraction generation nanoscale hemispherical SiO2Mask.
(2) to α-Al2O3Monocrystalline is pre-processed (step 1), and what this step removed is predominantly combined with the surface weaker point Subtype pollutant, beneficial to SiO2Bead is in α-Al2O3Single-crystal surface is uniformly distributed.
(3) do dispersant using absolute ethyl alcohol in step 2, it is cheap, and volatility is good, will not remain in α- Al2O3Single-crystal surface.
(4) 5 microns of SiO are made in step 32Microballoon is fixed on α-Al2O3Single-crystal surface uses common tube furnace, directly Burning is connect, avoids photoetching process SiO2Expensive equipment of metal organic chemical vapor deposition needed for mask.
Brief description of the drawings
Fig. 1 is covered with SiO in experiment one2α-the Al of mask2O3SEM (SEM) photo of monocrystalline；
Fig. 2 is covered with SiO in experiment one2α-the Al of mask2O3SEM (SEM) photo of monocrystalline；
Fig. 3 is the α-Al that will be covered with earth silicon mask2O3Monocrystalline is removed after high-temperature strong acid etches with hydrofluoric acid SiO2After mask, obtained patterned substrate photo；
Fig. 4 is the α-Al that will be covered with earth silicon mask2O3Monocrystalline is removed after high-temperature strong acid etches with hydrofluoric acid SiO2After mask, obtained patterned substrate photo.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition between each embodiment Any combination.
Embodiment one：Present embodiment is α-Al2O3Single-crystal surface SiO2The preparation method of mask is by following What step was realized：
First, pre-process：
At room temperature, by α-Al2O3Monocrystalline, which is placed in ethanol, soaks 12h, then with deionized water rinsing α-Al2O3Monocrystalline, Nitrogen dries up again；
At room temperature, by SiO2Ball is added in absolute ethyl alcohol, ultrasonic disperse 10min；
2nd, by the α-Al by step 1 processing2O3Monocrystalline is placed in corundum crucible, and will disperse SiO2Ball it is anhydrous Ethanol is added dropwise in α-Al2O3Single-crystal surface, to having disperseed SiO2The absolute ethyl alcohol of ball is paved with α-Al2O3The surface of monocrystalline；
3rd, by the α-Al after step 2 is handled2O3Monocrystalline is placed in 5min at room temperature, is then placed into tube furnace, sets Tubular type furnace temperature is warming up to 1000 DEG C, and constant temperature 20min by 20 DEG C through 200min, then is warming up to 1300 through 80min by 1000 DEG C DEG C~1450 DEG C, constant temperature 1h~2h, 20 DEG C finally are cooled to through 800min by 1300 DEG C~1450 DEG C, completes α-Al2O3Monocrystalline table Face SiO2The making of mask.
SiO in present embodiment step 1 and two2Ball and absolute ethyl alcohol are commercially available prod, absolute ethyl alcohol mass fraction 99.7%.
α-Al in present embodiment2O3Single-crystal surface SiO2The preparation method of mask is a kind of simple micron order, nanoscale SiO2Mask preparation method, can be simply in α-Al2O3Single-crystal surface prepares SiO2Mask, and can obtain micron order hexagon SiO2 Mask and nanoscale hemispherical SiO2Mask, the preparation method are reproducible.The SiO of preparation2Mask equipment is simple, easy to operate, It is easy to grasp, it is process safety, pollution-free.
Embodiment two：Present embodiment and SiO described in step 1 unlike embodiment one2Ball is straight Footpath is 5 microns.It is other identical with embodiment one.
Embodiment three：Again by 1000 in present embodiment step 3 unlike embodiment one or two DEG C 1310 DEG C~1440 DEG C are warming up to through 80min, constant temperature 1.2h~1.8h.Other steps and parameter and embodiment one or Two is identical.
Embodiment four：In step 3 unlike one of present embodiment and embodiment one to three again by 1000 DEG C are warming up to 1330 DEG C~1410 DEG C through 80min, constant temperature 1.3h~1.7h.One of other and embodiment one to three It is identical.
Embodiment five：In step 3 unlike one of present embodiment and embodiment one to four again by 1000 DEG C are warming up to 1350 DEG C~1400 DEG C through 80min, constant temperature 1.4h~1.6h.One of other and embodiment one to four It is identical.
Embodiment six：In step 3 unlike one of present embodiment and embodiment one to five again by 1000 DEG C are warming up to 1400 DEG C through 80min, constant temperature 1h.It is other identical with one of embodiment one to five.
Using following experimental verification beneficial effects of the present invention：
Experiment one：
α-Al2O3Single-crystal surface SiO2The preparation method of mask is through the following steps that realize：
First, pre-process：
A, at room temperature, by α-Al2O3Monocrystalline, which is placed in ethanol, soaks 12h, then with deionized water rinsing α-Al2O3It is single Crystalline substance, then nitrogen drying；
B, at room temperature, by a diameter of 5 microns of SiO2Bead is added in absolute ethyl alcohol, ultrasonic disperse processing 10min；
2nd, by the α-Al after step 1 is handled2O3Monocrystalline is placed in corundum crucible, will be dispersed with 5 microns of SiO2Bead Absolute ethyl alcohol be added dropwise in α-Al2O3Single-crystal surface, ethanol liquid are paved with single-crystal surface；
3rd, by the α-Al after step 2 is handled2O3Monocrystalline is placed in 5min at room temperature, then sets tube furnace heating-cooling bent Line, by 20 DEG C through 200min to 1000 DEG C, constant temperature 20min, 1400 DEG C are warming up to through 80min by 1000 DEG C, constant temperature 1h, by 1400 DEG C 20 DEG C are cooled to through 800min, that is, complete α-Al2O3Single-crystal surface SiO2The making of mask.
5 microns of SiO in experiment one2Bead and absolute ethyl alcohol are commercially available prod, absolute ethyl alcohol mass fraction 99.7%.
α-Al after the processing of experiment one2O3SEM (SEM) photo of monocrystalline as depicted in figs. 1 and 2, from It can be seen that 5 microns of SiO in Fig. 1 and Fig. 22Bead is in α-Al2O3Single-crystal surface generates the SiO of micron order hexagon2Mask and Nanoscale hemispherical SiO2Mask.
α-the Al covered with earth silicon mask after the processing of experiment one2O3Monocrystalline is after high-temperature strong acid etches, with hydrogen fluorine Acid removes SiO2The patterned substrate photo that mask obtains is as shown in Figure 3 and Figure 4.
It can be seen that through experiment one in α-Al2O3Single-crystal surface can obtain micron order hexagon SiO2Mask and nanoscale hemispherical SiO2Mask, the preparation method are reproducible.The SiO of preparation2Mask equipment is simple, easy to operate, is easy to grasp, process safety, It is pollution-free.

Claims (2)

1.α-Al2O3Single-crystal surface SiO2The preparation method of mask, it is characterised in that α-Al2O3Single-crystal surface SiO2The making of mask Method through the following steps that realize：
First, pre-process：
At room temperature, by α-Al2O3Monocrystalline, which is placed in ethanol, soaks 12h, then with deionized water rinsing α-Al2O3Monocrystalline, then nitrogen Air-blowing is done；
At room temperature, by SiO2Ball is added in absolute ethyl alcohol, ultrasonic disperse 10min；
2nd, by the α-Al by step 1 processing2O3Monocrystalline is placed in corundum crucible, and will disperse SiO2The absolute ethyl alcohol of ball It is added dropwise in α-Al2O3Single-crystal surface, to having disperseed SiO2The absolute ethyl alcohol of ball is paved with α-Al2O3The surface of monocrystalline；
3rd, by the α-Al after step 2 is handled2O3Monocrystalline is placed in 5min at room temperature, is then placed into tube furnace, sets tubular type Furnace temperature is warming up to 1000 DEG C, and constant temperature 20min by 20 DEG C through 200min, then by 1000 DEG C through 80min be warming up to 1300 DEG C~ 1450 DEG C, constant temperature 1h~2h, 20 DEG C finally are cooled to through 800min by 1300 DEG C~1450 DEG C, completes α-Al2O3Single-crystal surface SiO2The making of mask.
2. α-Al according to claim 12O3Single-crystal surface SiO2The preparation method of mask, it is characterised in that in step 1 The SiO2Bulb diameter is 5 microns.
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Citations (3)

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Publication number Priority date Publication date Assignee Title
CN101789467A (en) * 2010-02-20 2010-07-28 山东力诺太阳能电力股份有限公司 Polycrystalline silicon solar energy cell wet-method texturing manufacturing process
CN103647008A (en) * 2013-12-31 2014-03-19 中国科学院半导体研究所 Method for growing semi-polarity GaN (gallium nitride) thick film
CN104465900A (en) * 2014-12-03 2015-03-25 山东浪潮华光光电子股份有限公司 Structured arrangement manometer coarsened sapphire substrate and preparation method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7109068B2 (en) * 2004-08-31 2006-09-19 Micron Technology, Inc. Through-substrate interconnect fabrication methods
KR101062416B1 (en) * 2008-10-09 2011-09-06 성균관대학교산학협력단 Nano Device Formation Method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101789467A (en) * 2010-02-20 2010-07-28 山东力诺太阳能电力股份有限公司 Polycrystalline silicon solar energy cell wet-method texturing manufacturing process
CN103647008A (en) * 2013-12-31 2014-03-19 中国科学院半导体研究所 Method for growing semi-polarity GaN (gallium nitride) thick film
CN104465900A (en) * 2014-12-03 2015-03-25 山东浪潮华光光电子股份有限公司 Structured arrangement manometer coarsened sapphire substrate and preparation method

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